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  • 2005-2009
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  • 1
    ISSN: 1432-0789
    Keywords: Wheat ; Paddy straw compost ; N and P enrichment ; Rock phosphate ; Pyrite ; Triticum aestivum ; Nutrient uptake
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary A nutrient-rich compost from paddy straw was prepared using urea and Mussoorie rock phosphate for N and P enrichment respectively. Inorganic N was partly conserved in the compost by the addition of pyrite. Citric-acid-soluble P also increased with the addition of pyrite. Compost containing about 1.6% total N and 3.3% total P was found to be a good source of P for a wheat crop and also supplied a significant amount of N to the plants.
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  • 2
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    Biology and fertility of soils 7 (1989), S. 113-119 
    ISSN: 1432-0789
    Keywords: Vesicular-arbuscular mycorrhiza ; Herbicides ; Wheat ; Glomus spp. ; Spore germination ; Root infection ; Triticum aestivum L. ; Bifenox ; Mecoprop ; Difenzoquat methyl sulphate ; Chlortoluron
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary We studied the effects of field application rates of four herbicides (Avenge, Ceridor, Dicurane, and Harrier) on spore germination and infection of wheat roots by three species of Glomus grown under conditions of low P availability. Low concentrations of Ceridor (bifenox, mecoprop) and Harrier (mecoprop, ioxynil, clopyralid) inhibited spore germination while higher concentrations were stimulatory. Avenge (difenzoquat methyl sulphate) prevented spore germination completely, while Dicurane (chlortoluron) had no effect. The herbicide applications had no significant effect on the infection rates of any of the three fungi except Harrier on G. geosporum. The herbicide treatments did, however, affect plant growth and ear yields. Ceridor and Harrier increased ear yields, while Dicurane showed marked phytotoxic effects.
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  • 3
    ISSN: 1432-0789
    Keywords: Dentrification ; Immobilization ; Tillage ; N leaching ; Wheat ; Wetland rice
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary A field study was undertaken to examine the effects of various management strategies on wheat (Triticum aestivum L.) performance and N cycling in an intensively cropped soil. Microplots receiving 100 kg N ha−1 as15NH4 + 15NO3 − at sowing, tillering or stem elongation were compared with unfertilized microplots. Stubble from the previous rice crop was either incorporated, burnt without tillage, burnt then tilled or retained on the surface of untilled soil. Wheat grain yield ranged from 1.5 to 5.1 t ha− and was closely related to N uptake. Plant accumulation of soil N averaged 36 kg N ha−1 (LSD 5% = 10) on stubble-incorporation plots and 54 kg N ha−1 on stubble-retention plots. Fertilizer N accumulation averaged 18 kg N ha−1 (LSD 51% = 6) on stubble-incorporation plots and 50 kg N ha−1 on stubble-retention plots. Tillage had little effect on burnt plots. Delaying N application from sowing until stem elongation increased average fertilizer N uptake from 26 to 39 kg N ha−1 (LSD 5% = 6), but reduced soil N uptake from 50 to 37 kg N ha− (LSD 5% = 10). Immobilization and leaching did not vary greatly between treatments and approximately one-third of the fertilizer was immobilized. Less than 1% of the fertilizer was found below a depth of 300 mm. Incorporating 9 t ha−1 of rice stubble 13 days before wheat sowing reduced net apparent mineralization of native soil N from 37 to 3 kg ha−1 between tillering and maturity. It also increased apparent denitrification of fertilizer N from an average 34 to 53 kg N ha−1 (LSD 5% = 6). N loss occurred over several months, suggesting that denitrification was maintained by continued release of metabolizable carbohydrate from the decaying rice stubble. The results demonstrate that no-till systems increase crop yield and use of both fertilizer and soil N in intensive rice-based rotations.
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  • 4
    ISSN: 1432-203X
    Keywords: Wheat ; Maize ; Intergeneric cross-Embryo culture ; Haploid production
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Four Japanese wheat varieties, three crossable and one non-crossable with Hordeum bulbosum, were pollinated with maize pollen of 5 genotypes. By the application of 2,4-dichlorophenoxyacetic acid after pollination, embryos kept developing on wheat plants until 14 days after pollination. The frequency of embryo formation was significantly different among the maize genotypes, varying from 18.0% to 31.9%, but not among the wheat varieties. By bagging spikes with flag leaves the frequency of embryo formation was increased by about 7%. Ten- to twelve-day-old embryos gave higher frequencies of plant formation (83.6%) than 14-day-old embryos(50.0%). All 6 regenerated plants investigated cytologically were found to be haploid. Twelve of the 14 colchicine-treated plants produced florets setting seeds. The overall efficiency of our procedure is considered to be higher than that reported by Laurie and Bennett (1988).
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  • 5
    ISSN: 1432-2242
    Keywords: Mitochondrial DNA ; Chondriome variability ; In vitro culture ; Plant regeneration ; Wheat
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Plants have been regenerated from short-and long-term in vitro somatic tissue cultures made from immature embryos of the hexaploid wheat cultivar “Chinese Spring”. The mitochondrial genome organization of each regenerated plantlet was studied, after one selfing, by probing Sal I-restricted total DNA with cloned Sal I fragments of wheat mitochondrial DNA derived from a segment of the genome, which displays marked structural changes in response to in vitro culture. Short-term in vitro cultures give rise to regenerated plants whose mitochondrial genome organization is either close to that of the parental cultivar or to that of embryogenic callus cultures, except for a single plant which has an organization resembling that of short-term non-embryogenic cultures. In contrast, all but one of the plants regenerated from long-term cultures exhibited a mitochondrial genome organization similar to that of long-term nonembryogenic cultures. In addition, extra labelled bands were detected in some of the regenerated plants with two of the probes used. These results emphasize the importance of the duration of the in vitro step preceding the regeneration process: the longer it is, the higher the probability is of obtaining mitochondrial DNA variability in regenerated plants. Furthermore, since increasing the duration of the in vitro stetp results in the production of regenerated plants with a mitochondrial genome organization resembling that of non-embryogenic tissue cultures, the question is thus raised as to whether regeneration from long-term cultures is suitable for use in plant breeding.
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  • 6
    ISSN: 1432-2242
    Keywords: Wheat ; Aegilops ventricosa ; Powdery mildew resistance ; Biochemical markers ; Addition and transfer lines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary The gene encoding a variant of alcohol dehydrogenase, Adh-μ, has been found to be associated with the chromosome of the Mv genome which is present in type 9 wheat/Aegilops ventricosa addition line, to which the genes for protein CM-4 and for a phosphatase variant, Aph-v, had been previously assigned. Transfer line H-93-33, which has 42 chromosomes and has been derived from the cross (Triticum turgidum x Ae. ventricosa) x T. aestivum, carries genes encoding all three biochemical markers. Linkage between these genes has been demonstrated by analysis of individual kernels of the F2 (H-93-33 x T. aestivum cv. “Almatense” H-10-15). A study of the hybrids of line H-93-33 with T. aestivum H-10-15 and with the 4DS ditelosomic line has confirmed that, as suspected, the linkage group corresponds to chromosome 4Mv from Ae. ventricosa. Additionally, it has been found that the previously reported resistance of line H-93-33 to powdery mildew (Erysiphe graminis) is also linked to the biochemical markers; this indicates that either the gene responsible for it is different from that in lines H-93-8 and H-93-35, or that a translocation between two different Mv chromosomes has occurred in line H-93-33.
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  • 7
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    Theoretical and applied genetics 77 (1989), S. 516-520 
    ISSN: 1432-2242
    Keywords: Wheat ; Single seed descent (SSD) ; Single plant selection (SPS) ; Bulk population (BP) ; Mechanical mass selection (MMS)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Four methods of generation advance (SPS, SSD, BP and MMS) were compared in F3 and F4 generations. In the F3 generation, the SPS and SSD methods of generation advance proved superior to the BP and MMS methods for grain yield per plant and for at least one of the yield component traits. The F3 SSD population did not differ significantly from the F3 SPS for any of the traits. However, the F3 SSD population retained more range and cv for different traits than with other methods of generation advance. F4 progenies derived from F3 SSD population were significantly superior for grain yield than lines derived from the other three F3 populations. The MMS method of generation advance proved useful for increasing the 1,000-grain weight for which initial selection was made.
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  • 8
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    Theoretical and applied genetics 77 (1989), S. 685-688 
    ISSN: 1432-2242
    Keywords: Wheat ; Triticale ; Cytoplasmic effects
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Thirteen wheat-like advanced-generation triticale x wheat derivatives, having tetraploid wheat cytoplasm from triticale, were reciprocally crossed with three improved bread wheats, and the resulting F1s were evaluated for determining the comparative performance of the bread wheat and triticale cytoplasms for different traits. Significant reciprocal differences in the mean performance were observed for days to heading, days to maturity, spikes/plant, flag-leaf area, peduncle length, plant height, spike length, grains/spike, 1,000-grain weight, grain yield and grain protein content, and most of them were in favour of hexaploid wheat cytoplasm. However, this superiority of the hexaploid cytoplasm was not universal for a particular trait, implying that the differences in the performance of the evaluated reciprocal crosses depended not solely on the cytoplasmic background, but also on the interplay of the specific genotype with the cytoplasm.
