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  • Column liquid chromatography  (495)
  • maize  (201)
  • 42.75
  • Chemistry
  • GEOPHYSICS
  • Springer  (700)
  • 1990-1994  (700)
  • 1950-1954
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  • 1
    Electronic Resource
    Electronic Resource
    Modelling the constancy of X (1994)
    Springer
    Astrophysics and space science 216 (1994), S. 153-154 
    Details
    ISSN: 1572-946X
    Keywords: Chemistry ; Molecular Hydrogen ; Cloud Models
    Source: Springer Online Journal Archives 1860-2000
    Topics: Physics
    Notes: Abstract Observations of the CO J=1-0 line are commonly used as a tracer for molecular material in clouds. The ratio of the H2 column density to the integrated intensity of this line,X, is often taken to be constant, despite theoretical and observational uncertainty. We have tried to identify how this ratio depends on cloud parameters, testing a simple theoretical argument suggesting its invariance with respect to density. The apparent constancy can be understood if clouds are clumpy on scales of Av ≈ 1-2 mag.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00982486
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  • 2
    Electronic Resource
    Electronic Resource
    Characterization of four new β-tubulin genes and their expression during male flower development in maize (Zea mays L.) (1994)
    Springer
    Plant molecular biology 24 (1994), S. 295-315 
    Details
    ISSN: 1573-5028
    Keywords: β-tubulin ; microtubules ; maize ; gene expression
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Four different β-tubulin coding sequences were isolated from a cDNA library prepared from RNA from maize seedling shoots. The four genes (designated tub4, tub6, tub7 and tub8) represented by these cDNA clones together with the tub1 and tub2 genes reported previously encode six β-tubulin isotypes with 90–97.5% amino acid sequence identity. Results from phylogenetic analysis of 17 β-tubulin genes from monocot and dicot plant species indicated that multiple extant lines of β-tubulin genes diverged from a single precursor after the appearance of the two major subfamilies of α-tubulin genes described previously. Hybridization probes from the 3′ non-coding regions of six β-tubulin clones were used to quantify the levels of corresponding tubulin transcripts in different maize tissues including developing anthers and pollen. The results from these dot blot hybridization experiments showed that all of the β-tubulin genes were expressed in most tissues examined, although each gene showed a unique pattern of differential transcript accumulation. The tub1 gene showed a high level of transcript accumulation in meristematic tissues and almost no accumulation in the late stages of anther development and in pollen. In contrast, the level of tub4 transcripts was very low during early stages of male flower development but increased markedly (more than 100 times) during the development of anthers and in pollen. Results from RNAse protection assays showed that this increased hybridization signal resulted from expression of transcripts from one or two genes closely related to tub4. The tub4-related transcripts were not present in shoot tissue. Transcripts from the tub2 gene accumulated to very low levels in all tissues examined, but reached the highest levels in young anthers containing microspore mother cells. RNAse protection assays were used to measure the absolute levels of α- and β-tubulin transcripts in seedling shoot and in pollen. The α-tubulin gene subfamily I genes (tua1, tua2, tua4) contributed the great majority of α-tubulin transcripts in both shoot and pollen. Transcripts from the β-tubulin genes tub4, tub6, tub7, and tub8 were predominant in shoot, but were much less significant than the tub4-related transcripts in pollen.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00020169
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  • 3
    Electronic Resource
    Electronic Resource
    Addition of A- and U-rich sequence increases the splicing efficiency of a deleted form of a maize intron (1994)
    Springer
    Plant molecular biology 24 (1994), S. 449-463 
    Details
    ISSN: 1573-5028
    Keywords: AU-rich ; intron ; maize ; splicing
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Plant introns are generally short (〈200 nt) and AU-rich, and an elevated AU content is necessary for efficient splicing. Further, an intron in some plant genes enhances gene expression by a post-transcriptional mechanism that results in an increase of cytoplasmic mRNA. The specific intron features responsible for efficient splicing and enhancement are not well characterized in plants. Internal deletions of up to 80% of two maize introns, Adh1 intron 1 and maize actin intron 3, indicate that large segments of these introns are dispensable for normal function. However, extensive deletion (〉75%) of Adh1 intron 1 diminishes both intron enhancement and splicing efficiency. This finding suggests that there are internal sequence motifs required for intron function, and that these motifs are redundant. We attempted to repair a deletion-impaired Adh1 intron 1 variant by adding back either oligomers of defined sequence content or fragments of maize internal intron sequence. The addition of AU-rich oligomers improved splicing efficiency and in one example, a U-rich oligomer activated a cryptic 3′ splice acceptor. We also found that replacing the region proximal to the Adh1 intron 1 3′ acceptor with U-rich sequence improved splicing. We found that adding G- and C-rich oligomers did not improve intron function, but a C-rich oligomer activated a cryptic 3′ acceptor. The addition of internal intron sequence to an impaired intron improved splicing, and in one case, resulted in the activation of a cryptic 3′ acceptor. We present evidence that U-rich sequence immediately upstream of the 3′ splice junction increases splicing efficiency and contributes to, but does not uniquely specify, 3′ acceptor AG choice.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00024113
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  • 4
    Electronic Resource
    Electronic Resource
    Differential transcription of plastome-encoded genes in the mesophyll and bundle-sheath chloroplasts of the monocotyledonous NADP-malic enzyme-type C4 plants maize and Sorghum (1994)
    Springer
    Plant molecular biology 25 (1994), S. 669-679 
    Details
    ISSN: 1573-5028
    Keywords: C4 photosynthesis ; maize ; plastid gene expression ; Sorghum
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The transcription of plastome-encoded genes in mesophyll and bundle-sheath chloroplasts of the monocotyledonous NADP-malic enzyme-type C4 species Zea mays L. (maize) and Sorghum bicolor (L.) Moench. was investigated. RNA accumulation and transcription were assayed starting from isolated mesophyll and bundle-sheath chloroplasts and using quantitative northern and run-on transcription analysis. Determination of the mesophyll to bundle-sheath ratios of transcript abundance in maize and Sorghum chloroplasts showed that the mRNAs of the plastome-encoded photosystem II genes analysed (psbA, psbB, psbD, psbH and psbE/F) varied from 2.5- to 4.0-fold (maize) and 3.1- to 5.2-fold (Sorghum), respectively. The rbcL transcript, in contrast, was more abundant in bundle-sheath chloroplasts of both species, about 3-fold in maize and more than 10-fold in Sorghum. On the other hand, transcripts of genes encoding the 16S ribosomal RNA (r16) and subunits of photosystem I (psaA) and the cytochrome b/f complex (petB, petA) accumulated to similar levels in both types of chloroplasts. Determination of absolute transcript levels for rbcL and psbA in chloroplasts from maize and Sorghum demonstrated that for both genes, the mesophyll to bundle-sheath differences in transcript abundance were more pronounced in Sorghum. Measurements of the transcriptional activities of rbcL and psbA showed that the transcription rate of rbcL is higher in bundle-sheath chloroplasts while psbA is more actively transcribed in mesophyll chloroplasts. The differences in the transcription rates between the two chloroplast types were again more pronounced in Sorghum, thus reflecting the differences between maize and Sorghum in the relative levels of the rbcL and psbA transcripts. However, although transcription rate and mRNA abundance are correlated, they did not exactly match one another. This indicates additional regulation of transcript abundance at the level of RNA stability.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00029605
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  • 5
    Electronic Resource
    Electronic Resource
    Structure and function of selectable and non-selectable transgenes in maize after introduction by particle bombardment (1994)
    Springer
    Plant molecular biology 25 (1994), S. 951-961 
    Details
    ISSN: 1573-5028
    Keywords: Cell biology ; epigenetics ; maize ; transformation ; transgenes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Zea mays transformants produced by particle bombardment of embryogenic suspension culture cells of the genotype A188 × B73 and selected on kanamycin or bialaphos were characterized with respect to transgene integration, expression, and inheritance. Selection on bialaphos, mediated by thebar orpat genes, was more efficient than selection on kanamycin, mediated by thenptII gene. Most transformants contained multicopy, single locus, transgene insertion events. A transgene expression cassette was more likely to be rearranged if expression of that gene was not selected for during callus growth. Not all plants regenerated from calli representing single transformation events expressed the transgenes, and a non-selectable gene (uidA) was expressed in fewer plants than was the selectable transgene. Mendelian inheritance of transgenes consistent with transgene insertion at a single locus was observed for approximately two thirds of the transformants assessed. Transgene expression was typically, but not always, predictable in progeny plants-transgene silencing, as well as poor transgene transmission to progeny, was observed in some plant lines in which the parent plants had expressed the transgene.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00014669
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  • 6
    Electronic Resource
    Electronic Resource
    Partial sequencing and mapping of clones from two maize cDNA libraries (1994)
    Springer
    Plant molecular biology 26 (1994), S. 1085-1101 
    Details
    ISSN: 1573-5028
    Keywords: cDNA clones ; EST sequencing ; maize ; RFLP mapping
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract As one component of a maize genome project, we report the analysis of a number of randomly selected cDNAs, by a combination of measuring mRNA expression, ‘single-pass’ sequencing (SPS), and genome mapping. Etiolated seedling (490) and membrane-free polysomal endosperm cDNA clones (576) were evaluated for their transcription levels by hybridizing with a probe prepared from total mRNA and categorized as corresponding to abundantly or rarely expressed mRNAs and as either constitutive or tissue-specific. A total of 313 clones from the two libraries were submitted to ‘single-pass’ sequencing from the presumed 5′ end of the mRNA and the nucleotide sequence compared with the GenBank database. About 61% of the clones showed no significant similarities within GenBank, 14% of the clones exhibited a high degree of similarity, while the remaining 25% exhibited a lesser degree of similarity. The chromosomal location of more than 300 clones was determined by RFLP mapping using standard populations. The results demonstrate that a combination of analyses provides synergistic information in eventually deducing the actual function of these types of clones.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00040691
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  • 7
    Electronic Resource
    Electronic Resource
    Non-systemic expression of a stress-responsive maize polyubiquitin gene (Ubi-1) in transgenic rice plants (1994)
    Springer
    Plant molecular biology 26 (1994), S. 1007-1012 
    Details
    ISSN: 1573-5028
    Keywords: cell cycle ; maize ; non-systemic expression ; polyubiquitin gene ; stress response
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract We have used the promoter, 1st exon and 1st intron of the maize polyubiquitin gene (Ubi-1) for rice transformation experiments and revealed the characteristic expression of Ubi-1 gene: (1) Ubi-1 gene is not regulated systemically but rather individual cells respond independently to the heat or physical stress; (2) Ubi-1 gene changes its tissue-specific expression in response to stress treatment; (3) the expression of Ubi-1 gene is dependent on cell cycle.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00028868
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  • 8
    Electronic Resource
    Electronic Resource
    Isolation and characterisation of a maize cDNA that complements a 1-acyl sn-glycerol-3-phosphate acyltransferase mutant of Escherichia coli and encodes a protein which has similarities to other acyltransferases (1994)
    Springer
    Plant molecular biology 26 (1994), S. 211-223 
    Details
    ISSN: 1573-5028
    Keywords: maize ; 1-acyl-sn-glycerol-3-phosphate acyltransferase ; complementation cloning
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract We selected cDNA plasmid clones that corrected the temperature-sensitive phenotype of Escherichia coli strain JC201, which is deficient in 1-acyl-sn-glycerol-3-phosphate acyltransferase activity. A plasmid-based maize endosperm cDNA library was used for complementation and a plasmid that enabled the cells to grow at 44°C on ampicillin was isolated. Addition of this plasmid (pMAT1) to JC201 restored 1-acyl-sn-glycerol-3-phosphate acyltransferase activity to the cells. Total phospholipid labelling showed that the substrate for the enzyme, lysophosphatidic acid, accumulated in JC201 and was further metabolised to phosphatidylethanolamine in complemented cells. Membranes isolated from such cells were able to convert lysophosphatidic acid to phosphatidic acid in acyltransferase assays. The cDNA insert of pMAT1 contains one long open reading frame of 374 amino acids which encodes a protein of relative molecular weight 42 543. The sequence of this protein is most similar to SLC1, which is thought to be able to acylate glycerol at the sn-2 position during synthesis of inositol-containing lipids. Homologies between the SLC1 protein, the 1-acyl-sn-glycerol-3-phosphate acyltransferase of E. coli (PlsC) and the maize ORF were found with blocks of conserved amino acids, whose spacing was conserved between the three proteins, identifiable.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00039533
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  • 9
    Electronic Resource
    Electronic Resource
    In vivo analysis of intron processing using splicing-dependent reporter gene assays (1994)
    Springer
    Plant molecular biology 26 (1994), S. 1785-1795 
    Details
    ISSN: 1573-5028
    Keywords: intron ; maize ; splicing ; vectors ; Zea mays
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The mechanisms of intron recognition and processing have been well-studied in mammals and yeast, but in plants the biochemistry of splicing is not known and the rules for intron recognition are not clearly defined. To increase understanding of intron processing in plants, we have constructed new pairs of vectors, pSuccess and pFail, to assess the efficiency of splicing in maize cultured cells. In the pFail series we use translation of pre-mRNA to monitor the amount of unspliced RNA. We inserted an ATG codon in the Bz2 (Bronze-2) intron in frame with luciferase: this construct will express luciferase activity only when splicing fails. In the pSuccess series the spliced message is monitored by inserting an ATG upstream of the Bz2 intron in frame with luciferase: this construct will express luciferase activity only when splicing succeeds. We show here, using both the wild-type Bz2 intron and the same intron with splice site mutations, that the efficiency of splicing can be estimated by the ratio between the luciferase activities of the vector pairs. We also show that mutations in the unique U-rich motif inside the intron can modulate splicing. In addition, a GC-rich insertion in the first exon increases the efficiency of splicing, suggesting that exons also play an important role in intron recognition and/or processing.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00019492
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  • 10
    Electronic Resource
    Electronic Resource
    Molecular and physiological evaluation of transgenic tobacco plants expressing a maize phosphoenolpyruvate carboxylase gene under the control of the cauliflower mosaic virus 35S promoter (1994)
    Springer
    Transgenic research 3 (1994), S. 287-296 
    Details
    ISSN: 1573-9368
    Keywords: C4-plant ; maize ; phosphoenolpyruvate carboxylase ; quantum yield ; transgenic tobacco
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The expression of maize (Zea mays) phosphoenolpyruvate carboxylase (PEPC) gene constructs in transgenic tobacco plants (Nicotiana tabacum) was studied. Where transcription was under the control of a CaMV 35S promoter, maize PEPC transcripts of the correct size were detected. Western blot analysis indicated that the transgenic plants contained about twice as much PEPC as non-transformed plants. Furthermore, the enzymatic activity of PEPC in the leaves of these transgenic plants was up to twice as high as that in non-transformed plants. Two forms of PEPC with different kinetic properties were identified in leaf extracts of the transgenic plants: one form (the maize isoform) gave a high apparentK m value for phosphoenolpyruvate (PEP) and a high maximum activity, and the other (the tobacco isoform) exhibited a low apparentK m value for PEP and a low maximum activity. These biochemical differences resulted in several significant physiological changes in the transgenic plants: (1) the growth rate of the transgenic plants was lower than that of non-transgenic plants: (2) chlorophyll content per leaf area was relatively lower in the transgenic plants; and (3) the quantum yield of photosynthesis in the transgenic plants was not affected by changes in leaf temperature.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01973588
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  • 11
    Electronic Resource
    Electronic Resource
    Determination of triamterene in urine by HPLC using fluorescence detection and column-switching (1994)
    Springer
    Chromatographia 38 (1994), S. 29-34 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column-switching ; Determination of triamterene ; Fluorescence detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A liquid chromatographic method incorporating column-switching and fluorimetric detection for the determination of triamterene in untreated urine, is described. The urine samples (5 μL) were directly introduced onto an Hypersil ODS-C18, 30 μm (20 mm×2.1 mm I.D.) pre-column. Polar urinary compounds were removed by flushing the pre-column with water for 1 min, and the analyte was then switched onto an HP-LiChrospher RP C18,5 μm (125 mm×4mm ID) analytical column using an acetonitrile/phosphate buffer gradient elution. Fluorescence detection was performed at 230 nm excitation and 430 nm emission wavelengths. The recovery of drug was 102±2% in the 0.10–20.0 μg/mL concentration range, the limit of detection being 5 ng/mL. A validation of the usefulness of this procedure was accomplished by analysing urine extracts obtained from real samples.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02275723
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  • 12
    Electronic Resource
    Electronic Resource
    Statistical evaluation of the validity of a method for characterizing stationary phases for reversed-phase liquid chromatography based on retention of homologous series (1994)
    Springer
    Chromatographia 38 (1994), S. 137-146 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Characterization of reversed phases ; Column hydrophobicity ; Column hydrophylicity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The validity of a method for characterizing stationary phases for reversed-phase, liquid chromatography, based on the use of homologous series, has been evaluated. The method is based on a retention model which describes the dependence of the logarithm of the capacity factor on mobile phase composition and the carbon number of specific homologous series. A first-order as well as a second-order version of this model was investigated. The second-order model proved to be a significant improvement on the first-order model, even for smaller mobile-phase ranges. Nevertheless both models showed a significant lack of fit, reflecting the incompleteness of these models. Therefore, it is very questionable whether this method is suitable to describe HPLC-column characteristics like hydrophobicity and hydrophylicity.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02290326
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  • 13
    Electronic Resource
    Electronic Resource
    Control of adsorption and solubility in gradient high performance liquid chromatography. Part 3. Sudden-transition gradient elution of styrene/ acrylonitrile copolymers (1994)
    Springer
    Chromatographia 38 (1994), S. 749-755 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Copoly(styrene/acrylonitrile) ; Gradient elution ; Precipitation chromatography of polymers ; Solubility of polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Copolymers from styrene and acrylonitrile could be separated according to composition by gradient elution through methanol after injection inton-heptane and sudden addition of 50, 60, or 70 vol% tetrahydrofuran. The peak sequence was the same as with a common binary gradientn-heptane/tetrahydrofuran, i.e., retention increased with acrylonitrile content of the samples. With copolymers containing 37, 31, or 26% acrylonitrile, the elution characteristics in the ternary systems could be logically extrapolated towards the points measured in the corresponding binary gradient system.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02269631
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  • 14
    Electronic Resource
    Electronic Resource
    Chiral recognition of structurally related aminoalkylphosphonic acid derivatives on an acetylated beta-cyclodextrin bonded phase (1994)
    Springer
    Chromatographia 38 (1994), S. 771-775 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral recognition ; Aminoalkylphosphonic acid derivatives ; β-cyclodextrin bonded phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An acetylated β-cyclodextrin column was used to analyse the enantiomeric resolution of a number of aminophosphonic acids. Effects of the structure of these compounds on the extent of separation was examined. Molecular modelling studies were also carried out in an attempt to relate any interaction between the amino and phosphonic acid groups to chiral recognition by the stationary phase.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02269635
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  • 15
    Electronic Resource
    Electronic Resource
    Interaction of cyclodextrins with drugs. Chromatographic investigation using a cyclodextrin bonded-phase and its application to chiral separations (1994)
    Springer
    Chromatographia 38 (1994), S. 381-385 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral separation ; Association constants ; Frontal analysis ; Cyclodextrin bonded-phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The interaction between cyclodextrin and the drug (1R,2S,3S,4S)-(5Z)-7-(3-((phenylsulfonyl)amino)bicyclo[2.2.1]hept-2-yl)hept-5-enoic acid ((+)-S-145), was studied using α-, β-, and γ-cyclodextrin bonded-phase columns. Retention behavior of (+)-S-145 on these columns revealed that the strength of inclusion was β→γ→α-cyclodextrin. Interaction between β-cyclodextrin and (+)-S-145 was found to increase as the proportion of carboxylic ion in the (+)-S-145 molecule increased. Comparison of binding capacities of these bondedsilica gels obtained by frontal analysis and surface coverage indicated that availability of the immobilized β- and γ-cyclodextrin was 20–25%. The synthesized β-cyclodextrin bonded-phase column was superior to that of commercial columns in terms of chiral separation of (±)-S-145. A typical usage of the β-cyclodextrin column is discussed for separation of (±)-S-145 in plasma samples.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02269784
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  • 16
    Electronic Resource
    Electronic Resource
    Reverse phase high-performance liquid chromatographic determination of primary and secondary aliphatic alcohols as phthalate monoesters by UV detection (1994)
    Springer
    Chromatographia 38 (1994), S. 417-420 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Primary and secondary aliphatic alcohols ; Aqueous derivatization ; Phthalic acid monoesters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Determination of primary and secondary aliphatic alcohols in aqueous and nonaqueous solutions by high-performance liquid chromatography (HPLC) is described. The alcohol is derivatized with phthalic anhydride to yield the corresponding monophthalate. Separation of the derivative is achieved on an ODS-10 reverse phase (RP) column by elution with an appropriate isocratic mobile phase of acetonitrile and aqueous phosphoric acid (0.1%). Detection is accomplished by UV absorption at 230 nm or 280 nm giving linear calibration plots, for alcohols in aqueous solution from 0.05% to 0.50% (w/v) and in pyridine solution from 0.0025% to 0.0250% (w/v).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02269829
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  • 17
    Electronic Resource
    Electronic Resource
    Solute-micelle association constants of some polynuclear aromatic hydrocarbons by micellar liquid chromatography with alcohol additives to mobile phase (1994)
    Springer
    Chromatographia 38 (1994), S. 342-348 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hybrid mobile phases containing alcohols ; Solute-micelle association constants ; Polynuclear aromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The interaction between some polynuclear aromatic hydrocarbons of environmental concern, and sodium dodecylsulphate and hexadecyltrimethylammonium bromide in the presence of methanol, 2-propanol and n-butanol has been evaluated by high-performance liquid chromatography using micellar mobile phases. Solute-micelle association constants have been determined for the compounds investigated. The results show that the addition of the alcohol to the mobile phase decreases the association constant values, methanol 〈2-propanol 〈n-butanol, relative to those in the absence of any additive.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02269778
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  • 18
    Electronic Resource
    Electronic Resource
    Solid phase extraction applied to the determination of biogenic amines in wines by HPLC (1994)
    Springer
    Chromatographia 38 (1994), S. 571-578 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Wine ; Biogenic amines ; Solid-phase extraction ; Derivatization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method suitable for the determination of 19 biogenic amines in wine has been developed. The method involves derivatization of amines by treatment with dansyl chloride and solid-phase extraction of the derivatives. Prior to the derivatization procedure, clean-up of the wine sample with polyvinylpyrrolidone is carried out. Reversed-phase gradient elution HPLC with UV detection at 250 nm was used to determine these compounds. Some consideration was given to the effect of temperature on the separation process. Linearity of derivatization was obtained for amounts of all the biogenic amines ranging from 500 μg·L−1 to 20 mg·L−1. Limits of detection (signal-to-noise ratio=3) of the amines were similar for all the dansylderivatives (between 50 and 150 μg·L−1). Addition of standard amines was used for the determination of amine recoveries. These were better than 85% for ethanolamine, tryptamine, phenetylamine, putrescine, cadaverine and histamine. The overall process was succesfully applied to identify and quantify biogenic amines in white and red wines.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02277156
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  • 19
    Electronic Resource
    Electronic Resource
    Enantiomer separaton of tifluadom and analogues by liquid chromatography with cellulose-based chiral stationary phases (1994)
    Springer
    Chromatographia 38 (1994), S. 629-632 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral/enantiomeric iseparation ; Cellulose-based chiral phases ; Tifluadom analogues ; 2-acylaminomethyl-1,4-benzodiazepines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The resolution of nine recamic mixtures of tifluadom analogues has been evaluated using the chiral stationary phases Chiralcel OD and Chiralcel OJ. The separation was performed on an analytical scale to optimize the conditions for chiral resolution, approaching baseline separation, of the two enantiomers. Eight racemates were baseline separated on Chiralcel OJ using a mobile phase of hexane/2-propanol.
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    URL: http://dx.doi.org/10.1007/BF02277166
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  • 20
    Electronic Resource
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    Comparative study of solid-phase extraction of phenolic compounds. Influence of the ion pair reagent (1994)
    Springer
    Chromatographia 38 (1994), S. 579-584 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenolic compounds ; Ion-pair solid-phase extraction ; Comparison of sorbents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A comparative study of the solid phase extraction of phenolic compounds in water was carried out. Three different sorbents, C18, CH and PLRP-S, were tested for the preconcentration process in order to determine phenolic compounds in water at μg l−1 levels by reversed-phase LC separation and diode-array detection. The addition of an ion-pair reagent in the extraction process was also studied in order to increase the breakthrough volume of some compounds. Using the optimized conditions the limit of detection was less than 0.5 μg l−1, the maximum admissible concentration (MAC) in drinking water. The method was applied to determine phenolic compounds in Ebro river water however no phenols were found within the detection limits of the method.
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    URL: http://dx.doi.org/10.1007/BF02277157
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    Extraction of basic drugs from whole blood and determination by high performance liquid chromatography (1994)
    Springer
    Chromatographia 38 (1994), S. 617-623 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Extraction-determination ; Basic drugs ; Blood
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method for the extraction of basic drugs from whole blood based on the use of a buffered protein precipitating reagent at pH9, to form NiWO4 in biological fluids and a ternary organic extracting phase of density below 1 is proposed. The extract is analysed by high performance liquid chromatography using a Hypersil C8 column and detection at 230 nm; the mobile phases used consist of binary mixtures of acetonitrile and aqueous solutions containing 20 mmol/l ofn-propylamine at pH 5 andn-hexylamine at pH 4, as blockers of the free silanol groups. The proposed method was applied to the determination of 16 basic drugs including narcotics, analgesics, cocaine-related compounds and adulterants, as well as 8 benzodiazepines, in whole blood.
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    URL: http://dx.doi.org/10.1007/BF02277164
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    Determination of imazethapyr and imazapyr residues in soil by coupled-column liquid chromatography (1994)
    Springer
    Chromatographia 39 (1994), S. 62-66 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column switching ; Imidazolinone herbicides in soil ; Imazethapyr ; Imazapyr
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A column-switching method using two separation columns combined with UV detection at 260 or 236 nm has been used to determine the imidazolinone herbicides imazethapyr and imazapyr in soils. The residues were extracted from the soil with 0.1 M aqueous sodium carbonate solution and, after adjusting the pH to 2.0, the solution was partitioned with dichloromethane. Limits of determination for imazethapyr and imazapyr were 3 μg/kg. Recoveries were from 55 to 75% for both imidazolinone herbicides in the range 3–100 μg/kg in soil.
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    URL: http://dx.doi.org/10.1007/BF02320459
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    A novel derivatisation procedure for inorganic mercury(II) for HPLC analysis (1994)
    Springer
    Chromatographia 39 (1994), S. 246-248 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mercury ; Diphenylethynylmercury
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new procedure for derivatisation of inorganic mercury(II) to diphenylethynylmercury with simultaneous extraction into dichloromethane is proposed. The organomercury derivative is effectively analysed by HPLC using UV detection. The calibration curve is linear over three orders of magnitude (0.02–50 mg L−1 Hg); the detection limit is 0.1 ng Hg. A preliminary study of the effect of potential interfering agents, in particular Cu(II), Zn(II), Cd(II), Pb(II), and cysteine, and applications of the present methodology to real environmental samples are presented.
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    URL: http://dx.doi.org/10.1007/BF02274507
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    Determination of short chain aliphatic acids in silage effluents by ion exclusion chromatography (1994)
    Springer
    Chromatographia 38 (1994), S. 43-51 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion exclusion ; Alipathic acids ; Silage effluents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Short chain aliphatic acids are important components of the dissolved organic matter in silage effluents. Although ion exclusion chromatography offers some advantages for the analysis of these compounds, no attempt has yet been made to prove the suitability of this method for silage effluent analysis. In order to gain experience in this field, the separation characteristics of a Dionex ion exclusion column (IonPac-ICE As5) have been evaluated, the separation conditions have been improved, and several sample clean-up methods have been checked. Ten effluents generated during silaging of five different crops were collected from Bavarian farms and analyzed. Lactic and acetic acids were the predominant aliphatic acids. Pyruvic, formic, propionic, and succinic acid were detected in all samples, whereas glyceric and iso-citric acid were found in a few samples only. If some restrictions of substance specificity and separation efficiency can be accepted, the analytical method presented will be a reliable tool for the analysis of carboxylic acids in silage effluents.