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  • 9
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    Theoretical and applied genetics 77 (1989), S. 809-814 
    ISSN: 1432-2242
    Keywords: Wheat ; Ribosomal DNA ; Tissue culture ; Somaclonal variation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary In a previous study we observed extensive Nor region variability in tissue-culture derived plants of only one out of three tested wheat cultivars. This finding prompted us to further question whether or not this variability was invariably caused by in vitro culture. In the present study, the upper halves of spikes from four source plants of the inbred cultivar ‘ND7532’ were removed 12 days after anthesis. The immature embryos from these halves were cultured and regenerated into plants. The lower halves of the same spikes were retained on the plants to obtain mature caryopses. DNA was extracted from seedlings, cut with TaqI endonuclease, run on agarose gels, and the respective Southern blots were probed with the plasmid pTA71 to reveal the Nor region patterns. The sexual progeny of regenerants from three out of four source plants derived from the immature embryos provided Nor region patterns which were exactly identical to the patterns obtained from seedlings which germinated from the caryopses matured on the respective source spikes. The regenerants from the fourth source plant provided variable Nor region patterns. Analyses of the Nor region patterns of 21 individual seedlings germinated from caryopses of this source plant showed that 18 had a three-fragment pattern (consisting of 3.0, 2.7 and 1.9 kb fragments) while three seedlings lacked one (2.7 of 1.9 kb) fragment. Furthermore, the next sexual progeny of the regenerants which had a three-fragment pattern further segregated into three- and two-fragment patterns.These results, in conjunction with previous reports on Nor region variability among tissue-culture derived plants, suggest that this variability is not invariably related to in vitro culture.
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  • 10
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    Theoretical and applied genetics 78 (1989), S. 57-60 
    ISSN: 1432-2242
    Keywords: Hybrid necrosis ; Wheat ; Immature embryoculture ; Young ear culture
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Hybrid necrosis in wheat is a barrier to gene transfer in wheat breeding practice. It is based on two complementary genes, Ne1 and Ne2. Recovery mutants (Re1, Re2 and Re3) which can grow to maturity were recovered from immature embryo cultures of necrotic hybrids between T. aestivum and T. durum. Cytological observation demonstrated that Re1 had 34 chromosomes instead of 35. This indicated that one of the chromosomes carrying the Ne genes was lost. Genetic study suggested that for Re1, the lost chromosome was chromosome 5B of the durum parental line. Re mutants are male sterile but can be maintained through a young ear culture method. Re mutants could be successfully pollinated by either parental line and the BC1 progeny is partially fertile. Re mutants were repeatedly induced in about 1% of the regenerated plants from immature embryo culture. This technique provides a practical way to bypass hybrid necrosis.
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  • 11
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    Theoretical and applied genetics 78 (1989), S. 137-142 
    ISSN: 1432-2242
    Keywords: Wheat ; Diallel analysis ; Somatic embryogenesis ; Plant regeneration ; In vitro culture
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Diallel analyses of F1 and reciprocal crosses among five winter wheat lines show that additive, non-additive, and cytoplasmic genetic effects were significant in the genetic control of somatic embryogenesis, shoot, and root induction frequencies as well as in numbers of somatic embryos, shoots, and roots. However, additive genetic effect appears to be most important since, in most cases a larger portion of the cross variation was accounted for by general combining ability. The results suggest that somatic embryogenesis and organ regeneration in winter wheat can be improved through genetic manipulation. Due to the presence of maternal effects, it may be critical to use a suitable genotype as a female parent in a selection program.
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  • 12
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    Theoretical and applied genetics 78 (1989), S. 783-787 
    ISSN: 1432-2242
    Keywords: Tissue culture ; Callus ; Wheat ; Ditelosomics ; Nullisomic-tetrasomics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary The ability of immature embryos of wheat (Triticum aestivum L.) to respond to tissue culture has been shown to involve the group 2 chromosomes. The available group 2 ditelosomic and nullisomic-tetrasomic lines of ‘Chinese Spring’ wheat were used to determine the chromosome arm location and chromosome dosage effect associated with the expression of tissue culture response (TCR). Significant differences were found between the aneuploid lines and the euploid control for the expression of both regenerable callus formation and callus growth rate. A model is proposed suggesting that a major TCR gene is located on 2DL and that 2AL and 2BS possess minor TCR genes. Furthermore, a major regulatory gene controlling the expression of TCR genes may be located on chromosome 2BL.
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  • 13
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    Theoretical and applied genetics 78 (1989), S. 867-872 
    ISSN: 1432-2242
    Keywords: Wheat ; Cytoplasm ; Anther culture ; Microspore embryogenesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Anthers were cultured from two sets of seven lines of hexaploid wheat (Triticum aestivum L.) with different cytoplasms, the euplasmic nucleus donors, ‘Siete Cerros 66’ and ‘Penjamo 62’, as well as their six alloplasmic lines derived from wild relative species of the genera Triticum and Aegilops. Significant cytoplasmic and nuclear effects but no cytoplasmic-nuclear interaction were found for embryogenic anther response, with the best performance of ‘Penjamo 62’ in Ae. kotschyi cytoplasm. Plant regeneration was not affected significantly by the cytoplasmic background of the lines cultured. The possible genetic implications of the observed cytoplasmic and nuclear influences on the in vitro haploid induction of wheat are discussed.
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  • 14
    ISSN: 1432-2242
    Keywords: Wheat ; Anther culture ; Regeneration ability
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Marked effects of genotype on wheat anther culture response have been observed. Genetic factors have been recognised to be one of the major contributors to in vitro responses of cultured wheat tissues. In wheat anther culture, embryo induction, plant regeneration and albina/green ratio have been determined to be heritable traits. Using Chinese Spring (CS) monosomic 1D, single chromosome substitution lines of chromosome 5B or chromosome arm 5BL from Chinese Spring into six varieties, and F1 hybrids heterozygous for the 1B chromosome structure (1BL-1BS/1BL-1RS), the anther culture response was studied: genes on CS1D chromosome and 5BL chromosome arm increases the embryo frequency; gene(s) involved in regeneration ability are located on the 1RS chromosome arm; a gene increasing albina frequency is located on Chinese Spring 5B chromosome. Our results support the fact that without gametic selection, a differential development occurred from the particular classes of microspores carrying genes for higher regeneration ability. Moreover, in some crosses, a few genes with major effects were involved in determination of anther culture response.
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  • 15
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    Theoretical and applied genetics 78 (1989), S. 173-176 
    ISSN: 1432-2242
    Keywords: Wheat ; Tiller index ; Competitive ability ; Interplant competition ; Modified pedigree method of selection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary A dismal 81% failure of newly bulked lines against checks was observed in Indian wheat material evolved by the pedigree method. This is considered to be the consequence of selection in space planting in early generations followed by yield tests in a competitive environment which did not allow any scope of selection for competitive ability. Thus, most of the homozygous lines, which were until now raised and carried forward under space planting, failed to compete with the checks for yield in close planting. It is, therefore, necessary to modify the method to combine both the competitive ability and identity of selected plants. The proposed modified procedure involves raising the population under spaced planting as well as under drilling from F2 onwards. Evaluation for tiller index marks an important step. On the basis of tiller index, single plants are isolated from spaced populations. Steps of the modified procedure are outlined in detail. The modified method, which economises on breeders' workload and other physical inputs, besides having other advantages, can also be used for certain other grain crops. Preliminary results based on the modified method during the past two seasons have indicated its utility.
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  • 16
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    Theoretical and applied genetics 78 (1989), S. 349-352 
    ISSN: 1432-2242
    Keywords: Wheat ; Malate dehydrogenase ; Isozymes ; Triticeae
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary A third set of malate dehydrogenase loci have been identified and located on the short arms of homoeologous group 5 chromosomes in wheat. Allelic differences have been found at each of the three Mdh-3 loci. However, Mdh-D3 appears to be least variable, with a second allele found only in Sears' ‘Synthetic’ among a survey of 42 varieties. Homoeoloci were identified on chromosome 7 (5H) of Hordeum vulgare, the short arm of 5E in Agropyron elongatum and 5U in Aegilops umbellulata.
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  • 17
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    Theoretical and applied genetics 78 (1989), S. 436-444 
    ISSN: 1432-2242
    Keywords: Intergeneric hybrids ; Wheat ; Leymus ; Chromosome pairing ; Meiosis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Hybrid plants were obtained between Triticum aestivum (2n=6x=42, AABBDD) and Leymus innovatus (2n=4x=28, JJNN) at a frequency varying from 0.4% to 1.2% of the pollinated florets. Improvement of the embryo culture medium resulted in a higher frequency of embryo rescue. Eight of ten hybrids had the expected chromosome number of 35 (ABDJN). Meiotic analysis indicated that there was no homology between the genomes of the two species. Two hybrids had only 28 chromosomes. Comparison of chromosome pairing between the two types of hybrids suggested that Leymus innovatus carries genes that affect chromosome pairing and behavior. The relatively high occurrence of spontaneous doubling in the meiocytes of these hybrids may indicate that backcrossing of the hybrids to wheat should be possible, although frequent chromosome irregularities observed in the meiocytes of the hybrids may decrease the probability of success of this step, which is essential to the process of gene transfer from L. innovatus to wheat.
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  • 18
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    Theoretical and applied genetics 78 (1989), S. 495-504 
    ISSN: 1432-2242
    Keywords: Wheat ; Genetic mapping ; RFLPs ; Isozymes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Restriction fragment length polymorphism (RFLP) mapping was attempted using 18 cDNA clones, 14 anonymous and 4 of known function, which had been shown to have homologous DNA sequences on the group 7 chromosomes of wheat. The loci identified by these probes have been mapped on one or more chromosomes in this homoeologous group using linkage data derived from various F2, random inbred, doubled haploid and single chromosome recombinant populations. The maps also include three isozyme loci, five disease resistance loci, two anthocyanin pigment loci and a vernalisation response locus. The mapping data have been used to determine the extent of map co-linearity over the A, B and D genomes, the degree of RFLP variability in the three genomes and the relative efficiency of various restriction enzymes in detecting RFLPs in wheat. The strategy for future mapping in wheat, particularly the use of “alien” genomes or segments, such as that from Aegilops ventricosa used here, is discussed.
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  • 19
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    Theoretical and applied genetics 78 (1989), S. 657-664 
    ISSN: 1432-2242
    Keywords: Aminopeptidase ; Wheat ; Isoelectric focussing ; Isozymes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Isoelectric focussing was used to separate the isozymes of aminopeptidase of wheat and its relatives. Three distinct homoeoallelic sets of genes have been shown to be present. AMP-1, controlled by genes on the long arms of group 6, has previously been described, but two new systems, AMP-2 (group 4) and AMP-3 (group 7) are described here. The three systems are distinguished by their electrophoretic characteristics, by their genetic control and by their substrate specificity. Intervarietal, interspecific and intergeneric polymorphism has been observed at most of the loci. A further set of isozymes, AMP-4, was detected but the chromosomal control of these could not be determined.
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  • 20
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    Theoretical and applied genetics 78 (1989), S. 879-883 
    ISSN: 1432-2242
    Keywords: Wheat ; Anther culture ; Androgenetic responsiveness ; Albinism ; Genetic control
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Inheritance of the ability to respond in wheat anther culture was studied from 6×2 reciprocal crosses between six varieties with high and two varieties with low capacity for green plant formation and their parents, replicated in two environments. Effects of genotypes dominated embryo formation and percentages of green plants, accounting for 78.4% and 85.4% of total variation, respectively, while smaller genetic effects were indicated for regeneration. Nuclear genes could explain almost all the genotype effects in this material. Embryo formation showed heterosis over high parent for 5 of the 12 hybrids, while percentages of green plants from the hybrids were intermediate to the parents. General Combining Ability (GCA) could explain 78.8% of the variation for embryo formation among the hybrids, whereas differences in percentage of green plants were dominated by Specific Combining Ability (SCA), accounting for 67.9% of hybrid variation. A positive correlation (r=0.81**) was observed between the genetic capacity for regeneration and green plant formation. Analysis of covariance indicated that effects causing GCA for green plant formation were mainly responsible for this correlation. A regression model with two parallel lines divided the six parent lines with high green plant formation into three groups with respect to their reactions with the two testers. The results are discussed with regard to possible involvement of two sets of nuclear genes affecting the percentage of green plants obtained in wheat anther culture: one set consisting of mainly additive effects affecting green plant percentage through an initial effect on regeneration ability, and another set of two or a few more major genes with dominance or epistatic effects uncorrelated with regeneration.
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  • 21
    ISSN: 1617-4623
    Keywords: LMW glutenin ; Seed storage protein ; Molecular evolution ; Tissue-specific expression ; Wheat
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary The isolation and characterisation by DNA sequencing of a low molecular weight (LMW) glutenin gene from wheat is described. The deduced protein contains a signal peptide, a central repetitive region rich in proline and glutamine and N and C terminal non-repetitive domains, similar to other prolamins. A detailed comparison of the C terminal domain of 20 prolamin genes enabled us to divide them into 4 families. The LMW glutenin family is distinct from the α, β-and γ-gliadin families of wheat and is closest to the B hordein genes of barley. This and other comparisons were also used to assess the pattern of genetic variation among prolamin sequences and to provide a molecular basis for the interpretation of prolamin size polymorphism. The 5′ flanking fragment of the isolated gene was previously shown to direct endosperm-specific expression of a reporter gene in transgenic tobacco. Evidence is provided that the isolated gene is also active in wheat and its transcription initiation site was determined. Features of the gene which may be relevant to its activity are discussed.
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  • 22
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    Chromatographia 27 (1989), S. 27-30 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; 1,ω-Di(alkoxy)-polysulphides ; Retention contributions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The reaction of S2Cl2 with alcohols yields products, the reversed-phase liquid chromatograms of which are similar to those of dialkyl-polysulphides RSnR, i.e., they represent homologous series. Four of the products were identified via GC-MS as 1,ω-di(alkoxy)-polysulphides having the general structure ROSnOR. Retention contributions of alkyl groups R and sulphur atoms in the −Sn — chain are not much different from values observed with polysulphides. The effect of oxygen, however, is only about −100 index units per O atom, while in dialkyl ethers values of −500 units have been reported.
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  • 23
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    Chromatographia 27 (1989), S. 5-14 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Retention behaviour ; Column parameters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Retention of small molecules on reversed phase or other hydrophobic stationary phases can be represented by k′ values of members of a homologous series at varying solvent compositions. The evaluation of simple linear relationships leads to the introduction of a set of four parameters that contain all the information about retention behaviour of this homologous series in the binary solvent system chosen. It is possible to extrapolate to a hypothetical non-hydrophobic molecule and a solvent, the polarity of which equals that of the stationary phase, to characterize the properties of the stationary phase — eluent system. In addition, a chromatographic method for determination of the phase ratio of the column is proposed.
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  • 24
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion exchange separation ; Preparative separations ; Human chorionic gonadotropin hormone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A high-performance liquid chromatography (HPLC) method was developed for the purification of 50mg crude human chorionic gonadotropin (HCG) hormone sample in one chromatographic run on a 250×10 mm SERVA DEAE Poliol-Si-500 column. During the 60-minute linear gradient of 0.05 M sodium sulfate, 0.05 M sodium hydrogen sulfate and 0.05% (v/v) acetonitrile in buffer “B” complete separation was accomplished in 40 min. Identity and purity of the fractions were checked by SDS electrophoretic method. The eluted HCG fractions were dialyzed for 24 hours to remove the buffer salts and liophilized. The activity of the hormone did not decreased significantly during the purification procedure.
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  • 25
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Microcrystalline cellulose triacetate ; Molecular modeling ; Computer graphics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Molecular modeling and energy calculations have been used to study the chromatographic separation of aromatic compounds on microcrystalline cellubose triacetate. A linear relationship has been found between the logarithms of the capacity factors and the energy values of the interaction of these compounds with this stationary phase. The interaction energies have been calculated for two different spatial dispositions of the solutes in relation to the sorbent.
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  • 26
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Liquid crystals ; Synthesis of new bonded phases
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    Topics: Chemistry and Pharmacology
    Notes: Summary A compound which becomes a liquid crystal when bonded to a polysiloxane was reacted with dimethylchlorosilane to produce a reagent suitable for bonding to a silica surface. After the silanization reaction was complete, the product was characterized by elemental analysis, diffuse reflectance Fourier transform Infrared Spectroscopy (DRIFT), CP/MAS carbon-13 NMR and differential scanning calorimetry (DSC). Preliminary chromatographic testing was done by retention index measurements using the alkylarylketone homologous series and by measuring the separation factor, α, for anthracene/phenanthrene at two different mobile phase compositions.
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  • 27
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    Chromatographia 27 (1989), S. 633-638 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Adsorption isotherms ; Equilibria criteria ; Silica and carbon adsorbents ; Aromatic compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary Examples of high-performance liquid chromatography (HPLC) are given for the determination of adsorption equilibrium and distribution coefficients, calculation of excess adsorption isotherms from solutions ranging from 10−7 to 10−1 mole fraction, changes in activity coefficient of the component predominantly adsorbed from solution and substitution enthalpy. These examples stem from studies of HPLC and the static adsorption of benzene, anisole and benzaldehyde from solutions in n-heptane on macroporous silica and active carbon at various temperatures. A criterion is suggested for evaluating equilibrium in the HPLC process. The potential of size-exclusion chromatography (SEC) for evaluating the volume and predominant diameter of adsorbed pores as well as pore diffraction are discussed. Prospects for HPLC application to molecularstructural analysis and other purposes are discussed briefly.
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  • 28
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    Chromatographia 27 (1989), S. 118-122 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase chromatography ; Non-aqueous reversed-phase chromatography ; Polycyclic aromatic hydrocarbons ; Solvent strength
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    Topics: Chemistry and Pharmacology
    Notes: Summary Elution strengths of 11 common HPLC solvents on a polymeric C18 phase were compared using a marker set of polycyclic aromatic hydrocarbons. Naphthalene, pyrene, benzo[ghi]perylene, and three larger naphthologues of 8, 10, and 12 rings (constituting a “naphthalene zigzag” series) were chosen because they span the solvent strength range up to and including the strongest solvents, tetrahydrofuran (THF) and chlorobenzene. Four pairs of similarly shaped isomers were used to probe solvent selectivity. With the exception of THF, HPLC solvent strength correlated with observed red shifts of fluorescence band maxima in each solvent. For THF, the pure solvent and blended mixtures behaved quite differently.
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  • 29
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    Chromatographia 27 (1989), S. 156-158 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mobile phase retention time ; Capacity factor ; Negative capacity factor
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    Topics: Chemistry and Pharmacology
    Notes: Summary Numerous ideas and procedures have been suggested in the literature for the determination of tm, the retention time of a non-retained species, in high-performance liquid chromatography. In some cases chromatograms have been obtained showing sample components eluting prior to the assumed non-retained species. This phenomenon results in apparent negative capacity factors for the species in question. We have proposed a method employing small inorganic anions which results in a limiting value for tm and eliminates apparent negative capacity factors.
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  • 30
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    Chromatographia 27 (1989), S. 228-232 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase ; 13C n.m.r. ; Arginine-aldehyde peptides ; GYKI-14166
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    Topics: Chemistry and Pharmacology
    Notes: Summary High-performance liquid chromatographic and13C n.m.r. spectrometry methods were used for the investigation of peptides containing arginine-aldehyde moiety. Investigation of a model compound, N-benzoyl-Arg-H, showed that in an acidic mobile phase peptides containing the arginine-aldehyde group elute in three characteristic peaks. The components of the peaks were found to be constituents of an equilibrium mixture. The structures of the two components were identified, one as the aldehyde hydrate, the other as the cyclanol derivative. The reactivity of TRIS (HCl) buffer at pH 8.5 with the arginine aldehyde moiety was used for the assignment of the equilibrium structures.
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  • 31
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase ; Ion-pair ; Recoveries ; Hepatocytes ; Purine compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary Three groups of metabolites were analyzed in extracts of rat hepatocytes by an HPLC method: (i) nucleotides (ATP, ADP, AMP, GTP, GDP, UTP, UDP, IMP, UMP), (ii) nucleosides and nucleobases (adenosine, adenine, guanosine, inosine, xanthine, hypoxanthine, uridine) and (iii) inhibitors of xanthine oxidoreductase (oxypurinol, allopurinol). Perchloric acid extracts were neutralized with K2CO3/triethanolamine and analyzed at 254 nm by reversed-phase ion-pair high-performance liquid chromatography. The nucleotides and their derivatives were separated with a gradient elution using 10 mM NH4H2PO4/2 mM t-butylammonium-phosphate and acetonitrile. Recovery values were estimated for the extraction procedure used. The method was applied to the investigation of nucleotide metabolism of hepatocytes of starved rats at anoxia and reoxygenation.