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    URL: http://dx.doi.org/10.1007/BF02275725
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    Polymer encapsulated packing material for reversed phase liquid chromatography (1994)
    Springer
    Chromatographia 38 (1994), S. 756-760 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polymer encapsulated packings ; Poly(ethylstyrene-divinylbenzene) ; Preparation and evaluation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A series of polymer-encapsulated packing materials for reversed phase high-performance liquid chromatography was prepared by radical polymerization of ethylstyrene and divinylbenzene with vinyl-modified silica in solution. Some characteristics such as polymer structure, swelling propensity, residual silanols, column efficiency and retention properties were evaluated. Such material is easy to pack and yields high column efficiencies. Its superior performance for the separation of mixtures of aromatic hydrocarbons, amino- and hydroxyl group containing compounds are demonstrated by several examples.
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    URL: http://dx.doi.org/10.1007/BF02269632
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    Application of β-cyclodextrin for the analysis of estrogenic steroids in human urine by high-performance liquid chromatography (1994)
    Springer
    Chromatographia 38 (1994), S. 168-172 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; β-Cyclodextrin in mobile phase ; Estrogens ; Pregnant and non-pregnant women
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A procedure is described for simultaneous determination of estriol, estrone and 17β-estradiol in human urine. After acid hydrolysis of the sulphate conjugates, the estrogens were extracted into diethyl ether. The ether extracts were concentrated and applied directly to an HPLC column. Using a 25 cm C-18 column and acetonitrile-water modified by the addition of β-cyclodextrin as mobile phase, the separation of estriol, estradiol and estrone was achieved within 20 minutes. The extraction of estrogens from the biological matrix is excellent. Estrogens were detected using a UV-detector (280 nm) or a spectrofluorimetric detector (λexc=280nm, λem=312 nm). The latter detection system has been used for the determination of estrogens in the urine of non-pregnant women. The procedure is simple and can be used in clinical practice.
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    URL: http://dx.doi.org/10.1007/BF02290331
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    Convergence of retention for small solutes in reversed-phase liquid chromatography (1994)
    Springer
    Chromatographia 38 (1994), S. 158-162 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase chromatography ; Retention mechanism ; Retention convergence ; Small molecules
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary It is shown theoretically that when the concentration of organic solvent in the mobile phase increases, or solute size decreases, log k′ values of small solutes in reversed-phase liquid chromatography (RPLC) will tend to have a minimum value called the convergence point. A theoretical model for evaluating the convergent coordinates of small solutes is presented by using a stoichiometric displacement model for retention (SMDR). The physical meaning of the coordinates of each kind of convergence are also elucidated. The convergence points have either two-dimensional coordinates with a common ordinate (the logarithm of the phase ratio of the column, log φ) or threedimensional corrdinates with two common axes: — log φ and the logarithm of the molar concentration of the pure displacing agent in mobile phase, log aD. The other axis relates to the nature of the solutes, such as carbon number of a homolog, van der Waal's surface area, hydrophobic fragment constant etc. for the latter and those and/or concentration axis for the former. The model was tested with published data and found to give a good fit.
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    URL: http://dx.doi.org/10.1007/BF02290329
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    CP/MAS NMR investigations of silica gel surfaces modified with aminopropylsilane (1994)
    Springer
    Chromatographia 38 (1994), S. 283-290 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemically bonded phase (CBP) ; Silica-gel with aminopropylsilyl ligands ; Physico-chemical characterization ; CP/MAS NMR investigation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Aminopropyl chemically bonded phases for high performance liquid chromatography (HPLC) have been prepared using mono- and trifunctional methoxyor ethoxysilanes. Three types of silica gel with different surface characteristics were used as support for the chemically bonded phases (CBPs). Surface characteristics of the packings before and after chemical modification were determined by porosity parameters, elemental analysis and CP/MAS NMR spectroscopy.29Si and13C CP/MAS NMR investigations gave informations about different interactions between aminosilyl ligands and/or these ligands and/or water molecules condensed in the pores of the silica gel surface. With decreasing pore diameter of the silica gel the proportion of protonated aminopropyl ligand increases.
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    URL: http://dx.doi.org/10.1007/BF02269769
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    The application of ‘Z’-shaped UV cells in open-tubular capillary column liquid chromatography (1994)
    Springer
    Chromatographia 38 (1994), S. 313-316 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Open-tubular capillary columns ; ‘Z’-shaped UV cells ; Solvent make-up
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary ‘Z’-shaped UV cells for packed capillary columns cannot be used in open-tubular capillary column liquid chromatography (OT-LC) because of their relatively large volume. With post-column solvent make-up, a commercial ‘Z’-shaped cell (volume 100 nl) was used in our OT-LC system, resulting in 9-fold sensitivity increase against on-column UV detection and with little efficiency loss. A small volume (5 nl) ‘Z’-shaped cell allows the direct coupling of the cell to high efficiency columns. For dilute samples, 9-19-fold sensitivity enhancement could be obtained. However, column efficiency decreases with increasing signal level as a result of peak deformation.
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    URL: http://dx.doi.org/10.1007/BF02269773
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    Interconversion of cyclosporin molecular form inducing peak broadening, tailing and splitting during reversed-phase liquid chromatography (1994)
    Springer
    Chromatographia 38 (1994), S. 359-364 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Cyclosporin ; Reversible conversion ; Activation energy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Reversed-phase liquid chromatography of cyclosporin A, a peptide immunosuppressant, at various temperatures produced remarkably different chromatograms. At 60°C one sharp peak was obtained, at 23°C this became a single broad peak and between 15° and 0°C this became one high sharp peak followed by a tailing or low plateau. Remarkably different chromatograms were produced also by varying the mobile phase flow-rate. The effects of both temperature and flow-rate on the chromatogram could be accounted for by interconversion between two forms of the cyclosporin molecule. Kinetic analysis showed that one form was converted by first-order kinetics with a half-life of 2.0 min at 20°C and that the apparent activation energy for the conversion was about 18 kcal/mol. The other two immunosuppressants, cyclosporin C and D, were also shown to undergo interconversion. This kinetic analysis of the interconversion should be helpful in clarifying the relationship between molecular structure and activity of the immunosuppressants.
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    URL: http://dx.doi.org/10.1007/BF02269781
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    Determination of carbendazime in lettuce samples by SFE-HPLC (1994)
    Springer
    Chromatographia 38 (1994), S. 395-399 
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    ISSN: 1612-1112
    Keywords: Supercritical fluid extraction ; Column liquid chromatography ; Carbendazime analysis ; Vegetable samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An SFE-HPLC method for the determination of carbendazime in lettuce leaves is described. The method involves a prior lyophilization of the sample and subsequent extraction with supercritical carbon dioxide containing methanol. The extraction conditions are as follows: amount of lyophilized sample, 1 g; CO2 density, 0.75 g/ml; temperature, 50 °C; flow-rate, 1.8 ml/min; dynamic extraction time, 25 min. Carbendazime is determined with an octadecylsilane column, an acetonitrile/water 30∶70 mobile phase and fluorescence detection at 285/317 nm. Carbendazime recoveries from spiked samples were all close to 100%. A comparison with the results from a conventional method for the determination of carbendazime reveals the new method to be more rapid, simple and reproducible for samples with low concentrations of analyte.
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    URL: http://dx.doi.org/10.1007/BF02269786
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    A photometric flow measurements method for characterisation of HPLC pumps (1994)
    Springer
    Chromatographia 38 (1994), S. 421-430 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Pumps ; Flow control
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The measurement of flow constancy and pulsation amplitudes of HPLC pump based on the photoconversion of malachite green leucocyanide is described. The irradiation time and hence the degree of conversion of the leucocyanide is correlated to flow fluctuations of piston driven HPLC pumps. It is possible to measure the amplitude of pulsations and determine the constancy of the flow rate. Most of the pumps show a flow stability better than ±1% measured as relative standard deviation of the flow rate under HPLC conditions (pressure drop 100 bar at 1 ml/min flow rate). The most expensive pump of those tested showed less than ±0.5% flow instability, however, this result was achieved by installation of a large-volume pulsation damper. The method described also allows flow rate measurements under FIA conditions where there is little or no pressure drop at the pump outlet.
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    URL: http://dx.doi.org/10.1007/BF02269830
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    Surface modification by calcium ions—Effect on chromatographic properties of silica (1994)
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    Chromatographia 39 (1994), S. 29-34 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Calcium modified silica ; Calcium adsorption isotherms
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The modification of silica surfaces by calcium ions has been studied by high-performance liquid chromatography. After treatment at pH 7.0 and 9.0 with calcium hydroxide, the modified silicas were characterised by physical and chemical analysis. From measurements by atomic absorption, the amount of calcium adsorbed was 650 ppm on silica modified at pH 7.0, and 4800 ppm on silica modified at pH 9.0. The amount of calcium on the modified silica was 0.574 groups nm−2 at pH 9.0 (original silica: mean pore diameter 176 Å, specific surface 279 m2 g−1, pore volume 1.23 ml g−1, mean particle size 9.8 μm). On the other hand, the amount of calcium in the original silica was 58 ppm. The separation factor, α for N-methylaniline and N,N-dimethylaniline was 5.2 on silica modified at pH 9.0, but could not be measured on silica modified at pH 7.0 and the original silica, using iso-propyl alcohol—n-hexane (0.5∶99.5) eluent.
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    URL: http://dx.doi.org/10.1007/BF02320454
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    Dual injector solvent elution and focussing technique for the on-line analysis of solid-phase extraction cartridges in HPLC (1994)
    Springer
    Chromatographia 39 (1994), S. 45-50 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Sample preconcentration ; Solid-phase extraction ; Solvent focussing ; Injection techniques
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new dual injector solvent focussing and elution technique developed for high-performance liquid chromatography (HPLC) greatly improves chromatographic efficiency for the on-line analysis of C18 solid-phase extraction (SPE) cartridges. Solutions containing three benzene homologs were used to characterize the dual injector analysis technique and to compare the chromatographic efficiency of this method with conventional SPE analysis methods. Sampling was performed off-line using a glass precolumn cartridge (3 mm i.d. × 30 mm) packed with 15–35 μm C18 silica. On-line cartridge analysis was achieved with two injection valves in either serial or parallel configuration. The injection loop of the first valve contains the eluting solvent, and the cartridge holder is connected in place of the injection loop of the second valve. When an injection is made, both valves are turned to the inject position, and the solvent plug is forced through the cartridge, focussing the analyte at the solvent front as it elutes the cartridge. Solvent focussing at the head of the column, resulting from preconditioning of the column with a small plug of water during injection, further minimizes the variance of the injection plug and improves the chromatographic efficiency. The technique has potential applications to environmental and biological fluid analysis where analyte preconcentration and resolution from the sample matrix components may be difficult with current SPE methods.
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    URL: http://dx.doi.org/10.1007/BF02320457
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    An improved method for the determination of free sphingosine in serum (1994)
    Springer
    Chromatographia 39 (1994), S. 85-90 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid phase extraction ; Carbopack B ; Free sphingosine in human plasma
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid, sensitive and selective high-performance liquid chromatographic method has been developed for the determination of sphingosine in human serum. After precipitation with methanol, the samples were extracted using Carbopack B disposable columns; the sphingosine was eluted with 0.05 M hydrochloric acid in methanol-dichloromethane (20∶80, v/v) and the extract evaporated to dryness at 40°C. The sample residue was then reconstituted with methanol and reacted with o-phthaldialdehyde reagent to produce a fluorescent compound. Separation was performed using an LC-18 column with 0.05 M phosphate buffer (pH 7)-methanol-acetonitrile (15∶80∶5, v/v) as mobile phase. Fluorescence detection was performed with excitation and emission wavelengths of 340 and 455 nm, respectively. The serum extract was re-analyzed with a cyano LC column to minimize the possibility of false positive results. The possible interference of compounds having a structure similar to that of sphingosine was evaluated. The mean recovery of sphingosine was 〉94.5%. The limit of detection of the assay was 1 ng mL−1. The between-run and within-run coefficients of variation for replicate analyses were 〈4.0% and 〈3.4%, respectively. The levels of free sphingosine in the serum of 40 normal subjects (20 male and 20 female) was investigated; the average level was 81.6±41.1 ng mL−1 (mean ±S.D.) for males and 85.5±33.7 ng mL−1 for females.
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    Analysis of thiamine in dried yeast by high-performance liquid chromatography and high-performance liquid chromatography/atmospheric pressure chemical ionization-mass spectrometry (1994)
    Springer
    Chromatographia 39 (1994), S. 91-96 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Atmospheric pressure chemical ionization-mass spectrometry ; Dried yeast ; Thiamine ; Ion-pair extraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary High-performance liquid chromatography (HPLC) and high-performance liquid chromatography/atmospheric pressure chemical ionization-mass spectrometry (HPLC/APCI-MS) have been applied to the analysis of thiamine in dried yeast. Thiamine was extracted from dried yeast with isobutanol containing sodium 1-octanesulfonate as an ion-pairing agent and determined by HPLC on a reversed phase ODS column with UV detection at 254 nm. Response was linear in the range 25–300 μg/g of thiamine in dried yeast with a coefficient of variation in the reproducibility of 8.0%. Thiamine was recovered in good yield (109.2%, n=5). Identification of the thiamine peak was obtained by the mass spectrum using the HPLC/APCI-MS system. The utility of the selected ion monitoring technique using the HPLC/APCI-MS was also investigated. The results obtained by this method are in good agreement with those obtained by the thiochrome method [1].
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    An improved high-performance liquid chromatographic determination of chlorpropamide in human plasma (1994)
    Springer
    Chromatographia 39 (1994), S. 107-109 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Drug assay ; Chlorpropamide ; Tolbutamide ; Human plasma
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Samples were extracted with dichloromethane and the organic layer evaporated to dryness. The residue was dissolved in methanol, and 10 μl aliquot injected onto the column. Tolbutamide was used as the internal standard for chlorpropamide. The UV detector response was linear over the range 0–200 μg ml−1 with a correlation coefficient of 0.999; detection limit: 0.002 μg ml−1. Within-day and between-day assay variation was generally ≤7%. No interference from endogenous constituents was observed. The utility of the method was demonstrated by determining chlorpropamide in samples from six healthy volunteers following a single oral dose of 250 mg. The procedure is simple and requires small volumes of plasma.
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    The modiffication of alumina, zirconia, thoria and titania for potential use as HPLC stationary phases through a silanization/hydrosilation reaction scheme (1994)
    Springer
    Chromatographia 39 (1994), S. 649-654 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemically bonded phases ; Non-silica based supports ; Hydrosilation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A process for bonding a monolayer of silane to the surface of alumina, zirconia, thoria and titania by reaction with the hydrolysis product of triethoxysilane is described. The hydride containing material is then further reacted with a terminal olefin in the presence of a platinum catalyst to produce a chemically modified oxide surface which could be used as a chromatographic stationary phase. The success of this reaction is monitored by diffuse reflectance infrared Fourier transform and cross-polarization magic-angle spinning nuclear magnetic resonance spectroscopy as well as by differential scanning calorimetry. On all four oxides both the hydride intermediate and the alkyl bonded product are successfully formed via the silanization/hydrosilation reaction sequence.
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    Studies of some experimental conditions for the polymerization of the continuous beds (cross-linked polyacrylamide gels) in order to improve their chromatographic properties (1994)
    Springer
    Chromatographia 39 (1994), S. 655-662 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Continuous beds ; Compressed beds ; Proteins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Continous chromatographic beds are synthesized by a simple and cost-effective procedure which does not involve the conventional, time-consuming preparation of beads. The aim of this study was to improve the flow properties of the beds by investigating how they are affected by polymerization temperature, the pH of the buffer in which the polymerization takes place, the nature of the constituents of this buffer, the concentrations of catalyst and accelerator and the concentration of the precipitating agent (ammonium sulfate). The infuence of flow rate and the time constants of the detector and recorder on peak width was also studied.
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    Reversed phase C18 packings for the separation of polycyclic aromatic hydrocarbons by high performance liquid chromatography (1994)
    Springer
    Chromatographia 39 (1994), S. 668-672 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Monomeric and oligomeric RP packings ; Preparation of RP stationary phases ; Polycyclic aromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of C18 stationary phases for the separation of polycyclic aromatic hydrocarbons has been investigated. The effect of the pore size of the silica, the endcapping procedure, the amount of reagent and the amount of water in the preparation was also examined. A good correlation between surface coverage and capacity factor was found. The maximum surface coverage available with our preparation method lies between 3–3.5 μmol m−2, slightly depending on the pore size of the silica. Oligomeric not endcapped C18 packing materials are optimal for the separation of polycyclic aromatic hydrocarbons.
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    URL: http://dx.doi.org/10.1007/BF02274581
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    Estimation of phenolic compounds in green pepper berries (Piper nigrum L.) by high-performance liquid chromatography (1994)
    Springer
    Chromatographia 39 (1994), S. 743-746 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenolic compounds ; Green pepper berries
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An HPLC method is described for the separation and estimation of phenolic compounds in six commercial varieties of green pepper berries. Among these, two phenolic compounds namely 3,4-dihydroxyphenylethanol glucoside and 3,4-dihydroxy-6-(N-ethyl amino)benzamide that served as efficient substrates for pepper phenolase, showed wide qualitative and quantitative variation in their composition within the varieties. Quantitative estimations of these two compounds were carried out using 4-methylcatechol and epinephrine as external standards. This method is suitable for the estimation of phenolic compounds in green pepper berries in one run.
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    URL: http://dx.doi.org/10.1007/BF02274592
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    Analysis of basic hair dyes by HPLC with on-line post-column photochemical derivatisation (1994)
    Springer
    Chromatographia 39 (1994), S. 138-145 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Diode array detection ; Post-column photochemical derivatisation ; Hair dyes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed phase liquid chromatographic method is proposed for the analysis of basic hair dyes (raw materials and colourant formulations). The performance of the method was enhanced by introducing post-column on-line photochemical derivatisation in combination with a Diode Array Detector. On-line photoderivatisation provided an effective way of selectively transforming the analytes to compounds with different spectral properties. For each analyte two characteristic UV-Visible spectra (photoreactor on and off) were obtained with the same mobile phase and this information in combination with the chromatographic data (k' at pH 3.0 and 4.5) enabled the unambiguous identification of both commonly used, approved, and banned basic hair dyes. Additionally, this approach was found useful to improve the method sensitivity, allowing the determination of analytes present in low concentration (0.03%) in complex commercial formulations.
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    URL: http://dx.doi.org/10.1007/BF02274492
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    Control of adsorption and solubility in gradient high performance liquid chromatography. Part 4. Sudden-transition gradient elution of styrene/ethyl methacrylate copolymers in reversed phase mode (1994)
    Springer
    Chromatographia 39 (1994), S. 170-174 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Copoly(styrene/ethyl methacrylate) ; Gradient elution ; Precipitation chromatography of polymers ; Solubility of polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Copolymers from styrene and ethyl methacrylate have been separated according to composition byn-heptane gradients on a C18 bonded phase after injection into acetonitrile and subsequent sudden transition to a concentration of either dichloromethane or tetrahydrofuran between 30 and 50% or 20 and 50%, respectively. Acetonitrile is a polar non-solvent for the copolymers under investigation and ensures proper retention of the samples on a non-polar stationary phase. Dichloromethane and tetrahydrofuran are good solvents of moderate polarity. The addition of, e.g., 30 vol% of one of these solvents increased the dissolution power of the starting eluent but not to the extent necessary for elution. The latter was achieved by the addition ofn-heptane, which is a non-solvent for the polymers investigated. Thus, its eluting power must be understood as the consequence of its modifying effect on the polarity of the eluent mixture. The higher the content of copolymer in ethyl methacrylate the earlier it was eluted. Since acetonitrile andn-heptane are only partly miscible, phase diagrams were measured after the addition of either tetrahydrofuran or dichloromethane as a third component. Homogeneous mixtures were obtained on addition of about 30% solvent (one of both of the latter).
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    On-line trace enrichment — column liquid chromatography of polar pollutants in surface water using bifunctional membrane-based extraction-disk cartridges (1994)
    Springer
    Chromatographia 39 (1994), S. 239-245 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Membrane-extraction disks ; On-line trace enrichment ; Polar pollutants ; Surface water
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An on-line trace-enrichment system, using a bifunctional membrane extraction-disk cartridge, has been combined with a column liquid chromatography separation for the simultaneous determination of basic, neutral and acidic pollutants in surface water. The enrichment device consisted of a specially constructed holder containing both C-18 and cation-exchange disks. The holder can contain up to 25 disks of 0.5 mm thickness and 4.6 mm diameter. Before trace enrichment of 20 ml of surface water (pH 3.0), calcium ions were removed from the sample by means of an oxalic acid precipitation. Desorption of the cartridge was at elevated temperature using reversed-phase gradient elution; detection was performed with a diode-array UV absorbance detector. The detection limits for the test compounds in surface water are typically 0.5–2 μg/l; the calibration graphs are linear from the lower limit of determination up to 50 μg/l.
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    URL: http://dx.doi.org/10.1007/BF02274506
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    Retention characteristics of fluorinated bonded silica phase in reversed-phase liquid chromatography (1994)
    Springer
    Chromatographia 39 (1994), S. 285-293 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fluorinated chemically bonded silica ; Aromatic compounds ; Molecular shape vs. retention
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Fluorinated bonded silica has been evaluated as a packing material in reversed-phase liquid chromatography (RPLC) with polycyclic aromatic hydrocarbons, chlorinated benzenes and substituted benzenes as sample probes. The bonded material is useful as a reversed-phase stationary phase and for polar compounds it offers a specific selectivity not found with octadecylsilica (ODS) phases. The phase also retains non-planar compounds more than planar molecules. The results can be explained by conformational differences between ODS and the fluorinated bonded phase by MM2 calculation.
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    URL: http://dx.doi.org/10.1007/BF02274515
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    Optimization of mobile phases for HPLC of cis-trans carotene isomers (1994)
    Springer
    Chromatographia 39 (1994), S. 346-354 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; α-Carotene cis-isomers ; β-Carotene cis-isomers ; Polymer stationary phase
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Various methanol-based, binary and ternary solvent systems were compared with respect to resolution of cis isomers of α and β-carotene by reversed-phase HPLC. A ternary system: acetonitrile-methanol-methylene chloride (75∶15∶10), or a binary system: acetonitrilemethanol (90∶10 or 5∶95) provided the best separation of β-carotene and its four cis isomers, 9-cis, 13-cis, 15-cis and 13,15-di-cis-β-carotene. The elution order of 9-cis and 13-cis-β-carotene was dependent on the methanol concentration. Methanol-methylene chloride (99∶1) resolved α-carotene and its three cis isomers, 9-cis, 13-cis, and 15-cis-α-carotene. It also proved the best for simultaneous separation of cis isomers of α and β-carotene. Sample solvent can affect the separation efficiency of each isomer. The presence of cis isomers of α and β-carotene in fresh and cooked carrots was also determined.
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    Chromatographic determination of D-amino acids as native constituents of vegetables and fruits (1994)
    Springer
    Chromatographia 39 (1994), S. 419-426 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Chirasil-Val ; Amino acid enantiomers ; N-Isobutyryl-cysteine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Free D-amino acids (D-AA) were detected as native constituents in juices of vegetables (cultivars of cabbage, tomato, carrot, garlic) and fruits (organes, clementine, grapefruit, lemon, apples, pear, grapes) using gas chromatography (GC) or high-performance liquid chromatography (LC). For investigation by GC, AA enantiomers were converted into theirN(O)-pentafluoropropionyl 2-propyl esters and resolved on a Chirasil-L-Val capillary column. For determination by LC, precolumn derivatization of AA enantiomers usingo-phthaldialdehyde together with the chiral thiolsN-isobutyryl-L-cysteine orN-isobutyryl-D-cysteine and fluorescence detection of the diastereomeric isoindole derivatives, resolvable on an octadecylsilyl stationary phase, were used. D-Ala (0.6–3.8%) was detected in all freshly pressed plant juices usually in the highest relative amounts. Other D-AA detected were D-Asx (0.1–1.9%), D-Glx (0–1.3%), D-Ser (0–1.7%), D-Arg (0.4–1.2%, in grapes, orange, grapefruit, and clementine) and D-Leu and D-Val (1% in cabbage). Absolute amounts of native D-AA were totally 28–57 μmol L−1 in fruit juices, 14.5 μmol L−1 in a tomato juice and 8.5 μmol L−1 in a carrot juice.
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    Temperature effect in separation of fullerene by high-performance liquid chromatography (1994)
    Springer
    Chromatographia 39 (1994), S. 453-459 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fullerenes ; Octadecylsilicas ; Temperature effect
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The effect of column temperature, especially at low temperatures, on the separation of fullerenes on monomeric and polymeric octadecyl silica (ODS) bonded phases has been studied. Decreasing the column temperature induces an increase in selectivity. The best temperature for the separation of fullerenes was determined for both types of ODS phase with n-hexane eluent. The selectivity for higher fullerenes on monomeric phases becomes similar to that on polymeric phases to low temperature. It has been found that as the carbon content of monomeric phases is increased, the selectivity also becomes similar to polymeric phases.
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    A chromatographic and chemometric study of the bark phenolic compounds of two poplar clones with different resistance toDiscosporium populeum (1994)
    Springer
    Chromatographia 39 (1994), S. 481-489 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenolic compounds ; Poplar bark ; Discosporium populeum infection ; Chemometric data evaluation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Reversed-phase high performance liquid chromatography with diode array detection was used to analyze phenolic compounds contained in bark extracts of two different poplar clones known to have different resistance toDiscosporium populeum infection. Statistical treatments both monovariate and multivariate were applied to the results in order to identify regularities useful to discriminate the polar resistance and to check the importance of seasonal and cultivation site related factors. For the two clones examined phenolic compounds showed great discrimination ability not influenced by either sample collection period or cultivation site.
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    URL: http://dx.doi.org/10.1007/BF02278766
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    Determination of catecholamines in urine by micellar liquid chromatography with coulometric detection (1994)
    Springer
    Chromatographia 39 (1994), S. 591-596 
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    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micellar liquid chromatography ; Catecholamines in urine ; Coulometric detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The determination of catecholamines by HPLC with a sodium dodecyl-sulphate (SDS), micellar mobile phase on a C18 column and with coulometric detection was studied. The eluate was conditioned at +0.25 and +0.00 V, and the current at −0.16V was recorded. A previously developed model which describes the chromatographic behaviour of solutes in HPLC with hybrid, micellar mobile phases was used to optimize the SDS and ethanol concentrations. A mobile phase of 0.15M SDS in a phosphate buffer of pH 3.4 and without ethanol is recommended. The limits of detection were 0.4–0.7 ng ml−1. The procedure was applied to the determination of unconjugated L-dopa, norepinephrine and dopamine in urine. Direct injection of the urine samples gave high results but the unconjugated catecholamines could be determined with a single solid-phase extraction step on an alumina column.
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    Improved separation of diastereoisomers in capillary electrophoresis using a mixture of β-cyclodextrin and sodium taurodeoxycholate (1994)
    Springer
    Chromatographia 39 (1994), S. 627-630 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micellar electrokinetic capillary electrophoresis ; Tetrahydrocarbazole derivatives ; β-Cyclodextrin ; Taurodeoxycholate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary 2,3,4,6-tetra-O-acetyl-β-D-glucopranosyl isothiocyanate derivatives of a number of basic compounds, containing one chiral center, have been prepared. The indirect resolution of enantiomers was achieved with a high separation efficiency by capillary electrophoresis, using a sodium taurodeoxycholate/β-cyclodextrin system. This methodology was found to be superior to the resolution of the same derivatives by reversed phase HPLC analysis. A possible mechanism for stereoselectivity is described.