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  • 32
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    Chromatographia 27 (1989), S. 316-320 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion chromatography ; Silica-based cation-exchanger ; Trimethylsilyl chlorosulfonate ; Lanthanides
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    Topics: Chemistry and Pharmacology
    Notes: Summary A low exchange-capacity, silica-based cation-exchanger for use in ion chromatography has been synthesized. (p-Trimethylsilyl)benzyl-dimethylchlorosilane (TBDCS) reacts with trimethylsilyl chlorosulfonate (TMCS) to produce a compound sulfonated in the para position of the type ArSO2OSi (CH3)3, which is bonded to 5 μm porous silica beads and hydrolysed to the corresponding arylsulfonic acid. The product is hydrophilic and has a high degree of sulfonation, efficiencies of packed columns reaching about 40,000–50,000 plates per meter for the separation of the Mn2+ ion. The new stationary phase has been applied to the ion chromatography of some organic and inorganic ions. It is notable that 14 lanthanides can be separated by isocratic elution about one hour on a 150×4·6 mm column, with 4 mM ethylenediamine and 6 mM α-hydroxyl-isobutanoic acid (pH 3.67) as mobile phase.
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  • 33
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    Chromatographia 27 (1989), S. 191-193 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Dansyl amino acids ; Chemiluminescence ; Bis(2,4,6-Trichlorophenyl)oxalate, (TCPO) ; Enhancement of luminescence
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    Topics: Chemistry and Pharmacology
    Notes: Summary The dansylated amino acids alanine, glutamic acid, methionine and norleucine were separated by reversedphase HPLC and detected via chemical excitation using the post-column, TCPO-peroxyoxalate reaction system. Enhancement of the chemiluminescence emission was achieved by including the surfactant Triton X-100 in the eluent.
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  • 34
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reverse-phase chromatography ; Elastin Hydrolysis measurement ; On-line post-column derivatization
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    Topics: Chemistry and Pharmacology
    Notes: Summary Excessive breakdown of elastin, a structural protein, may be related to aortic disease and emphysema. Since L-valyl-L-proline occurs in high concentrations in elastin, a rapid and sensitive method using HPLC with post-column on-line derivatization was used to measure the dipeptide from swine aortic tissue, and the amount of elastin present was determined. Elastin was extracted by alkaline hydrolysis. After neutralization and filtration, the sample was injected onto a ODS-2 gel column, and the dipeptide was eluted by a linear gradient of 0 to 10% of 1-propanol in 50 mM heptafluorobutyrate, pH 3, at a flow rate of 1 ml/min. The eluent was reacted with fluorescamine at pH 8.6, and fluorescence was detected at an excitation wavelength of 395 nm and a 455 nm cutoff emission filter.
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  • 35
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    Chromatographia 27 (1989), S. 449-454 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion exchange and affinity columns in series ; Porcine pancreatic enzymes ; Trypsin and elastase
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    Topics: Chemistry and Pharmacology
    Notes: Summary In order to separate and purify some of the enzymes contained in porcine pancreas, operation of an ion-exchange column in series with an affinity column has been used. The enzymes dealt with possess very similar molecular weights, isoelectric points and active sites. Hence they are difficult to separate and purify by traditional separation and/or purification methods. CM-Sepharose anion-exchange resin adsorbs elastase and trypsin at low pH (4.5) and desorbs them at high pH (9.0) and high ionic strength. Chitin-CHOM affinity adsorbent adsorbs trypsin at high pH (8.0) and desorbs it at low pH (2.5). By virtue of this complementary relationship two chromatographic columns were connected in series for facilitating the separation and purification of elastase and trypsin from porcine pancreas. The result showed that the specific activities of elastase and trypsin had been increased 16 and 22 fold respectively.
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  • 36
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    Chromatographia 27 (1989), S. 472-474 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hydrous titanium oxide ; Anion exchange ; Polyvalent anions
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    Topics: Chemistry and Pharmacology
    Notes: Summary Hydrous titanium oxide (HTiO), prepared under varying conditions of precipitation, has been studied for its anion exchange behaviour. Its chemical and thermal stability has been examined. The stoichiometry of uptake for Cl− has been investigated using a36Cl radiotracer and the regeneration power of the exchanger checked. Distribution coefficients for halides and polyvalent anions have been determined and on the basis of sorption data some polyvalent anions have been separated using HTiO columns.
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  • 37
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    Chromatographia 27 (1989), S. 509-512 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flavonoids ; Crataegus ; Passiflora ; Matricaria ; Ginkgo
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    Topics: Chemistry and Pharmacology
    Notes: Summary Flavonoids of Crataegus monogyna, Passiflora incarnata, Matricaria chamomilla and Ginkgo biloba extracts have been separated by isocratic elution on C18 columns using eluents based on C3 alcohols, tetrahydrofuran or dioxane. Satisfactory results have been obtained at compared to the low resolution achieved with the customary system acetonitrile-water-acetic acid.
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  • 38
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    Chromatographia 28 (1989), S. 19-23 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Preparation of stationary phases ; Polymer coated stationary phases ; Polymer-octyl bonded phase
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    Topics: Chemistry and Pharmacology
    Notes: Summary Polymethyloctylsiloxane-coated stationary phases have been prepared for liquid chromatography, by thermal reaction. The influence of the reaction conditions on retention and efficiency of test substances with different structures has been discussed. The materials have good stability in both acidic and basic eluents.
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  • 39
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Size exclusion ; Vesicular packing material ; Proteins and polymers
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new vesicular packing material — prepared from plant cell clusters by purification of the intact cell wall framework —is suitable for chromatography, giving high performance at low pressure gradients. The separation is achieved by dialysis through the cell wall, which is an ultrafilter membrane with an extremely sharp size limit of separation. Almost the whole of the stationary liquid phase is located within the vesicle (empty cell) lumina. In contrast to gel filtration vesicle chromatography gives a practically ideal separation of two size groups with an extremely short fractionation range. The size limit of separation was investigated by chromatography of proteins and other polymers. Group separation of molecules of a polydisperse dextran standard preparation showed that the critical Stokes' diameter for dextran permeation into the stationary liquid phase of the vesicular packing is 5 to 6 nm.
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  • 40
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Preparative scale separation ; 1,1-Dimethylethyl 4- and 5-bromo-trans-2-methylcyclohexane-1-carboxylate ; Trimedlure-related isomers ; Ceratitis capitata
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    Topics: Chemistry and Pharmacology
    Notes: Summary A semi-preparative high-performance liquid chromatographic procedure on 5-μm silica was developed for the isolation of gram quantities of four 1,1-dimethylethyl 4- and 5-bromo-trans-2-methylcyclohexane-1-carboxylate isomers (trimedlure-related) for NMR studies and comparative biological evaluation as male medfly,Ceratitis capitata, attractants.
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  • 41
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrochemical detection ; Pseudouridine ; Creatinine ; Urine analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary The anodic behaviour of pseudouridine a modified nucleoside proposed as tumoral marker, has been studied at a mercury electrode. A method for its determination in urine samples by liquid chromatography with indirect anodic polarographic detection has been developed. The method is simple, highly selective and permits the direct injection of urine after dilution (1∶20) with mobile phase. Creatinine, which also gave an anodic response on mercury, could be simultaneously determined and used as an “internal standard” for Psi. This allowed the pseudouridine/creatinine ratio determination in a single run on the same specimen and the use of urine samples collected randomly instead of the 24h collection. The within-day RSD% for pseudouridine/ creatinine peak areas ratio was 3.4%.
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  • 42
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    Chromatographia 28 (1989), S. 9-14 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ester silicate silica gels ; Behaviour with organic bases ; Silanol groups ; Acidic centres
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    Topics: Chemistry and Pharmacology
    Notes: Summary Silica gels produced from ester silicates (ES-gels) are excellent chromatographic supports. In comparison with other silica gels the RP-materials obtained from them show little peak tailing even with polar, and, in particular, with basic compounds. Gels produced by various manufacturing processes have been classified by adsorption with methyl pyridinium chloride. ES-gels yield very low methyl pyridinium chloride values and small asymmetry parameters. The results indicate that there are strongly acidic, structurally-related surface centres which cause peak tailing on most commercial gels. It was shown that surface silanols on silica gels do not, in themselves, lead to peak tailing.
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  • 43
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    Chromatographia 28 (1989), S. 34-38 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Methylisothiazolones ; Preservatives ; Analysis of cosmetics
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    Topics: Chemistry and Pharmacology
    Notes: Summary Antimicrobially active formulations based on 2-methyl-3(2H)-isothiazolone and 5-chloro-2-methyl-3(2H)-isothiazolone (Kathon CG, Euxyl K 100) are incorporated into manufactured cosmetics as preservatives. In this paper we report on the analysis of these active components by means of liquid chromatography. It is conventional for the original methylisothiazolone components in cosmetics to be analyzed by reversed phase high-performance liquid chromatography after column chromatographic separation and flash chromatographic purification. In our new analytical method the methylisothiazolones are converted into the respective β-thiosubstituted acrylamide derivatives, which are ionic substances, with the help of the nucleophilic reagent hydrogensulfite. An ion pair high-performance liquid chromatographic method has been developed for the separation and quantification of these derivatives.