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    Progress in the research of artemisinin-related antimalarials: An update (1994)
    Springer
    Pharmacy world & science 16 (1994), S. 169-180 
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    ISSN: 1573-739X
    Keywords: Antimalarials ; Artemisia annua L ; Artemisinin ; Biosynthesis ; Chemistry ; Clinical trials ; Pharmacology ; Phytochemistry ; Sesquiterpenes ; Toxicology
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Artemisinin, a sesquiterpene lactone endoperoxide isolated fromArtemisia annua L., and a number of its semisynthetic derivatives have shown to possess antimalarial properties. They are all eflective againstPlasmodium parasites that are resistant to the newest and commonly used antimalarial drugs. This article gives a survey of the literature dealing with artemisinin-relaled antimalarial issues that have appeared from the end of 1989 up to the beginning of 1994. A broad range of medical and pharmaceutical disciplines is covered, including phytochemical aspects like the selection of high-producing plants, analytical procedures, and plant biotechnology. Furthermore, the organic synthesis of artemisinin derivatives is discussed, as well as their mechanism of action and antimalarial activity, metabolism and pharmacokinetics, clinical studies, sideeffects and toxicology, and biological activities other than antimalarial activity.
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    Response of root mRNA population to sulphate shortage in maize seedlings (1994)
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    Plant and soil 162 (1994), S. 309-313 
    Details
    ISSN: 1573-5036
    Keywords: in vitro translation ; maize ; nutrient stress proteins ; Poly(A)+RNA ; sulphate deprivation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Roots of ten-days-old seedlings obtained from a maize hybrid grown in complete or in sulphate-deprived medium were used to extract Poly(A)+RNA. The response to sulphate deprivation, which is known to increase the uptake capacity up to ten times, was manifested also by the expression of three mRNA species, as shown by the in vitro translation of the mRNA population. One hour after transfer to complete nutrient medium all three mRNAs were still present.
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    Plagiogravitropism of maize roots (1994)
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    Plant and soil 165 (1994), S. 327-332 
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    ISSN: 1573-5036
    Keywords: gravitropism ; maize ; nodal roots ; plagiogravitropism ; seminal roots ; Zea mays L.
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract The direction of root growth can be studied by analyzing the trajectories of roots growing in soil. Both the primary seminal root and nodal roots of maize attain a preferred, or liminal, angle of growth that deviates from the vertical. These roots are said to be plagiogravitropic. Experiments using plants grown in soil-filled boxes revealed that the primary seminal root is truly plagiogravitropic. It shows both positive and negative gravitropism in response to gravity stimuli and tends to maintain its direction even after growing around obstacles. These are experimental results suggesting that plagiogravitropic growth is controlled by internal factors. The orientation of the grain affects the establishment of the liminal angle of the primary seminal root, and both the position of their node of origin and the root diameter are closely related to the plagiogravitropic behaviour of nodal roots. Several external factors are also known to influence plagiogravitropism. Low soil water content causes a decrease in the angle of growth and soil mechanical resistance suppresses the gravitropic curvature. Plagiogravitropic behaviour of both seminal and nodal roots plays a significant role in shaping the root system.
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    Genetic and environmental effects on abscisic acid accumulation in leaves of field-grown maize (1994)
    Springer
    Euphytica 78 (1994), S. 81-89 
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    ISSN: 1573-5060
    Keywords: abscisic acid ; inheritance ; drought stress ; Zea mays ; maize
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary This study analyzes the components of phenotypic variation for abscisic acid (ABA) content in maize (Zea mays L.) leaves and the correlations with drought sensitivity index (DSI) and silk delay (SD), involved in the reaction to water deficit. Eight early- and seven medium-maturity inbreds were examined in field trials: in 1990 with low irrigation volume and in 1991 with low and high irrigation volumes. ABA concentration and DSI were investigated at growth stages (S) corresponding to stem elongation (S3), appearance of the first husks (S4), and mid-end of silking (S5). The ABA concentration was significantly higher in conditions of water deficit and in the later growth stage. The genetic component for ABA concentration attained higher relative values than those shown by DSI in the same growth stages and by SD; moreover, it increased from growth stage 3 to stage 5. The genotype × year and genotype × irrigation volume interactions were smaller for ABA concentration than for DSI and SD. The broad sense heritability on a plant basis, estimated in drought conditions, for ABA concentration ranged from 21.4 to 55.1% according to maturity group and growth stage. A wide variation was observed among lines for ABA concentration: the medium-maturity group showed a three-fold range (from 219 to 605 ng ABA g−1 dry weight). No clear relationships between ABA concentration, DSI and SD were found. These results indicate the feasibility of a selection for ABA concentration within segregating populations derived from crosses between the inbred lines herein tested.
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    Feedback control of gene expression (1994)
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    Photosynthesis research 39 (1994), S. 427-438 
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    ISSN: 1573-5079
    Keywords: acetate ; glucose ; maize ; metabolic repression ; photosynthetic genes ; transcription regulation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Although feedback regulation of photosynthesis by carbon metabolites has long been recognized and investigated, its underlying molecular mechanisms remain unclear. The recent discovery that glucose and acetate trigger global repression of maize photosynthetic gene transcription provides the first direct evidence that a fundamental mechanism is used for feedback regulation of photosynthesis in higher plants. The metabolic repression of photosynthetic genes has now been found in many higher plants and is likely universal. It overrides other regulation by light, tissue type and developmental stage, and serves potentially as the molecular basis of interactions between sink and source tissues. Using simplified and convenient cellular systems and transgenic plants, the study of metabolic regulation of gene expression offers an excellent opportunity for the understanding of global and coordinate gene control and metabolite-mediated signal transduction in higher plants.
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    Evaluation of parameters describing the root system architecture of field grown maize plants (Zea mays L.) (1994)
    Springer
    Plant and soil 164 (1994), S. 155-167 
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    ISSN: 1573-5036
    Keywords: axile roots ; maize ; nodal roots ; root length ; root system ; seminal roots ; Zea mays L.
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract The objective of this work was to study elongation curves of maize axile roots throughout their elongation period under field conditions. Relationships between their elongation rate and the extension rate of their branched region were also studied. Maize, early-maturing cultivar Dea, was grown on a deep, barrier-free clay loam (depth 1.80m). Trenches were dug during four periods until after silking and axile roots were excavated. Parameters measured were total length and the lengths of basal and apical unbranched zones. The rank of the bearing phytomer and general data about the carrying plant were also recorded. Results showed that axile roots from lower phytomers had similar elongation rates irrespective of the rank of the carrying phytomer. This elongation rate declined with root age. A monomolecular elongation model was fitted to the experimental data. Elongation was much slower in roots from upper phytomers. A rough linear relationship was found between the elongation rate of axile roots and the length of the apical unbranched zone. This result suggests that laterals appeared on a root segment a constant time after it was formed. Possible mechanisms with may account for the declining elongation rate with root age (increasing distance from aerial parts or adverse environmental conditions in deep soil layers) and variability between individual roots are also discussed.
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    Evaluation of parameters describing the root system architecture of field grown maize plants (Zea mays L.) (1994)
    Springer
    Plant and soil 164 (1994), S. 169-176 
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    ISSN: 1573-5036
    Keywords: branching ; growth ; lateral roots ; maize ; root morphology ; Zea mays L.
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract The architecture of the root system is related to its water and mineral uptake. In this paper, the number, growth, and branching of first-order lateral roots are studied on field grown maize (early maturing cultivar ‘Dea’), mainly in relation to the depth and to the rank of the bearing phytomer. The soil was a deep clay loam, without any barrier until 1.80 m. The branching density was studied along axile roots until 1.40 m from the base, on a sample of individually excavated axile roots. A strong gradient of density was shown: the mean branching density decreased from 12 roots.cm−1 near the base to 4 roots.cm−1 at a 60 cm depth. Seminal roots were less densely branched than nodal roots. The mean difference was about 4 roots.cm−1. The length and branching density of lateral roots were studied on mature parts of the root systems where the growth and branching of the laterals were completed, using samples extracted from large soil monoliths. The length distribution of lateral roots was highly asymmetrical, for every source phytomer (mean: 25 mm; median: 16 mm). Many lateral roots were very short, and only 2 % reached a length higher than 10 cm. Only 29 % of all the laterals bore second-order lateral roots. Vigorous laterals branched more systematically and more profusely: the branching density varied from 2 to 5 roots.cm−1 according to the length of the mother lateral root. Both the number and length of lateral roots appeared to be affected by the soil bulk density which varied with the depth.
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    Amino-acid influx at the soil-root interface of Zea mays L. and its implications in the rhizosphere (1994)
    Springer
    Plant and soil 163 (1994), S. 1-12 
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    ISSN: 1573-5036
    Keywords: amino-acids ; maize ; rhizosphere ; root exudates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract The aim of the study was to investigate the ability of intact Zea mays. L. roots to regulate the amount of free amino-acids present in the rhizosphere. Using metabolic inhibitors it was demonstrated that the release of amino-acids from the root occurred by passive diffusion, whilst free amino-acids outside the root could be re-captured by an active transport mechanism. The influx of amino-acids into the root was shown to be relatively independent of spatial location along the root and was little affected by the presence of other organic compounds in solution. It was deduced from root concentration gradients that the main site of amino-acid exudation was at root tips. Amino-acid uptake by the root was shown to be independent of both inorganic-N concentration and the presence of other organic solutes in solution. A computer simulation model was constructed to assess the contribution of organic-N uptake (acidic, basic and neutral amino-acids) to the plant's N budget, in comparison to the inorganic solutes NO3 and NH4. Simulations of N uptake from a 0.5 mm radius rhizosphere indicated that when inorganic-N concentrations in soil were limiting (≤0.1 μmoles cm-3 soil), the uptake of amino-N accounted for up to 90% the total N taken up by the roots. In situations where fertilizer inputs are high, and levels of organic matter in soil are low, the contribution of amino-N might still be expected to form 〈30% of the total N taken up by the root system. It was concluded that the uptake of amino-acids from the rhizosphere may be important in both N nutrition and in the minimization of root C and N losses to the soil. Consequently this may be important in governing the size of the rhizosphere microbial population.
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    Light differentially regulates lateral and longitudinal auxin transport in the mesocotyl of etiolated maize seedlings (1994)
    Springer
    Plant growth regulation 14 (1994), S. 167-171 
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    ISSN: 1573-5087
    Keywords: auxin-transport ; indoleacetic acid ; maize ; photoinhibition ; transport ; Zea mays
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract The uptake of IAA into excised mesocotyls of non-irradiated maize seedlings was linear up to a concentration of about 4×M and in this range there was a tight coupling between the IAA in the stele and the cortex. Prior irradiation with white light of intact seedlings unbalanced this coupling. Lateral and longitudinal transport were affected differently. In the stele, the effect of prior irradiation on longitudinal transport was multiphasic, with an initial stimulatory effect followed by a negative effect at longer prior irradiation times. The lateral transport from the stele to the cortex showed no stimulatory effect and appeared to be inhibited within at least 15 min. The effect of the prior irradiation on longitudinal transport in the stele appeared to be a high intensity effect. In contrast, the effect of the prior irradiation on the lateral transport from the stele to the cortex was saturated at much lower intensities. The data suggest that the light induced change in the lateral transport of IAA between the two tissues may be due to changes either in the number of open lateral transport channels/carriers or in the conductivity of these channels/carriers.
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    Comparative isozyme polymorphisms of north American eastern gamagrass,Tripsacum dactyloides var.dactyloides and maize,Zea mays L. (1994)
    Springer
    Genetica 94 (1994), S. 77-83 
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    ISSN: 1573-6857
    Keywords: isozymes ; Tripsacum ; maize ; wide hybridizations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Random samples, consisting of at least 100 individual seedlings, were taken from the diploid (2n=2x=36) eastern gamagrass (Tripsacum dactyloides var.dactyloides) and assayed to determine which of 12 enzyme marker loci and isozyme systems would be most informative in providing satisfactory resolution of both maize andTripsacum isozyme systems. For comparison, eight maize inbreds were included in the study to aid evaluation and comparison of the various isozyme systems. In addition, evaluations were conducted to identify if the identified optimum isozyme system could be used to detectTripsacum introgression in maize following a maize ×Tripsacum backcrossing scheme. Using the established isozyme techniques for maize (Zea mays L.), theAdh, Pgd, Cat, Est, B-Glu, Got, Idh, Tpi isozyme systems detected no polymorphism among theTripsacum individuals assayed. TheEst andB-Glu systems forTripsacum were unscorable due to poor staining and resolution. TheAcp, Mdh, Pgm, andPhi isozyme systems were found to be satisfactory markers for differentiating between eastern gamagrass individuals as well as detectingTripsacum introgression in maize. The availability of useful isozyme systems which can simultaneously provide significant isozyme resolution of maize,Tripsacum and maize-Tripsacum backcross hybrids, on a single gel system, will be useful for the detection of marker assistedTripsacum introgression into maize. In addition, the identification of a set of variable biochemical markers should also assist breeding, selection and genetic manipulations in eastern gamagrass.
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    URL: http://dx.doi.org/10.1007/BF01429223
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    Light inducibility and tissue specificity of theR gene family in maize (1994)
    Springer
    Genetica 94 (1994), S. 225-234 
    Details
    ISSN: 1573-6857
    Keywords: anthocyanin ; maize ; helix-loop-helix ; tissue specificity ; paramutation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The red and purple anthocyanin pigments of plants are visible genetic markers and their spatial and temporal accumulation is strictly regulated. Anthocyanin biosynthesis is also modulated by environmental factors such as light and temperature. Thus this process represents an appealing model system for the study of gene regulation, as well as for studying developmental biology. In maize, the pattern of pigmentation of the plant is controlled by theR, Sn andB genes, a small family of HLH transcription factors. Here we report the pattern of light induction and tissue specific expression of the regulatory and structural genes involved in this biosynthesis. TwoSn alleles differing in their light response have been considered and analyzed by Northern andin situ hybridization experiments. An unusual phenomenon of interaction between the homologousR andSn genes leading to a partial gene silencing is reported. We hypothesize a model in which silencing is achieved through methylation of specific sites.
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    URL: http://dx.doi.org/10.1007/BF01443436
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    Microbiological changes in mawè during natural fermentation (1994)
    Springer
    World journal of microbiology and biotechnology 10 (1994), S. 410-413 
    Details
    ISSN: 1573-0972
    Keywords: Enterobacteriaceae ; fermentation ; lactic acid bacteria ; maize ; mawè ; yeast
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Abstract Lactic acid bacteria increased from 3.2 × 106 and 1.6 × 107 c.f.u./g (wet wt) to 2 × 109 and 1.6 × 109 c.f.u./g after 12 to 24 h of fermentation of home-produced mawè (a dough produced from dehulled maize) and commercial mawè, respectively. In commercial mawè, the yeast count increased from 1.3 × 105 to 2.5 × 107 c.f.u./g after 48 h of fermentation before decreasing, whereas in the home-produced mawè it increased from 2.5 × 104 to 3.2 × 107 c.f.u./g after 72 h of fermentation; the dominant yeasts were mainly Candida krusei, although C. kefyr, C. glabrata and Saccharomyces cerevisiae were also present. Enterobacteriaceae counts increased slightly during the initial stage ofthe fermentation, but decreased below the detection level after 24 to 48 h. Enterobacter cloacae was mostly found in commercial mawè and Escherichia coli mostly in homeproduced mawè.
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    URL: http://dx.doi.org/10.1007/BF00144462
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    Alley cropping and mulching withErythrina poeppigiana (Walp.) O. F. Cook andGliricidia sepium (Jacq.) Walp.: effects on maize/weed competition (1994)
    Springer
    Agroforestry systems 25 (1994), S. 119-134 
    Details
    ISSN: 1572-9680
    Keywords: alley cropping ; Erythrina poeppigiana ; Gliricidia sepium ; weeds ; maize ; mulch ; weed competition ; weed reduction potential
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract The potential of allye cropping systems to sustain a high productivity with low external inputs and the reduction of maize/weed competition through weed suppression in different alley cropping and sole-cropped mulched systems was studied in Costa Rica at CATIE. Data were recorded eight years after establishment of the experiment. Plant residues ofErythrina poeppigiana trees (10 t/ha dry matter) planted at 6 by 3 m reduced weed biomass by 52%, whileGliricidia sepium trees (12 t/ha dry matter) planted at 6 by 0.5 m reduced weed biomass by 28%, in comparison to controls.Erythrina had a considerable impact on grass weeds, whileGliricidia reduced the incidence of some dicot weeds. Weed competition significantly reduced maize yield in all systems. Nevertheless weed suppression contributed to the higher maize grain yield underErythrina andGliricidia alley cropping of 3.8 t per hectare as opposed to the unmulched control yield of 2.0 t per hectare.
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    URL: http://dx.doi.org/10.1007/BF00705672
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    Evaluation of phytotoxic effects ofGliricidia sepium (Jacq.) Walp prunings on maize and cowpea seedlings (1994)
    Springer
    Agroforestry systems 26 (1994), S. 249-254 
    Details
    ISSN: 1572-9680
    Keywords: phytotoxicity ; cowpea ; Gliricidia sepium prunings ; maize ; seedlings
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Phytotoxic effects ofGliricidia prunings were tested on maize seedlings in the laboratory and on maize and cowpea seedlings in the field. In the laboratory test, growth of maize seedlings was significantly depressed by addition of leachate ofGliricidia prunings. In the field, leaf, chlorosis of maize and cowpea seedlings occurred when mulched withGliricidia prunings; number of affected leaves increased with increasing mulch rate. Maize was more susceptible than cowpea. This phytotoxic effect, however, did not reduce growth of maize and cowpea seedlings in the field. ApplyingGliricidia mulch one week before planting eliminated the phytotoxic effects on maize.
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    URL: http://dx.doi.org/10.1007/BF00711214
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    The effects of alley cropping withLeucaena leucocephala and of different management practices on the productivity of maize and soil chemical properties in lowland coastal Kenya (1994)
    Springer
    Agroforestry systems 27 (1994), S. 31-51 
    Details
    ISSN: 1572-9680
    Keywords: alley cropping ; leucaena mulch ; dairy cattle slurry ; maize ; cowpea ; lowland coastal tropics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract The effects of leucaena hedgerows, mulching with leucaena foliage (0,50 and 100% of harvested foliage), cowpea intercropping and adition of dairy cattle slurry (55 t ha−1 per maize crop) on the yield of maize from a sandy soil were assessed. The four-year results from five maize crops are reported. Except in the first year, yields of maize grain and stover were significantly reduced by 30% in the presence of leucaena hedgerows. Use of leucaena mulch eliminated this effect; application of all the harvested leucaena mulch (100%) increased the total maize grain yield of the five crops by 44% over sole maize. Hedgerow and mulching management required an additional 36 mandays labour ha−1 which was more than compensated by the increased maize yields. Furthermore leucaena hedgerows substantially depressed the growth of weeds between cropping seasons. Intercropping with cowpea significantly depressed yields of maize grain and stover when both crops were sown together, but not in later seasons when cowpea was sown four weeks after the maize. Application of slurry increased the total yields of maize grain and stover by 35 and 37%, respectively. The grain yield of maize in leucaena hedgerow treatments fertilized with slurry did not respond to application of more than 50% of leucaena foliage, which suggested that half of the foliage could be spared for feeding to livestock. The cumulative yield of maize grain from the highest yielding organic system was 85% of the yield from the fertilizer treatment. The study, which is continuing, demonstrates that large increases in agricultural productivity are possible through the intercropping of maize with woody forage and grain legumes and the integration of dairy cattle production into the system. It thus shows the importance of exploiting crop/livestock interactions.
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    URL: http://dx.doi.org/10.1007/BF00704833
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    Relationships among American and Spanish populations of maize (1994)
    Springer
    Euphytica 79 (1994), S. 149-161 
    Details
    ISSN: 1573-5060
    Keywords: maize ; germplasm ; cluster analysis ; landraces ; Zea mays
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary Two experiments were carried out with two objectives. First, to establish the phenetic relationships among the maize (Zea mays L.) landraces from Galicia (Northwestern Spain) maintained at the Misión Biológica de Galicia. Second, to assess the resemblance between a collection of Spanish populations (including the landraces from Galicia) and a set of US Corn Belt varieties. For the first objective 73 varieties from Galicia, along with 9 hybrid checks, were grown in 9×9 simple lattices at two locations for two years. For the second objective 131 populations from the US Corn Belt and Spain, along with 9 hybrid checks, were grown for three years in unreplicated experiments. Cluster analyses were carried out with the first principal components that accounted for a significant amount of the total variation. Four groups were found among the landraces from Galicia. The populations from Spain and America were classified as belonging to nine main groups. The replicated experiment was more accurate than the unreplicated one. However, it is concluded that an unreplicated test grown in several environments is accurate enough to detect the main groups, although some inaccuracies should be expected.
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    URL: http://dx.doi.org/10.1007/BF00023586
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    Genetic variation for resistance to low-temperature photoinhibition of photosynthesis in maize (Zea mays L.) (1994)
    Springer
    Euphytica 80 (1994), S. 85-93 
    Details
    ISSN: 1573-5060
    Keywords: maize ; Zea mays ; photoinhibition ; photosynthesis ; low-temperature adaptation ; breeding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary Sixty-seven inbred lines of maize were evaluated for resistance to low-temperature photoinhibition of photosynthesis, using a pulse-modulated chlorophyll fluorescence technique. The evaluation procedure was based on leaf discs, which were exposed to a high irradiance (1000 µmol/m2/s) at 7°C. The efficiency of open PSII reaction centres as a reflection of overall photosynthesis was measured before and after a photoinhibition-inducing treatment. Exposure of leaf discs to photoinhibitory condition for 2, 4, and 8 hours resulted in an efficiency reduction of 30, 53 and 83%, respectively. Testing of inbred lines showed large differences for photoinhibition susceptibility. The difference in photosynthetic efficiency between the most extreme lines after a treatment of eight hours was 39%. Resistance to photoinhibition was shown to be relevant under cool field conditions. It proved to be a trait strongly amenable to selection.
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    URL: http://dx.doi.org/10.1007/BF00039302
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    Response of vesicular-arbuscular mycorrhizas of maize to various rates of P addition to different rooting zones (1994)
    Springer
    Plant and soil 158 (1994), S. 119-128 
    Details
    ISSN: 1573-5036
    Keywords: maize ; P placement ; P supply ; rooting zone ; VAM colonization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Colonization of plant roots by vesicular-arbuscular mycorrhizal fungi is known to be reduced as the phosphorus nutrition of the plant is increased. It is generally accepted that the concentration of P in the plant rather than the soil regulates VAM colonization. Whether it is the shoot P concentration, the mean P concentration in the root system or the P concentration in the specific root being colonized is not known, but is of agronomic significance because fertilizer P is frequently applied in concentrated zones which would be expected to result in higher P concentration in roots growing in the fertilized zone than in the remainder of the root system. Growth chamber and field experiments were conducted to determine the effect on colonization of supplying varying amounts of P to different portions of the rooting zone. In growth chamber studies using a split-pot technique, the proportion of maize (Zea mays L.) root length containing arbuscules in a high-P zone was lower than that of roots of the same plant growing in a low- or medium-P zone. Root P concentration was higher in the high-P zone. In a field experiment conducted over a two-year period, VAM colonization of roots of young maize plants growing in fertilized soil was affected differently than that of roots growing outside the fertilized zone. A small addition of fertilizer P increased colonization of roots in the fertilized soil, but further additions resulted in an abrupt decline followed by a slower further decline, although colonization was not eliminated even by rates of 1600 μg P g-1 soil. Colonization of roots growing outside the fertilized zone declined gradually with increasing P addition but the overall decline was less than for roots in the fertilized zone. The data support the hypothesis that it is P concentration in the portion of the root system being colonized rather than the general P status of the plant which regulates VAM colonization. The agronomic implication of this is that, although a fertilizer band may reduce VAM colonization of roots in the band volume, roots growing outside this volume may be well colonized so the mycorrhizal symbiosis may be an important contributor to P nutrition.
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    URL: http://dx.doi.org/10.1007/BF00007924
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    Stably transformed cell lines from protoplasts of maize endosperm suspension cultures (1994)
    Springer
    Plant cell, tissue and organ culture 37 (1994), S. 39-46 
    Details
    ISSN: 1573-5044
    Keywords: endosperm cell culture ; maize ; protoplast ; transformation ; zeins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Protoplasts were isolated from Zea mays (L.) A69Y endosperm suspension cultures and transformed by polyethylene glycol mediated DNA uptake with chimaeric gene constructs containing β-glucuronidase (GUS) or neomycin phosphotransferase II (NPTII); GUS-expressing and Kanamycin-resistant cultures were recovered. The transformed cells showed integration of the introduced foreign genes into genomic DNA and maintained their ability to synthesize endosperm-specific reserve proteins (zeins). No deletion or rearrangement of zein genes were observed in transformed cultures. Stable transformation of cultured maize endosperm cells may therefore represent a new methodological approach for the study of the transcriptional regulation of endosperm-expressed genes.
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    URL: http://dx.doi.org/10.1007/BF00048115
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    Properties of maternal haploid maize plants and potential application to maize breeding (1994)
    Springer
    Euphytica 79 (1994), S. 13-18 
    Details
    ISSN: 1573-5060
    Keywords: Zea mays ; haploid induction ; maternal haploids ; inducer line ZMS ; maize
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary Presented are the results of a two-year study of haploid maize plants in the field. The haploids were produced with the aid of inducer line ZMS. In total, 604 and 1030 haploids were obtained and studied in the first and second years, respectively. Tassels of haploid plants were found to be almost completley sterile. Fertility of ears was studied by pollinating them with the pollen from diploid inbred lines, the cross resulting in almost all of the haploid ears carrying kernels. On average 27.4 kernels per ear of haploid plant were obtained in the first year of study and 26.3 in the second. These gave rise to normal diploid plants. This property allows genotypes selected at the level of haploid plants to be involved in breeding process. Unusual plants were found among haploids, phenotypically resembling homozygous lines. It was assumed that the plants had resulted from spontaneous chromosome doubling in haploids. The results of comparative studies of progenies of unusual plants and inbred lines derived from the same synthetic population are presented.
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    Changes in the photosynthetic light response curve during leaf development of field grown maize with implications for modelling canopy photosynthesis (1994)
    Springer
    Photosynthesis research 42 (1994), S. 217-225 
    Details
    ISSN: 1573-5079
    Keywords: photosynthesis ; leaf age ; maize
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Changes in the photosynthetic light-response curve during leaf development were determined for the fourth leaf of maize crops sown on 23 April and 10 June. Temperatures were unusually mild during late spring/early summer and neither crop experienced chilling damage. The concept of thermal time was used to take into account the effects of different temperature regimes on developmental stage, thereby enabling photosynthetic light-response data to be combined for both crops to describe the general response. Large variations in the upper asymptote (Asat) and convexity (Θ) of the light-response curve occurred during leaf development, but the maximum quantum yield of CO2 assimilation remained relatively constant throughout. Dark respiration rates showed a small but significant decrease with leaf age and generally ranged between 5 and 10% of Asat. A simple mathematical model was developed to assess the sensitivity of daily leaf photosynthesis (AL) to reductions in the Asat, Θ and the initial slope (Φ) of the light-response curve at different stages of leaf development. On bright sunny days, and at all developmental stages, AL was ca. twice as sensitive to reductions in Asat than to reductions in Φ and Θ. In overcast conditions, however, all three parameters contributed significantly to reductions in leaf photosynthesis, although the contribution of Φ was greatest during early leaf growth, while older leaves were most sensitive to depressions in Asat. The implications of these results for modelling the sensitivity of canopy photosynthesis to chill-induced photoinhibition of the light-response curve are discussed.