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  • 44
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Oxygen radicals ; Nucleotides ; Aldehydes
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    Topics: Chemistry and Pharmacology
    Notes: Summary The analysis of two metabolite groups, nucleotides and aldehydes, is necessary for assessment of oxygen radical metabolism during hypoxia and reoxygenation. Nucleotides and their derivatives were determined by HPLC using gradient elution with 10 mM NH4H2PO4 buffer containing 2 mM t-butylammoniumphosphate and acetonitrile. Aldehydes occuring after lipid peroxidation were analyzed by derivatisation to dinitrophenylhydrazones followed by TLC and HPLC separation with methanol/water on an ODS column.
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  • 45
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    Chromatographia 28 (1989), S. 209-211 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Triazine herbicides
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    Topics: Chemistry and Pharmacology
    Notes: Summary A number of 11 triazine herbicides and 7 of their corresponding metabolites were separated in a single HPLC run. The separation was achieved on a reversed-phase column using gradient elution with acetonitrile/buffer. Detection was by UV absorption at a wave-length of 220 nm.
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  • 46
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid phase extraction ; Polycyclic aromatic hydrocarbons ; Diode array and fluorescence detection
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    Topics: Chemistry and Pharmacology
    Notes: Summary Both the separation of polycyclic aromatic hydrocarbons (PAH's) on tailor made HPLC phases, and their chromatographic enrichment and quantitative determination are of great interest. Because of the generally low concentrations of PAH's in the environment, and the low limiting values in German legislation for drinking water, methods for selective enrichment and sensitive detection are indispensable. On account of their relatively high amounts in soil, the determination of PAH's is valuable for the assessment of the potential danger to ground water by waste materials. These requirements can be fulfilled by used of solid phase extraction on enrichment columns, and fluorescence or UV/VIS diode array detection. For the detection of PAH's in the picogram range, the wavelengths for excitation and emission were time programmed over the chromatogram. With this feature, it is possible to detect all the individual compounds at the highest sensitivity, over the entire analysis.
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  • 47
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    Chromatographia 28 (1989), S. 289-292 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micro-bore and capillary columns ; Gradient techniques
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gradient delivery system for microbore and open tubular liquid chromatography is described. A gradient mixing vessel of 5–100μl, or 25–1000μl allows the generation of binary gradients with high reproducibility. The suitability of the system for short packed micro bore columns and open tubular columns is demonstrated.
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  • 48
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flecainide in plasma ; Fluorescence detection
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    Topics: Chemistry and Pharmacology
    Notes: Summary A high performance liquid chromatographic method for the determination of flecainide in serum has been developed. The analysis is performed on a microparticulate silica column. The eluate is monitored by fluorescence detection at an excitation wavelength of 300nm and an emission wavelength of 370nm. No sources of interference were identified and a coefficient of variation of less than 8% was observed on repeated flecainide determinations. The method has a good reproducibility, specificity and accuracy, and can be applied in therapeutic drug monitoring of flecainide in patients.
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  • 49
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Coulometric electrochemical detection ; Methylnaltrexone ; Rat brain and serum analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary A simple and sensitive method is described for the determination of methylaltrexone, a quaternary narcotic antagonist, in discrete rat brain regions and serum. Separation and quantitation are performed by reversedphase high-performance liquid chromatography with coulometric electrochemical detection. Perchloric acid extracts of the brain tissue or serum were passed through a normal-phase solid-phase extraction CN column, and methylnaltreexone was subsequently eluted with a mixture of absolute ethanol and 25mM trifluoroacetic acid. Methylnaltrexone gave a linear response over the range of 12.5–100ng in 1.0ml for cerebellar homogenates and 25–200ng in 50μl for serum. The average betweenassay coefficients of variation for methylnaltrexone from 1.0ml of cerebellar homogenate and 50μl of serum were 5.2 and 3.6%, respectively, over the concentration range studied. The within-assay coefficients of variation at 12.5ng/ml cerebellar homogenate and 25ng/50μl for serum were 7.4 and 4.6%, respectively. Analytical recovery of methylanyltrexone, added to cerebellar homogenate and serum samples, were 85 and 89%, respectively. The method was applied to the analysis of methylnaltrexone in discrete rat brain regions and serum after intraperitoneal injection.
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  • 50
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    Chromatographia 28 (1989), S. 129-132 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carotenoids ; Paprika, Rose hips, Marigold
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the preparative HPLC of carotenoids and carotenoid esters using a self-packing axially-compressed column. The reversed-phase system used employs an RP-18 stationary phase and a mobile phase consisting of a mixture of petroleum spirit, acetonitrile, methanol and tetrahydrofuran. The method is demonstrated for paprika fruit, rose hips and marigold flowers.
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  • 51
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Wheat proteins ; γ-gliadins ; Effect of pH on separation ; Effect of organic modifier on separation
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    Topics: Chemistry and Pharmacology
    Notes: Summary Reversed-phase, high-pressure liquid chromatography has been used to separate similar protein (γ-gliadin) components from 70% ethanol extracts of endosperm flour from two different accessions of the diploid wheatTriticum monococcum L. The effect of acetonitrile as the organic eluent was compared to acetonitrile: 2-propanol (3:1) at two different pH's. Conditions for maximum resolution of the γ-gliadin components were found to be at pH 7.2 with acetonitrile: 2-propanol (3:1) as the eluent. These conditions allowed the components to be obtained in sufficient purity for further charaterization.
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  • 52
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ligand-exchange ; Preparative racemate resolution ; Amino-acids
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    Topics: Chemistry and Pharmacology
    Notes: Summary Preparative resolutions of racemic amino-acids by ligand-exchange chromatography are described. Base-line resolution of multigram quantities of many racemic solutes was obtained using very simple equipment (open tubular column).
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    Chromatographia 28 (1989), S. 354-358 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ternary mobile phases ; Solute retention model
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    Topics: Chemistry and Pharmacology
    Notes: Summary In our previous publications we have established a new physico-chemically grounded retention model valid for the adsorption and partition mechanism of retention using multicomponent mobile phases. Moreover, we have demonstrated its practical usefulness for predicting solute retention in several different chromatographic modes (i.e. in TLC, normal-phase and reversed-phase HPLC) employing binary mobile phases. In this paper we give an ultimate check to the physicochemical correctness of our new retention model, using it for the description of solute retention in reversedphase HPLC systems with ternary mobile phases of the B+AB1+AB2 type. The complexity of these mobile phases and of the possible intermolecular interactions among the consitituent solvents was supposed to rigidly scrutinize the premises of the assumed new approach. We have observed a good agreement between the experimental retention parameter for a number of solutes chromatographed with the use of two different mobile phases of the B+AB1+AB2 type, and the retention parameter calculated according to the assumed model. Therefore, we believe to have sufficiently tested our new approach and confirmed its physico-chemical correctness.
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  • 54
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Optical resolution ; Polymeric adsorbents ; Penicillin sulfoxide ; Substituent effect
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Fourteen new vinyl polymers carrying penicillin sulfoxide nucleus, poly (substituted-benzyl 1-oxo-6-metha-crylaminopenicillanate)s, were synthesized in order to investigate the influence of the substituents on the optical resolution capabilities. The resolution efficiency of the high-performance liquid chromatography columns comprising the obtained polymers were examined usingtrans-stilbene oxide and N-acetyl-1-phenethyl-amine. It was found that some columns resolved both racemates, some one, while the others did not separate either. A polymer which has 2,6-dichlorobenzyl moiety was found to resolve both racemates more effectively than the unsubstituted polymer.
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  • 55
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    Chromatographia 28 (1989), S. 465-468 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chlorinated phenols ; 4-Aminoantipyrine derivatives of phenols ; Metabolites of phenoxy alkanoic acid herbicides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary High performance liquid chromatography (HPLC) has been applied to the separation and determination of o-chlorophenol, 2,4-dichlorophenol, 3,4-dichlorophenol, 2,5-dichlorophenol, and 2,4,5-trichlorophenol in water samples after prior derivatization with 4-aminoantipyrine. These substances are the phenolic decomposition products of the phenoxy-alkanoic acid herbicides: 2,4-dichlorophenoxyacetic acid (2,4-D), 2,4-dichlorophenoxybutyric acid (2,4-DB), and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T). An RP-C18 column was used, with gradient elution starting at 50/50 and changing to 70/30 methanol/water (v/v) after 24 min. Detection was carried out at 470 nm where the 4-aminoantipyrilquinonimine derivatives show maximum absorbance. The method was linear over a concentration range of 5–10,000 ppb phenol in the original water sample. By using an enrichment step a detection limit of 2 ppb phenol could be approached. The method was used to study the degree of degradation of the phenoxy acids to phenols under different conditions of temperature, pH, and UV irradiation.
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  • 56
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ligand exchange ; Chiral phase ; Optical resolution of 2-hydroxy acids
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    Topics: Chemistry and Pharmacology
    Notes: Summary Using an MCl GEL CRS10W column, which was packed with octadecyl silica (ODS) coated with N,N-dioctyl-L-alanine, optical resolution of 2-hydroxy acids was performed. The optical resolution of mandelic acid derivatives and C2 to C5 2-hydroxy acids was carried without any pretreatment. The MCl GEL CRS10W column could resolve amino acids and 2-hydroxy acids. For their selective detection, a post-column method was employed in which the specific color reaction of 2-hydroxy acids with iron(III) ion was utilized. For the analysis of foodstuffs, in which amino acids and 2-hydroxy acids often coexist, the present method was found to be effective in distinguishing between these enantiomers.
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  • 57
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    Chromatographia 28 (1989), S. 497-501 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Collagen metabolites ; Amino acid derivatives ; Glycosides
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    Topics: Chemistry and Pharmacology
    Notes: Summary Methods are described for the isolation of galactosyl hydroxylysine and glucosylgalactosyl hydroxylysine from collagen and for the quantitative analysis of these hydroxylysine glycosides. The isolation procedure, based upon gel filtration and preparative ionpaired reversed-phase high-performance liquid chromatography, is simple and rapid in comparison with existing methods, allowing the production of tens of milligrams of each glycoside in a single day. Quantitative analysis of the hydroxylysine glycosides is effected by reversed-phase high-performance liquid chromatography with precolumn derivatization (usingo-phthal-dialdehyde) and fluorescence detection.