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    Determination of sugars by liquid chromatography with post-column catalytic derivatization and fluorescence detection (1994)
    Springer
    Chromatographia 38 (1994), S. 12-16 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carbohydrates ; Post-column fluorescence derivatization ; Post column catalytic reaction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the determination of reducing sugars such as fructose and glucose and nonreducing sugar such as sucrose by high performance liquid chromatography followed by an acidic hydrolysis and a derivatization with benzamidine has been developed. After separation of sugars on a gel column packed with a polymer-based cation exchange material (Sugar-Pak I, Waters-Millipore), the sucrose is first hydrolysed in a solid phase reactor to convert it into reducing subunits. A post-column fluorigenic reaction with benzamidine under alkaline condition allows the selective determination of both natural and converted reducing carbohydrates. This procedure has proven to be selective (fluorigenic detection) and highly sensitive (allowing detection as little as picomoles amounts), reproducible and linear over a broad range of concentrations: 5×10−4 to 1.0×10−2 M. The applicability of this method to natural matrices such as plant extracts and beverages is also described. The sugar content of a barley extract has been determined and compared with a specific enzymatic test. The determined sugar content of natural and commercial lemon juices as well as of Cola beverages has been compared with those found by the conventional LC refractive index analytical procedure. In all cases, the results were comparable and were within the experimental errors of the methods.
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    Chromatography of esculin from stems and bark ofAesculus hippocastanum L. for consecutive vegetative periods (1994)
    Springer
    Chromatographia 38 (1994), S. 766-770 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thin-layer chromatography ; Densitometry ; Spectrophotometry of extracts ; Esculin, fraxin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Coumarin glucosides, esculin and fraxin, were determined in several older and younger layers of stems ofAesculus hippocastanum L. by three methods (TLC-densitometry, TLC-extraction and spectrophotometric determinations, HPLC) during the vegetative period (May–October). Variation of their content during these months is discussed.
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    Rapid method for determination of phenylurea herbicides in milk (1994)
    Springer
    Chromatographia 38 (1994), S. 88-92 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenylurea herbicides ; Milk
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method has been developed for the determination of thirteen phenylurea herbicide residues in milk. It involves one-step solvent extraction of the milk with methanol by ultrasonication. The extract is cleaned up on an Amberchrom resin cartridge. Reversed-phase, gradient elution, high-performance liquid chromatography with UV detection at 242 nm is used to analyse the residues. The recovery of thirteen phenylurea pesticides is quantitative, ranging from 71.4% to 97.9% for the individual herbicides investigated at concentrations around 0.05 mg kg−1 and from 65.1% to 95.6% around 0.005 mg kg−1. The method is not associated with any of the emulsion problems common to conventional solvent extraction, which considerably reduce the sample clean-up process compared with existing methods.
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    Lipid class analysis by normal phase high performance liquid chromatography, development and optimization using multivariate methods (1994)
    Springer
    Chromatographia 38 (1994), S. 317-324 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Lipid class analysis ; Experimental design and optimization ; Chemometrics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A general method for the analysis of lipid classes by liquid chromatography has been developed using a multivariate optimization strategy to target optimal system conditions. The method was validated using a ruggedness test in the form of a Plackett-Burman design thereby exploring the immediate region around the optimum to ensure stable analytical conditions. Detection and quantitation were optimized by a factorial design in the light scattering detector parameters thus ensuring maximum detector response. This method was found to be suitable for a broad range of lipid sources from vegetable and animal origin, examples of the separation achieved are given for oat kernel, soybean and bovine milk lipids.
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    Determination of catecholamines as aminochromes by micellar liquid chromatography with thermal lens spectrophotometric detection (1994)
    Springer
    Chromatographia 38 (1994), S. 365-372 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micellar liquid chromatography ; Determination of catecholamines ; Aminochromes ; Thermal lens spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The determination of catecholamines (CAs) using micellar liquid chromatography with thermal lens spectrophotometric detection has been studied. CAs are oxidized with hexacyanoferrate(III) to aminochromes which are separated with a mobile phase of 0.05 M sodium dodecyl sulphate, 7% propanol and 0.03 M citrate buffer, pH 4.8, on a partially endcapped C18 column. The aminochrome-micelles and aminochrome-stationary phase association constants are evaluated. Using the 488 nm line of an Ar+ laser with 250 mW pump power the limits of detection are about 4 ng mL−1. The technique is applied to the determination of unconjugated CAs in urine using isoproterenol as internal standard.
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    Control of adsorption and solubility in gradient high-performance liquid chromatography. Part 2: Sudden-transition gradient elution of styrene/ethyl methacrylate copolymers (1994)
    Springer
    Chromatographia 38 (1994), S. 559-565 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Copoly(styrene/ethyl methacrylate) ; Gradient elution, sudden transition ; Precipitation chromatography of polymers ; Solubility of polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Copolymers from styrene and ethyl methacrylate have been separated according to composition by methanol gradients on a cyanopropyl column after injection inton-heptane and a subsequent rapid increase of dichloromethane (DCM) concentration from zero to a constant value in the range from 10 to 40%. Retention and resolution in sudden-transition gradients increased with decreasing DCM concentration. The gradient rate was varied between 2.5 and 7.5%/min with optimum resolution at 2.5% min. At a level of 20% DCM and a gradient rate of 5%/min, the separation of a mixture of five copolymers in a sudden-transition gradient was the same as with the corresponding common gradient, i.e., with injection into a mixture ofn-heptane and 20% DCM. Elution was also achieved at a level of 20% DCM by continuous addition of tetrahydrofuran (THF) instead of methanol. With THF, the peaks appeared later than with methanol in spite of the fact that methanol is a non-solvent and THF a good solvent for the polymers investigated. This indicates that elution was, in the first instance, caused by the polarity of the eluent. The elution characteristics of the copolymers in the system heptane/methanol at constant DCM concentration were basically similar to the already known characteristics iniso-octane/methanol at constant THF concentrations.
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    Ligand-exchange chromatography of amino acid enantiomers and its application to the biotransformation of DL-aspartic acid byPseudomonas dacunhae (1994)
    Springer
    Chromatographia 39 (1994), S. 15-22 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ligand exchange ; Amino acid enantiomers ; DL-aspartic acid ; Pseudomonas dacunhae
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of the D and L enantiomers of eighteen essential α amino acids has been investigated by ligand-exchange chromatography (LEC). The effect of column temperature on the retention times and resolution of individual amino acid enantiomers has been studied by varying the temperature from 25 to 50 °C for a mobile phase containing Cu2+ ions. By use of a temperature of 50 °C and Zn2+ in the mobile phase, eight of the eighteen amino acid enantiomers can be resolved sufficiently well for practical application. Only phenylalamine, tyrosine, and tryptophan can be separated by use of Ni2+ as complexation metal at 50 °C. LEC has been used to monitor the decarboxylation of racemic DL-aspartic acid byPseudomonas dacunhae. Analysis of DL amino acid enantiomers in different media was performed at column temperatures of 30 and 50°C by addition of 0.125 mM Cu2+ to the aqueous mobile phase. It was found that the analytical performance is most dependent on the identity of the metal used for complexation; the concentration of the metal was of secondary importance and the column temperature less important still.
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    Retention and selectivity of aromatic hydrocarbons with mono-substituted polar groups in ternary RP-HPLC systems (1994)
    Springer
    Chromatographia 39 (1994), S. 67-70 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed phase systems ; Ternary eluents ; Mono-substituted aromatics ; Retention and selectivity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The variation in selectivity for aromatic hydrocarbons with mono-substituted polar groups is investigated in ternary mobile-phase systems on C18 stationary phases. The dependence of log k′ on the proportions of two modifiers was determined for the solutes within the concentration range of ternary systems obtained by mixing two binary eluents: methanol + water and tetrahydrofuran + water or acetonitrile + water and tetrahydrofuran + water. The nature of the relationships is explained in terms of molecular shape, molecular interactions between solute and extracted modifier and the ordering of solvated ligands on the stationary phase.
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    URL: http://dx.doi.org/10.1007/BF02320460
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    The simultaneous determination of L-697, 661, a HIV-1 specific reverse transcriptase inhibitor, and its 6-hydroxy metabolite in human plasma via column-switching high performance liquid chromatography (1994)
    Springer
    Chromatographia 39 (1994), S. 79-84 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column switching ; HIV type 1 reverse transcriptase inhibitor ; Acquired immune deficiency syndrome ; L-697, 661
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the determination of L-697, 661, a human immunodeficiency virus type 1 reverse transcriptase inhibitor, and its 6-hydroxy metabolite in plasma is described. Following analyte isolation via solid phase extraction, samples are analyzed by HPLC using a column switching system. Column switching allows each analyte to be simultaneously analyzed under isocratic reverse phase conditions in a run time of 21 minutes. The assay was linear in the concentration range of 10–500 ng/mL for each analyte when 1 mL aliquots of plasma were extracted. The assay has been fully validated and utilized for human pharmacokinetic studies.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02320463
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  • 82
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    Reversed phase behaviour of high molecular mass polystyrenes in ethyl acetate solvent mixtures (1994)
    Springer
    Chromatographia 39 (1994), S. 663-667 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polystyrene ; Ethyl acetate ; Dichloromethane
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The reversed phase behaviour of high molecular mass polystyrenes was investigated on C18 bonded phase columns with ethyl acetate-methanol and ethyl acetateacetonitrile mobile phases. The results are compared with the corresponding dichloromethane mobile phases. The ethyl acetate-methanol mobile phase showed anomalous elution behaviour, similar to other previously investigated solvent combinations with methanol. The ethyl acetate-acetonitrile mobile phase showed no anomalous behaviour, increased retention and, elution over a wider composition range compared with the dichloromethane-acetonitrile system. However, resolution between adjacent molecular masses was considerably worse.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02274580
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    Simultaneous quantitative measurement of a new platelet activating factor antagonist (BN 50730) and its two main metabolites in human plasma and urine by LC-MS (1994)
    Springer
    Chromatographia 39 (1994), S. 228-238 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; LC/MS coupling ; Particle Beam interface ; Plasma and urine samples ; BN50730 and its metabolites
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple and sensitive assay has been developed for the quantitative measurement of a new platelet activating factor antagonist (BN50730), and its two main metabolites (BN50727 and BN50922), at the picomole level in human plasma and urine. The three compounds of interest and the internal standard (BN50765) were measured by combined LC-negative chemical ionization MS. A simple solid-liquid extraction procedure was used to isolate the parent drug and the two metabolites. The MS was tuned to monitor the intense ionm/z 333 generated in the ion source by a dissociative capture process. The assay was on 1 ml plasma or 0.1 ml urine and the quantitation limit was calculated as 1 ng·ml−1. The very low relative standard deviations and mean percentages of error calculated for within-day or between-day repeatability assays demonstrate the ruggedness of the technique for routine determination in biological fluids. Some preliminary results on the pharmacokinetics of the parent drug and its two main metabolites illustrate the applicability of this method.
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    URL: http://dx.doi.org/10.1007/BF02274505
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  • 84
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    Generation of split-flow micro-gradients for capillary HPLC (1994)
    Springer
    Chromatographia 39 (1994), S. 279-284 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Capillary columns for LC ; Micro-gradient generation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The generation of a micro-gradient for micro HPLC capillary columns is described. The system used is a modified and improved version of a split flow gradient elution device. Gradient tests have been performed and have shown good reproducibility under all conditions. The system has been successfully coupled with a particle beam LC-MS interface and the analysis of a mixture of twenty seven basic or neutral pesticides is reported.
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    URL: http://dx.doi.org/10.1007/BF02274514
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  • 85
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    Salt effects in anion exchange displacement chromatography: Comparison of pentosan polysulfate and dextran sulfate displacers (1994)
    Springer
    Chromatographia 39 (1994), S. 409-418 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-exchange chromatography ; Protein purification ; Pentosan polysulfate displacers ; Dextran sulfate displacers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Experimental studies were carried out to investigate the utility of pentosan polysulfate as a low molecular weight polyelectrolyte displacer for the purification of proteins in anion-exchange displacement systems. In addition, the influence of mobile phase salt concentration on displacer efficacy, protein-protein resolution, and displacement development were studied for several anionic displacers. It was found that while large polyelectrolytes (50 kd dextran sulfate) were efficient displacers for a wide range of salt concentrations, relatively small polyelectrolytes (3 kd pentosan polysulfate) were seen to act as an efficient displacer only under conditions of high salt micro-environments. In addition, for proteins exhibiting similar affinities, zone mixing at the protein-protein boundary was found to be quite sensitive to the salt concentration. Finally, displacement chromatography was successfully implemented for the separation of proteins from milk whey.
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    URL: http://dx.doi.org/10.1007/BF02278755
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  • 86
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    Separation of chlamydosporol epimers by reversed-phase HPLC using commercial solvent optimisation software (1994)
    Springer
    Chromatographia 39 (1994), S. 443-447 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mycotoxins ; Chlamydosporol epimers ; Solvent optimisation ; Fusarium species
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two epimers of the mycotoxin chlamydosporol were separated by HPLC on an RP-18 column using a quaternary mobile phase consisting of water (79.1%), methanol (10.0%), acetonitrile (10.4%) and tetrahydrofuran (0.5%), with a flow rate of 1 ml min−1. This optimal composition of mobile phase, with which the resolution value for the two epimers (1 and2) was 2.73 with retention times of 5.88 and 7.12 min, respectively, was achieved by the application of Philips Solvent Optimisation Software PU 6100. The presence of free silanols on the stationary phase was shown to be an essential requirement for the separation of the chlamydosporol epimers.
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    URL: http://dx.doi.org/10.1007/BF02278760
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    Determination of tacrolimus (FK 506) in whole blood using liquid chromatography and fluorescence detection (1994)
    Springer
    Chromatographia 39 (1994), S. 490-496 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Precolumn derivatization ; Dansylhydrazine ; Fluorescence detection ; Tacrolimus (FK 506) in blood
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A sensitive and selective liquid chromatographic method, using precolumn derivatization with dansylhydrazine followed by fluorescence detection, has been developed for the determination of tacrolimus (FK 506) in whole blood. After haemolysis, whole blood samples are extracted with diethyl ether and derivatized. After on-line removal of excess dansylhydrazine on a C18 precolumn, the derivative is loaded on to a C18 clean-up column, and a heart cut is subsequently transferred to a graphitized carbon column, where the final separation takes place. The method requires 1 ml of sample and has a limit of quantitation of 3 ng/ml. At the 15 ng/ml level the precision isca 10%, and the response is linear from the limit of quantitation toca 200 ng/ml of FK 506 in whole blood. The capacity of the method is 50 samples/day and about 1000 1-ml samples can be analyzed without changing either clean-up or separation column. Finally, the applicability of the method for therapeutic drug monitoring is shown.
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    URL: http://dx.doi.org/10.1007/BF02278767
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    Spectroscopic studies of butylphenyl, mono-ol and perfluorinated bonded phases (1994)
    Springer
    Chromatographia 39 (1994), S. 520-528 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; New bonded phases ; 13C and29Si CP-MAS NMR ; DRIFT ; ESCA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A variety of olefins were bonded to silaceous supports through a hydride modified substrate. The products were then examined by13C and29Si solid state-NMR with cross-polarization (CP) and magic angle spinning (MAS). Information about the surface was also obtained by diffuse reflectance infrared Fourier transform spectroscopy (DRIFT) and the related photoelectron spectroscopic technique (ESCA). Carbon analysis on bonded silicas was carried out and surface coverage was calculated. Confirmation of the organic groups bound to the silica support was possible. The hydride intermediate is shown to be a versatile material for bonding a wide variety of organic moieties to silica surfaces.
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    URL: http://dx.doi.org/10.1007/BF02268274
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  • 89
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    Analysis of isomers of cholesteryl acetate hydroperoxides by HPLC and GC-ITDMS (1994)
    Springer
    Chromatographia 39 (1994), S. 577-580 
    Details
    ISSN: 1612-1112
    Keywords: Gas chromatography-mass spectrometry ; Column liquid chromatography ; Cholesteryl acetate ; Hydroperoxide formation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic, high performance liquid chromatographic and GC-ion trap detector mass spectrometric analyses of the hydroperoxides formed during thermal peroxidation of cholesteryl acetate, are reported and discussed. The hydroperoxides were separated from the thermal-oxidised mixture by solid-phase extraction, fractionated and individually collected by HPLC. Each hydroperoxide was then chemically reduced with NaBH4 to a hydroxy-derivative. The GC and MS characteristics of hydroxy- and TMS-derivatives were compared against available standards. Only 7β-hydroperoxide and 7α-hydro-peroxide of cholesteryl acetate were found, as reported in the literature for cholesterol.
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    URL: http://dx.doi.org/10.1007/BF02268282
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  • 90
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    Retention behavior of aromatic hydrocarbons in reversed-phase liquid chromatography with ion-exchange-induced stationary phases (1994)
    Springer
    Chromatographia 39 (1994), S. 597-601 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-exchange-induced stationary phase ; Retention behavior ; Aromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention behavior of aromatic hydrocarbons on anion-exchangers modified with alkylsulfate or alkanesulfonate has been examined by column liquid chromatography. Several parameters affected the retention of analytes, involving concentration of the modifier in the mobile phase, its alkyl chain length and mobile phase composition. Stationary phases modified with a reagent having longer alkyl chains achieved better column efficiency. The separation factor achieved on ion-exchange-induced stationary phases foro-terphenyl and triphenylene was larger than that on alkyl-bonded silica gel.
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    URL: http://dx.doi.org/10.1007/BF02268286
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    Application of liquid chromatography-particle beam mass spectrometry and gas chromatography-mass spectrometry for the identification of metabolites of polycyclic aromatic hydrocarbons (1994)
    Springer
    Chromatographia 38 (1994), S. 781-788 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Particle beam MS detection ; Polycyclic aromatic metabolites ; Biodegradation in water
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two liquid chromatography-particle beam mass spectrometry (LC-PBMS) systems have been used for analysis of polycyclic aromatic hydrocarbon metabolites in water samples from a biological decomposition model experiment. The results were compared with those obtained by classical gas chromatography-mass spectrometry. Evaluation of spectral data indicated the presence of six main metabolites; 1H,3H-naphtho [1,8-cd]pyran-1,3-dione, 1-(hydroxymethyl)naphthalene, and 1,2-acenaphthenedione were identified by use of standard substances and spiking experiments. Enrichment of the investigated water samples with online pre-column (C18) concentration, freeze-drying, and solvent extraction led to similar results with only slight differences. The application of microbore separation columns proved to be a promising tool in particle beam LC-MS measurements.
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    URL: http://dx.doi.org/10.1007/BF02269637
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    Efficiency of porous hydrophilic polymer-based packing materials in chromatographic analysis of drugs existing with polypeptide (1994)
    Springer
    Chromatographia 38 (1994), S. 177-182 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hydrophilic polymer-based packing material ; Direct injection of serum
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A size monodispersed restricted-access polymeric packing material has been prepared through a simple and easy one-step method of co-polymerization of glycerol monomethacrylate and glycerol dimethacrylate with cyclohexanol as prorogen. A typical seeded polymerization (two step swelling and polymerization method) in an aqueous medium gave a 90 % yield of porous beads which could be utilized as a packing material in high performance liquid chromatography (HPLC) without any size classification due to the excellent size monodispersity. A BET measurement and size exclusion chromatography in either tetrahydrofuran or water revealed that the prepared material had only small pores (around 100 Å in diameter). It showed ample hydrophobicity for the separation of hydrophilic drug molecules in 10% aqueous acetonitrile buffer, while polypeptides such as bovine serum albumin were excluded and eluted before the void volume of the column with quantitative recovery.
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    URL: http://dx.doi.org/10.1007/BF02290333
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    Selective and sensitive analysis of 1-nitropyrene in diesel exhaust particulate extract by multidimensional HPLC (1994)
    Springer
    Chromatographia 38 (1994), S. 199-206 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Nitro-PAHs ; Diesel particulate extract ; Column switching
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A multicolumn (MC) HPLC method for the determination of 1-nitropyrene (1-NP) at trace-levels via on-line reduction to 1-aminopyrene and fluorescence detection is presented. On the first column, packed with a pyrenebutyric acid amide stationary phase, the nitro-derivatives of PAHs are strongly retained and separated from other matrix components. The nitro-PAHs-containing fractions are transferred onto a RP18-column via stepwise gradient elution and finally separated according to their various lipophilicities and sizes. To increase the overall selectivity and sensitivity of the multidimensional method (MD-HPLC system) post-column, on-line reduction of the nitro-PAHs to the respective amino-PAHs via a short catalysis column is performed thus enhancing the sensitivity significantly (to low pg levels). The applicability of this method for the determination of trace amounts of 1-NP in real samples (diesel particulate extracts) is demonstrated.
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    URL: http://dx.doi.org/10.1007/BF02290337
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    Molecular shape recognition capability of liquid-crystal bonded phases in reversed-phase high performance liquid chromatography (1994)
    Springer
    Chromatographia 38 (1994), S. 295-303 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Liquid crystal phases ; Molecular shape recognition ; Polycyclic aromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The chromatographic retention behaviour of two liquidcrystal bonded phases have been evaluated using polycyclic aromatic hydrocarbons (PAHs) as the probe samples in reversed-phase high performance liquid chromatography (RP-HPLC). The results clearly indicate that these phases have better planarity and shape recognition capabilities than commercially-avaialble polymeric octadecylsilica (ODS) phases whose strong planarity and shape selectivities were found earlier. It can also be concluded from the chromatographic observations that the shape recognition capability of these phases is dependent on both mobile phase composition and column temperature, but that the effect of mobile phase and temperature on the shape selectivity work independently. The retention behaviour can be explained by changes in the phase structure with changes of eluent composition and temperature.
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    URL: http://dx.doi.org/10.1007/BF02269771
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    In-line derivatization method for fluorometric determination of catecholamines by high performance liquid chromatography (1994)
    Springer
    Chromatographia 38 (1994), S. 591-594 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; In-line derivatization ; Fluorometric determination ; Catecholamines in urine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A fluorometric method has been developed for the determination of norepinephrine, epinephrine and dopamine by high-performance liquid chromatography. Catecholamines extracted from urine were separated by reversed-phase chromatography with an alkaline mobile phase (pH 8.0, 20 mM sodium tetraborate containing 30 mM 1-butaneboronic acid) and were fluorometrically detected (Ex 400 nm and EM 475 nm) via in-line derivatization at high temperature (100 °C). Retention times for norepinephrine, epinephrine, dopamine and isoproterenol as an internal standard were 8, 10, 13 and 28 min, respectively. Calibration curves for these compounds were linear from 4 to 100 ng/ml standard solution. The detection limit (signalto noise ratio=3) for norepinephrine, epinephrine and dopamine was 0.1, 0.2 and 0.8 ng. The assay of catecholamines in human urine is also described.
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    URL: http://dx.doi.org/10.1007/BF02277159
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    Determination of glutathione in pharmaceuticals and cosmetics by HPLC with UV and fluorescence detection (1994)
    Springer
    Chromatographia 39 (1994), S. 23-28 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Glutathione ; Pharmaceuticals and cosmetics ; Pre-chromatographic derivatization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A selective HPLC determination of reduced glutathione (GSH) in pharmaceutical and cosmetic formulations is described based on prechromatographic derivatization with 4-(6-methylnaphthalen-2-yl)-4-oxo-2-buteneoic acid. The derivatization reaction is rapid under mild reaction conditions (10 min at ambient temperature and pH 7.5) and the excess reagent can be removed by liquid-liquid extraction. The thiol adducts were chromatographed on a C-8 column using 0.05 M triethylammonium phosphate (pH 4.0) — acetonitrile 68∶32 (v/v), as the mobile phase; UV and fluorescence detection (lem 450 nm, lexc 300 nm) were both used. The structure of the thiol adducts was confirmed by1H and13C NMR spectra using sodium methanethiolate as thiol nucleophile.
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    URL: http://dx.doi.org/10.1007/BF02320453
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    Retention parameters of aromatic hydrocarbons with mono-substituted polar groups in binary RP-HPLC systems (1994)
    Springer
    Chromatographia 39 (1994), S. 51-61 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase systems ; Binary eluents ; Mono-substituted aromatics ; Retention and selectivity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Capacity factor (k′) values of aromatic hydrocarbons with mono-substituted polar-groups are correlated for reversed-phase systems involving stationary phases with C18 or C4 ligands chemically bonded to silica and a binary aqueous eluent containing modifiers: methanol, acetonitrile, tetrahydrofuran, isopropanol, dioxane or dimethoxyethane. The relative retention variations of the solutes are interpreted with special consideration of their interactions with non-polar stationary phases and the molecular structure of the modifiers and solutes. Rules for retention and selectivity optimisation in RP-HPLC systems are given.
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    URL: http://dx.doi.org/10.1007/BF02320458
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    System peaks in single column ion chromatography (SCIC) with indirect spectrophotometric detection (1994)
    Springer
    Chromatographia 39 (1994), S. 713-718 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion chromatography ; System peaks ; Indirect detection ; Anions and cations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The most popular eluents for SCIC are organic acids and their salts with one or more kinds of ion taking part in the elution process. These ions compete for ion-exchange equilibria. After an injection, the equilibria are disturbed and a re-equilibration process occurs resulting in extraneous peaks (system peak). A mechanism based on these aspects is proposed which is used successfully in the interpretation of the effects of sample properties and eluent parameters on system peaks. Experiments in the analysis of both cations and anions have been carried out to support this mechanism with eluents comprising two kinds of eluent ions. An equation for capacity factors in such systems is also derived.
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    URL: http://dx.doi.org/10.1007/BF02274588
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    Kinetic performance of open-tubular and packed columns in LC using the same stationary phase: Immobilized polymethyloctadecylsiloxane (1994)
    Springer
    Chromatographia 39 (1994), S. 729-739 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polymeric stationary phase coatings ; PMSC18 ; Column evaluation ; Peak capacity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary For the first time a direct comparison of the kinetic performance of narrow-bore (5–15 μm I.D.) opentubular columns (OTCs) and conventional packed columns in LC was carried out with stationary and mobile phases with identical chemical composition. The polymeric stationary phase was a polymethyloctadecylsiloxane (PMSC18) and the columns were evaluated in reversed-phase LC. In the open-tubular columns oncolumn detection was performed with laser-induced fluorescence. The observed column performance is presented in various ways, to take account of the basic differences of OTCs and packed columns. Experimental data was compared with theoretical models by use of a curve fitting procedure. The static coating method generates OTCs that perform close to theoretical predictions, and the packed columns were outperformed by the OTCs with regard to efficiency. A 6 m long and 6.3 μm I.D. OTC showed a minimum reduced plate height, hmin. of 0.5 at k′=0.27, which equals 1 900 000 theoretical plates. Also, it was established that the open-tubular columns provide higher resolution in a given analysis time. However, the importance of sufficient retention in OTCs is once again substantiated. Peak capacity plots illustrate that the k′ “window” should be optimized in order to reach maximum resolution (k′ 0–2 for OTCs and 0–5 for packed columns).
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    URL: http://dx.doi.org/10.1007/BF02274590
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  • 100
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    Chromatographic characterization of a hexapeptide containing three thiol groups, intrinsic to the metallothionein structure (1994)
    Springer
    Chromatographia 39 (1994), S. 146-154 
    Details
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Peptide characterization ; Thiol groups ; Electrochemical detection ; Metallothionein
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The hexapeptide Lys-Cys-Thr-Cys-Cys-Ala [56–61] MT I is a molecule intrinsic to the metallothionein structure. Its chromatographic behaviour on a reversed-phase column, using electrochemical detection has been studied in order to get a better understanding of its chemical stability under various conditions. The chromatogram of the peptide consists of two peaks. The optimization procedure for their separation is presented and a hydrodynamic voltammogram has been generated. The relative proportion of the two peaks can vary with experimental conditions and is clearly dependent of the peptide concentration. Following the various experiments to which the peptide was submitted, namely elution after air oxidation, under inert atmosphere, in basic pH, after addition of an oxidizing agent (H2O2) and after addition of a reducing agent (2-mercaptoethanol), a reaction scheme was suggested: transformations of the reduced hexapeptide (three free thiol groups) into—as a first step—its intramolecular oxidized form (one SS bond, one free SH) and then into—as a second step—the fully oxidized dimeric form (no more free SH). Electrochemical detection allows a quantitative follow-up of the thiol oxidation and hence, of the disappearance of the reduced peptide.
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    URL: http://dx.doi.org/10.1007/BF02274493
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