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  • 58
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Optical resolution ; Polymeric adsorbents ; Penicillin sulfoxide ; Copolymerization
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    Topics: Chemistry and Pharmacology
    Notes: Summary A methacrylamide carrying penicillin sulfoxide skeleton, benzyl 1-oxo-6-methacrylaminopenicillanate, was copolymerized with methyl methacrylate. The optical resolution efficiency of the columns comprising the obtained copolymers was investigated using a high-performance liquid chromatography system. A copolymer incorporated by 27mol% of methyl methacrylate showed higher chirality recognition capability than the homopolymer, which suggests that the introduction of methyl methacrylate contributes to enriching desired penicillin sulfoxide alignment (i. e., tracticity) along the polymer main chain. An estimated penicillin monomer's number-average sequence length in the copolymer was 2.7.
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  • 59
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    Chromatographia 28 (1989), S. 519-522 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase chromatography ; Separation of metal acetylacetonates
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    Topics: Chemistry and Pharmacology
    Notes: Summary Using reversed-phase high-performance liquid chromatography acetylacetonate complexes with trivalent metals such as Al(III), Co(III), Cr(III) and Fe(III) have been examined in columns containing RP-2, RP-8 and RP-18 bonded phases. The mobile phase consisted of acetonitrile/water or methanol/water mixtures with various compositions. As shown the order of elution of the acetylacetonates depends on the type of the column packing and on the nature and concentration of the organic modifier in the mobile phase.
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  • 60
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thin-layer chromatography ; Penstemide and serrulatoloside
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    Topics: Chemistry and Pharmacology
    Notes: Summary Penstemide and serrulatoloside, two iridoids of similar molecular structure, were separated by stepwise gradient TLC in a straight-phase systems (silica-ethyl acetate+isopropanol) and by HPLC in a reversed-phase system (ODS-silica — water+methanol).
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  • 61
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Overpressured layer chromatography ; Furocoumarin isomers ; Preparative separation of plant extracts
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    Topics: Chemistry and Pharmacology
    Notes: Summary Preparative medium pressure liquid chromatography and semi-preparative high performance liquid chromatography on silica were employed for the isolation of eight furocoumarin isomers (iso-bergapten, angelicin, psoralen, bergapten, pimpinellin, sphondin, xanthotoxin and isopimpinellin). The conditions were transposed from analytical on-line overpressured layer chromatography and analytical high performance liquid chromatography, respectively. The retention data of the analytical on-line overpressured layer chromatographic separation and the preparative medium pressure liquid chromatographic isolation show a linear relationship. Using 15 μm TLC silica 60 as stationary phase a dry-packing procedure aas developed for labomatic medium pressure liquid chromatographic glass columns. The efficiency of the preparative separation techniques was demonstrated by the isolation of the investigated furocoumarins from Heraclei mantegazziani radix and from Pimpinellae radix (Balkan quality).
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  • 62
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    Chromatographia 27 (1989), S. 101-104 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Bromo/iodosubstituted thyronines ; Mobile phase optimization ; Radioimmunoassay detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed-phase high performance liquid chromatographic method on C-18 bonded silica is described for the separation of trisubstituted iodo/bromothyronines, which exert thyroid hormone activity. The composition of the mobile phase has been systematically optimized resulting in a ternary mixture of methanol/acetonitrile/water acidified with trifluoroacetic acid. The applicability of ultraviolet absorption detection, amperometric detection and off-line radioimmunoassay was investigated. The latter method allows detection of the different iodo/bromothyronines down to 40–120 ng/l mobile phase; this sensitivity is high enough for application to thyroid hydrolysates in order to clarify the question as to whether bromine can substitute iodine in the biosynthesis of thyroid hormones.
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  • 63
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    Chromatographia 27 (1989), S. 113-117 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Retention contribution of nitrogen ; Effect on methylene and sulphur chains
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The reaction of secondary amines R2NH with disulfur dichloride S2Cl2 in dichloro methane yields mixtures of bis-dialkylamino polysulphides R2N−Sn−NR2 with sulphur chain lengths varying from ns=2 to 14. The S chains are believed to be non-branched. The compounds form homologous series in each of which sulphur atoms give a constant contribution to retention. The sulphur retention index depends slightly on the carbon number in the terminal alkyl groups R. The presence of nitrogen lowers retention. The index increment of N is ca. −160 units, which is distinctly less negative than values found in alkylamines.
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  • 64
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Size-exclusion chromatography ; Fast atom bombardment-MS ; Peptic haemoglobin hydrolysate
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the ready identification of any peptide isolated from a complex peptic haemoglobin hydrolysate produced on the pilot-plant scale. A combination of size exclusion and reversed-phase, high-performance liquid chromatography have proved to be a useful strategy for fractionation of such a mixture. This technique enabled pure peptides from the total hydrolysate to be obtained. Amino acid analysis and fast atom bombardment mass spectrometry provided the accurate composition and molecular weight of any isolated peptide. Molecular weights are compared with those deduced from size-exclusion chromatography (SEC) and the usefulness of SEC is discussed. The procedure described in this study will be useful for acquiring a better knowledge of such an hydrolysate and could be extended to other crude protein digests.
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  • 65
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrochemical detector ; Amines ; Silages ; Feedstuffs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of the electrochemical detector (EC) in the high performance liquid chromatography (HPLC) of dansyl derivatives of biogenic amines is reported. Isocratic and gradient elution patterns of synthetic mixtures of putrescine, cadaverine, 1,6-diaminohexane, tryptamine, histamine, tyramine, spermine and spermidine on a reversed phase column are shown. Hydrodynamic voltammograms of standard compounds are presented. The detection limits of the EC are compared with those of ultraviolet and spectrofluorimetric detectors. A chromatographic profile of amines from the proteolytic catabolism of maize silage byClostridia is shown.
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  • 66
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Normal phase elution ; Silica and cyano columns ; Flavonoid compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary HPLC retention data for a number of flavonoid compounds have been evaluated on normal phase silica and cyano colums according to the Soczewinski-Snyder (S.-S.) model. On the silica phase most of the flavones examined exhibited asymetrical peak shapes indicating strong and mixed retention mechanisms; on the cyano phase the intercept of the S.-S. relationship was independent of any hydroxy substitution pattern or of molecular planarity. A similar behaviour, but with different intercept values, was observed with coumarin and quinone compounds.
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  • 67
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    Chromatographia 27 (1989), S. 292-296 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Selenium(IV)-tellurium(IV) separation ; Flow-through coulometric detector
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    Topics: Chemistry and Pharmacology
    Notes: Summary The chromatographic behaviour of selenium and tellurium has been investigated with two different reversed-phase chromatographic methods, using P-350 (methyl-bi-isooctyl phosphate) and TBP (tributyl phosphate) as the stationary phases. HCl, HBr, NaCl and NaBr were employed as mobile phase components in both methods. The results suggested that the separation mechanism corresponds to the formation of TeCl (or TeBr) and P-350H (or TBPH) ion associate. A coulometric flow-through detector was applied to determine Se(IV) and Te(IV). Complete separation and quantitative determination of Se and Te could be achieved in 10 minutes.
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  • 68
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    Chromatographia 27 (1989), S. 325-327 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carotenoid ; Xanthophyll ; Broccoli ; Paprika
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the preparative HPLC of up to 50mg of carotenoid using a self-packing axially-compressed column. Oxygenated carotenoids, xanthophylls, are separated with silica as the stationary phase and acetone/petroleum ether as the mobile phase, while carotenes are separated using magnesium oxide/polyamide as the stationary phase and undiluted petroleum ether as the mobile phase.
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  • 69
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    Chromatographia 27 (1989), S. 340-342 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Evaporative light scattering detection ; α, ω-Dicarboxylic and hydroxycarboxylic acids ; Alkylglucosides and glycerides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The advantages of an evaporative light scattering detector in HPLC are demonstrated using the separation of α, ω-dicarboxylic and hydroxycarboxylic acids, alkyl glucosides and mono-, di- and triglycerides as examples. By using this detector reversed phase as well as normal phase gradient HPLC becomes possible for substances with no UV absorption.
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  • 70
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    Chromatographia 27 (1989), S. 371-377 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Alkyl-bonded silica gel ; Enthalpy ; Van der Waals volume
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Starting from silica gel with a purity of 99.999%, octadecyl-(ODS), octyl-(C8) and propyl-(C3) bonded silica gels were synthesized, and end-capped by trimethyl groups. The pore size was 150 Å and the specific surface area was 320 m2/g. The ODS and C8 silica gels were stable in both acidic and basic solutions. The selectivity of these bonded-silica gels was examined from the difference of the retention behavior of alkanes (Al−Al), alkylbenzenes (Ph−Al), alkylalcohols (Al−OH) and polyaromatic hydrocarbons (PAH) in aqueous acetonitrile. On these packings the log k′ values decreased in the order Al−Al〉Ph−Al〉PAH〉Al−OH. Furthermore, the chromatographic behavior of these compounds was measured on polymer-coated octadecyl-bonded silica gel (CAP) and octadecyl-bonded vinyl alcohol copolymer gel (ODP). The selectivity was verified from the value of R* of these compounds: $$R = R_v + R^* $$ where R is the retention time, and Rv is the retention time of an alkane having the same Van der Waals volume as the analyte. The R* values indicated that this ODS had more selectivity than C8 and C3, however R* on C8 showed a very good correlation with R* on C3. Their retention behavior on CAP was similar to that of ODS, however, their capacity ratios measured on CAP were smaller than those on ODS. The ODP has selectivity for the retention of aromatic compounds, because PAHs were retained strongly on this column.
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  • 71
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Alternaria mycotoxins ; Food analysis ; Electrochemical detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The electroactivity of majorAlternaria mycotoxins has been explored in order to devise a liquid chromatographic-electrochemical detection (LC-EC) method for the determination of these toxic metabolites in fungal cultures and in naturally contaminated foodstuffs. Alternariol, alternariol methyl ether, altertoxin-I and altertoxin-II have been found to be electroactive and could be detected at sub-nanogram levels. Advantages and limitations of dual electrode (screen mode) coulometric detection and single electrode amperometric detection are presented and discussed. The feasibility of electrochemical detection in gradient elution liquid chromatography as well as its applicability to the analysis of contaminated foodstuffs is demonstrated.
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  • 72
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    Chromatographia 27 (1989), S. 431-435 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; UV diode array detection ; Electro chemical detection ; Herbicides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An automated procedure is described for simultaneous UV detection at three different wavelengths and electro chemical detection in series of some residual herbicides. UV spectra of nine compounds of different compound groups are presented. Liquid-liquid extraction with dichloromethane and an enrichment of about one thousandfold has been used. Recovery rates after enrichment and detection limits of four s-triazine, three phenyl urea herbicides, metazachlore and metamitrone in river and drinking water are shown. It is concluded that the herbicides examined can be detected at levels between 10ng l−1 and 50ngl−1, without the necessity of derivatisation or clean-up processes.
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  • 73
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    Chromatographia 27 (1989), S. 257-263 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Size exclusion ; Fractal dimension ; Retention model
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Some porous packings used in chromatography have been claimed to be fractals with a scale of sizes a〈l〈L, where a is a molecular size and L is the size of the largest pores. For a fractal porous packing, the excluded volume for molecules in solution in the vicinity of the packing surface is directly related to Df, the fractal dimension of the pore surface (2〈Df〈3). Since retention in size exclusion chromatography is itself directly related to this excluded volume, the fractal nature of the packing provides a model of retention in this technique. According to this model there is a linear relationship between log Rs and log(1-Kd), where Rs is the hydrodynamic radius of the solute macromolecules and Kd the distribution coefficient. The fractal dimension is derived from the slope of this plot. Size exclusion chromatographic retention data have been analyzed according to the model. It is found that some HPLC packings are fractals with fractal dimensions ranging from about 2.15 to 2.6, depending on the material. Such a large range of Df values indicates large variations in the selectivities and domains of applications of the different packings. For some classical gel filtration chromatographic gels, the fractal retention model does not seem to apply.
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  • 74
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micro-columns ; Flow rate and temperature programming ; PTH amino acid derivatives
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    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of phenylthiohydantoin (PTH) amino acid derivatives by flow rate and temperature programming in reversed-phase micro-column liquid chromatography (LC) has been investigated. For both programming modes a microcomputer-assisted retention prediction system (REPRES) was constructed. The performance of this system has been evaluated by comparing actually measured retention data to those predicted. Excellent agreements between those data were found. It is clearly indicated that simultaneous flow rate and temperature programming can improve the separation of PTH-amino acids in reduced analysis time.
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  • 75
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    Chromatographia 28 (1989), S. 89-91 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrophoresis ; Comparison of HPLC and electrophoresis ; Proteins, peptides and amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Protein structure analysis is an indispensible tool in modern biological research. However, the isolation of a protein or the separation of peptides in a form suitable for sequence analysis is a considerable technical challenge. The two predominant separation methods in protein biochemistry are chromatography and electrophoresis. In this paper the position, advantaged and disadvantages of both HPLC and electrophoresis for the separation of amino acids, peptides and proteins in protein structure analysis are discussed.
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  • 76
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    Chromatographia 28 (1989), S. 565-568 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; New bonded phases ; Alumina ; Protein separation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Several reactions are tested for the chemical modification of alumina. These include the following: chlorination of the surface hydroxyls followed by reaction with an organolithium compound; chlorination of the surface hydroxyls followed by reaction with a Grignard reagent; chlorination of the surface hydroxyls followed by reaction with an amine; chlorination of the surface hydroxyls followed by reaction with an alcohol; direct reaction of the alumina with an organochloroalane and direct reaction of the alumina with an alcohol. Only the first reaction gave a product which contained enough bonded organic material to be easily detected by FTIR. Preliminary stability tests show that the product of the first reaction retains the bonded organic material when exposed to nonpolar and polar organic solvents as well as aqueous solutions of pH 1.0, 7.0 and 12.0. Chromatographic testing establishes reversed-phase behavior for alkylarylketones as solutes and the bonded phase displays good biocompatibility for a series of protein standards.
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  • 77
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Adenosine phosphates ; Adenosine phosphate degradation products ; Innervated frog muscle
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Adenosine mono-, di- and triphosphates, inosine monophosphates, adenosine, inosine and hypoxanthine were separated in a single run by high-performance liquid chromatography with UV detection. AC-18 reversephase column was used. An isocratic elution with 100mM phosphate buffer (KH2PO4) pH6.5 and 1.2% methanol, followed by a 5 minute linear gradient up to 15% methanol after the 10th minute was performed during each run with a flow rate of 1.25ml/min. The time required for each analysis was 25 minutes. The detection limit for each substance ranged from 3 to 5 pmol. All the substances under study were detected in the incubation medium when adenosine triphosphate was exogenously applied to the innervated frog sartorius muscle.
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  • 78
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Molecular interactions ; Association effects ; Analyte solvation
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    Topics: Chemistry and Pharmacology
    Notes: Summary The linear Jaroniec equation has been utilized for the description of chromatographic systems in which the test substance molecule is solvated by the solvent molecules. A possibility of the formation of multimolecular solvates in the bulk phase has been confirmed. The measurements were made using liquid adsorption chromatography with ternary mobile phase.
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  • 79
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral separations ; Trypsin on silica ; Amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new HPLC stationary phase was synthesized by the covalent immobilization of the enzyme trypsin (TRYP) on silica. The hydrolytic activity of the immobilized enzyme was 72% of the activity of an equivalent molar amount of free TRYP. The initial chromatographic studies indicate that this phase can be used for chiral separations of enantiomeric O- and N,O-derivatized amino acids which are natural substrates on TRYP and that the stereochemical resolutions are a result of the activity of the enzyme.
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  • 80
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    Chromatographia 28 (1989), S. 574-578 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemically bonded phases ; End-capping ; Destructive effects on bonded phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMS) have been used as a secondary deactivation (end-capping) reagents for packing materials for RP HPLC. Three types of chemically bonded phases (CBP) with different structures and different coverage densities were used. The destructive effects of HMDS on the coverage density of chemically bonded C18 and C8 phases is discussed.
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  • 81
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Cellulose acetate ; Acetyl content ; Temperature effects
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Cellulose and cellulose mono-, di-, and triacetate were used as stationary phases for liquid chromatography with water as a mobile phase, and the retention behavior of alcohols, ethers, ketones, and chlorides was examined. For cellulose acetate columns, the logarithm of the specific retention volume, (logV g * ), correlated linearly with the logarithm of partition coefficient between 1-octanol and water (log Ko/w), for each homologous group, but all solutes were unretained on cellulose columns. With the exception of chlorides, the intercept values of the log V g * –log Ko/w regression lines increased significantly with increase of acetyl content of cellulose acetates, but the slopes of the regression lines changed little. This suggests that hydrophobic interaction between the acetyl groups of cellulose acetates and the alkyl chains of the solutes is the dominant factor in the retention. The capacity factors for 1-alcohols with cellulos diacetate column indicated a maximum at a column temperature of about 40°C. This unique retention behavior was assumed to be caused by small structural change of the cellulose acetate polymer, because this temperature effect on the retention corresponded with effects observed by differential scanning calorimetry (DSC).
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    Chromatographia 28 (1989), S. 161-166 
    ISSN: 1612-1112
    Keywords: Thin-layer chromatography ; Column liquid chromatography ; Micropreparative separations ; Furocoumarins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Furocoumarins from extracts ofHeracleum genus fruits were separated using normal and reversed phase TLC and HPLC and isolated in the milligram scale using overloaded systems of column chromatography. Binary or ternary solvents containing a polar modifier (methanol, diisopropyl ether or acetonitrile) were used as the mobile phases.
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  • 83
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion-exchange ; Mobile phase optimisation ; Egg-white proteins
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    Topics: Chemistry and Pharmacology
    Notes: Summary Factors influencing the capacity of Whatman QA52 anion-exchange cellulose for hen egg-white proteins have been investigated. While simply increasing the concentration of protein in the feedstock increases the loading there is a concomitant reduction in binding efficiency in a single pass through the column. Substitution of buffer by water in the mobile phase during sample preparation, thereby reducing the ionic strength of the feedstock, had the effect of significantly increasing protein capacity whilst improving binding efficiency. During column loading large changes in pH of the mobile phase were observed although this had no apparent effect on the chromatography for this system.
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    Chromatographia 28 (1989), S. 193-196 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral stationary phases ; Immobilized enzymes ; Racemic resolution of amino acid esters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Racemic resolution of aromatic and aliphatic amino acid esters into L-amino acid and D-amino acid ester via LC and HPLC is achieved by using enzyme reactors as chromatographic columns. For this purpose α-chymotrypsin and trypsin are immobilized on Eupergit C, Sepharose 4B and Lichrosorb-Diol.
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  • 85
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Bonded stationary phases ; Evaluation of the hydrophobicity of sorbents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The energy of interaction (∈0) between the methylene group and the surface of a sorbent is proposed for use in the quantitative evaluation of the hydrophobicity of a sorbent. A method was developed to determine the ∈0 parameter from chromatographic measurements using the investigated sorbent as the stationary phase and linear methylene-containing homologous series, e.g., alkanols, amino-alkanes, etc., as the test compounds. The effectiveness of this method is demonstrated by using, as examples, a series of bonded stationary phases and a series of cross-linked copolymeric sorbents differing in the concentration of the hydrophobic groups. The proposed method is compared with the Martin rule used extensively in the chromatography of oligomers.
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  • 86
    ISSN: 1612-1112
    Keywords: Thin-layer chromatography ; Column liquid chromatography ; Mobile phase optimization ; HPTLC transposition to HPLC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A computer-assisted method is presented for mobile phase selection for the optimal separation of pesticides by HPTLC and HPLC. The system is based on a plot of solute retention value and separation criterion vs. binary mobile phase composition for graphic optimization. The result of HPTLC can be transposed to HPLC for optimal separation. The transposition equation is given.
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  • 87
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    Chromatographia 28 (1989), S. 311-312 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flavonoid glycosides ; Betula
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The main flavonoid glycosides ofBetulae folium extracts (quercetin-3-glucuronide, myricetin-3-galactoside, hyperosid, quercetin-3-arabinoside and quercetin-3-rhamnoside) have been separated by isocratic elution on a C18 Aquapore RP-300 column. Elution was performed with 17% isopropanol at pH 6.2 confirming the validity of this eluent for the analysis of the flavonoid glycosides.
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  • 88
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral stationary phase ; Resolution of amino acid derivatives ; Enantioseparation by HPLC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A chiral stationary phase for the separation of some D-and L-amino acid derivatives using a new resolving agent is described. The enantiomeric resolution was accomplished by normal phase high-performance liquid chromatography. The support was easily prepared by coating an epoxy polymer of L-valinamide on aminopropylsilanized macroporous silica. The influence of subambient temperatures on the enantioselectivity was also examined.
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  • 89
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral recognition process ; Enantiomeric elution order ; Mobile phase modifiers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Three enantiomeric solutes, a sulphoxide, a piperidine derivative and a methyl ester have been chromatographed on an HPLC chiral stationary phase (CSP) based upon cellulose-tribenzoate (Chiralcel OB-CSP). The mobile phases used in the study were composed of hexane modified with homologous series of primary, secondary and cyclic alcohols. Interesting reversals in enantiomeric elution order have been observed for 2-phenoxypropanoic acid methyl ester associated with changes in chain length or ring size of the alcohol mobile phase modifier. The results of the study suggest that at least two chiral recognition mechanisms operate on the OB-CSP and point out the importance of acquiring elution order data in all studies involving chiral stationary phases.
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  • 90
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Prediction of retention times ; Gradient elution ; Substituted quinolines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A chromatographic model able to predict, from experimental isocratic data, retention times of solutes under gradient conditions has been proposed previously. The prediction was shown to be totally independent of the chemical properties of both solutes and eluents. In order to further check the general validity of the theory, the model has now been applied to a nonhomologous set of compounds, namely a range of substituted quinolines (methyl-, hydroxy- and amino-) and several different stationary phases. Results show a dependence on the stationary phase and, to a lesser extent, on the chemical structure of the solutes. The possible sources of errors are discussed. The generality of the method holds, within acceptable limits, if predictions concern the same type of stationary phase.
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  • 91
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thiol analysis ; Fluorimetric detection ; Derivatization with 4-(6-methylnaphthalen-2-yl)-4-oxobuten-2-oic acid
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of 4-(6-methylnaphthalen-2-yl)-4-oxobuten-2-oic acid as a fluorogenic reagent in pre-column derivatization for the high-performance liquid chromatography (HPLC) of biologically important thiols (L-cysteine, glutathione, N-acetylcysteine, homocysteine and mercaptopropionylglycine) was investigated. The aroylacrylic acid reacts selectively and rapidly (15 min. at room temperature) with the thiol compounds to give stable fluorescent adducts which can be separated by reversedphase HPLC and detected fluorometrically (λex 300nm); λem 445nm). The experimental conditions for the thiol derivatization and chromatographic separation are discussed. Applications to the determination of N-acetylcysteine, mercaptopropionylglycine and cysteine are described.
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  • 92
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    Chromatographia 27 (1989), S. 194-200 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Dissociation constants ; Potentiometric titration ; 2,4-Dimethylthiazole ; Trimethylpyrazine ; Methyl anthranilate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Reversed-phase liquid chromatography on two stationary phases—octadecylbonded silica Partisil ODS-3 and polystyrene-divinylbenzene resin PRP-1—and potentiometric titration in the water/methanol mobile phase were investigated in order to determine the dissociation constants of three weakly basic aroma compounds, namely trimethyl pyrazine, 2,4-dimethyl thiazole and methyl anthranilate. The data obtained from both methods are quite consistent and compare favourably to values found in the literature.
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  • 93
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Cathinone metabolites ; Plasma
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary High-performance liquid chromatography (HPLC) for the determination of (−)-cathinone in rabbit and human plasma has been studied. The problem of dimerization during extraction from plasma was satisfactorily resolved. Detection was by UV at 257 nm. Concentration levels as low as 24 ng ml−1 were satisfactorily determined. This level of sensitivity should be adequate for the detection of (−)-cathinone in the blood of khat users and also for the quantitative determination of (−)-cathinone in blood for pharmacokinetic purposes. The applicability of the assay procedure to pharmacokinetic studies is demonstrated.
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  • 94
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Glucose, maltose and maltotriose ; α-Amylase and glucoamylase ; Microfungal cultures
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In the hydrolysis of soluble starch by mixtures of α-amylase and glucoamylase, the ratios maltose/glucose and maltoriose/glucose linearly depend, over a wide range, on the relation between both enzymes and are independent on the activity level of the enzymatic preparation. HPLC determination of hydrolysis products (glucose, maltose and maltotriose) of soluble starch by mixtures of these enzymes, after incubation under controlled conditions, is a rapid method for the evaluation of the relative levels of each enzyme in the mixtures. The method, first developed using pure commercial amylases, is applied, with consistent results, to cell free media ofAspergillus niger cultures on a glycogen-rich effluent.
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  • 95
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Principal components analysis (PCA) ; Iterative target transformation factor analysis (ITTFA) ; Peak labelling ; Chromatographic peak deconvolution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The method of iterative target transformation factor analysis (ITTFA) used in conjunction with second derivative peak finding has shown to be a practical method for the peak deconvolution and reconstruction of HPLC chromatograms and spectra. The second derivative method of peak finding is acceptable for resolutions above 0.5 for peaks of similar heights. Above 0.5 resolution the labelling gives correct results where the spectra are substantially different and also when reasonably similar. Below this value the peak labelling was still accurate where the spectra were different. Solvent effects on the spectra of the compounds studied are small and do not hinder the peak labelling process. Thus small “local” libraries are feasible.
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  • 96
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chlorophyll-bonded stationary phase ; Cyano(pheophytinato a)cobalt(III) ; Pheophytin a
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The separation and determination of the nitrite ion by affinity chromatography is described. The good separation of the nitrite ion was obtained by using cyano-(pheophytinato a)cobalt(III) bonded octadecylsilica as the stationary phase and water of pH 4.3 adjusted by acetic acid as the mobile phase. Conventional ion chromatograph was also used for the analysis of the nitrite ion. For the synthetic samples prepared by mixing the nitrite and nitrate ions, analytical values obtained by affinity chromatography were in agreement with calculated values and close to the analytical values obtained by ion chromatography. In the proposed affinity chromatography, the nitrite and nitrate ions could be determined in the concentration range of 0.15–1.0ppm and 0.1–1.0ppm with relative standard deviations (n=10) of 5.3% and 4.7%, respectively.
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  • 97
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    Chromatographia 28 (1989), S. 27-30 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Atmospheric ammonia ; m-Toluamide derivative ; Annular denuder
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple and reliable method for routine measurement of ammonia in ambient air is described. It is based on the collection of ammonia on H3PO3-coated annular denuders and its subsequent derivatization withm-toluoyl chloride (MTC) in alkaline acetonitrile. The resultingm-toluamide is determined by reversed phase HPLC with UV detection at 230 nm. The limit of dotection is about 0.3μg m−3 for NH3 in air samples collected at 151 min−1 for one hour.
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  • 98
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    Chromatographia 28 (1989), S. 39-44 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thermus aquaticus ; Ribosome ; 50S and 30S subunit proteins ; Gel electrophoresis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The ribosomal 50S and 30S subunit proteins (r-proteins) ofThermus aquaticus have, for the first time, been characterized by size exclusion chromatography (SEC) and by reversed phase high performance liquid chromatography (RPC). To ensure that the best resolution in the RPC was obtained. the elution conditions, such as gradient time, flow rate, temperature, ionic strength of the eluent and the type of stationary phase were optimized. Correlation between experimentally found retention times and those predicted by DryLab G was better than 0.7% over 30 peaks. Protein fractions from RPC runs were desalted and processed by gel electrophoresis so that the ribosomal proteins could be identified by their position on SDS-polyacrylamide gels. The enhanced speed and quality of separation which has been achieved in this study is expected to bring advantaces in experimental work with ribosomal proteins as well as with other biopolymers. In our case the high resolution technique provides a basis for the preparation of a collection of individual ribosomal protein components for future rRNA-protein interaction studies.
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  • 99
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    Chromatographia 27 (1989), S. 321-324 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Simulation of peak profiles ; Rouchon model ; LEA model
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The possibilities and domain of applicability of the ideal chromatography model for calculating peak profiles in non-linear chromatography are analyzed. For this purpose we used the main conclusion of the model of a layer of equilibrium adsorption (LEA model), which determines the difference between ideal and non-ideal chromatography in terms of the relative length of a chromatographic column. It is shown that the experimental data of non-linear high-performance liquid chromatography can be approximated in terms of the elementary analytical relations known in the theory of ideal chromatography.
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  • 100
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    Chromatographia 27 (1989), S. 364-366 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Labetalol ; Separation of racemic diastereomers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A direct, isocratic, reversed phase HPLC procedure is developed for the separation of the diastereomeric racemates of labetalol, a combined α- and β-adrenoreceptor antagonist. The aminoalcohol-type diastereomers were resolved on a C18 column using methanolwater-25% ammonia 27-75-2 mobile phase and detection at 220nm. The procedure is simple and convenient to carry out. The method may be of use in the determination of the individual diastereomeric racemates of labetalol in different forms such as bulk substance, pharmaceutical dosage preparations and biological fluids.
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