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  • Column liquid chromatography  (349)
  • Drosophila  (150)
  • Analytical Chemistry and Spectroscopy
  • Chemistry
  • Life and Medical Sciences
  • Springer  (504)
  • 1985-1989  (504)
  • 1950-1954
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  • 1
    ISSN: 1432-1432
    Keywords: Drosophila ; Foldback element ; Transposable element
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Foldback elements are a family of transposable elements described inDrosophila melanogaster. The members of this dispersed repetitive family have terminal inverted repeats that sometimes flank a central region. The inverted repeats of all the family members are homologous. The study of the distribution and conservation of the foldback elements in differentDrosophila species shows that this distribution is different from that of the hybrid dysgenesis systems (PM and IR). Sequences homologous to foldback elements were observed by Southern blots and in situ hybridization in all species of themelanogaster subgroup and in some species of themontium andtakahashii subgroups. The element was probably already present before the radiation of these subgroups. No evidence of horizontal transmission of the foldback element could be observed.
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  • 2
    Electronic Resource
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    Aquatic sciences 51 (1989), S. 108-128 
    ISSN: 1420-9055
    Keywords: Chemistry ; mountain lakes ; silica ; acidity ; sediment
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Alpine lakes in siliceous catchments of Tyrol and Carinthia (Austria) show signs of acidification. About 9% of the studied lakes have no alkalinity, more than 20% are below pH 6. About two thirds of all lakes have acid neutralizing capacities below 100 μeq 1−1. In spite of moderate precipitation acidity, some lakes show considerable concentrations of dissolved reactive aluminum during or shortly after snowmelt. High altitude lakes of the Alps are definitely more acidic than high mountain lakes in remote areas. Large differences in water and soil chemistry of nearby situated lakes were attributed to heterogeneities of bedrock geology. Paleolimnological investigations on former pH values of five lakes, based on diatom assemblages in the sediment, showed different developments: recent and past acidification, stable conditions, and alkalinization.
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  • 3
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    Development genes and evolution 198 (1989), S. 227-232 
    ISSN: 1432-041X
    Keywords: Campaniform sensilla ; Drosophila ; Achaete-scute complex ; Cis regulatory sites
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary We have analysed the role of the achaete-scute gene complex in the development of the pattern of campaniform sensilla on the wing blade of Drosophila. We show that the complete pattern results from the superimposition of two independent subpatterns, one of which depends on the achaete gene and the other on scute. The scute subpattern comprises several clusters of sensilla, most of which seem to require the presence of control regions located upstream of the transcribed region. This is in contrast with the pattern of scute-dependent bristles, most of which depends on control elements located downstream of the transcribed region.
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  • 4
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    Development genes and evolution 198 (1989), S. 65-77 
    ISSN: 1432-041X
    Keywords: Cell communication ; Pattern formation ; Cell differentiation ; trans-regulatory genes ; Drosophila
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary The effects ofpolyhomeotic (ph) mutants in imaginal cells have been studied in a clonal analysis. Clones of cells, homozygous forph, sort-out after a few divisions, probably as a consequence of modified cell affinities. The dorso-ventral margin of the wing has special characteristics that retard this phenomenon. The formation and exclusion of a clone of 8–16 cells affect the polarity of the wild-type neighbour cells and can provoke pattern triplications. The results suggest that a defect in intercellular communication prevents the wild-type cells from maintaining coordinated positional information. The cells react by regenerative growth, and reorganize into a new pattern. The pleiotropic phenotypes ofph mutants are explained according to a common hypothesis aboutph + function.
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  • 5
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    Development genes and evolution 198 (1989), S. 157-169 
    ISSN: 1432-041X
    Keywords: Distal less ; Limb development ; Drosophila
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary The development of all of the adult limbs inDrosophila depends upon the activity of theDistal-less gene. We report here the phenotypic characterization of a number of hypomorphicDistal-less alleles which indicates that there is a graded requirement forDistal-less activity in the developing limbs. Previous analysis of genetically mosaic animals indicated that cells in the early primordia of the limb imaginal dises possess a graded proximal-distal positional information which depends on the presence of theDistal-less gene for its expression. Taken together these data suggest thatDistal-less may directly encode the graded positional information that is required to organise the proximal-distal axis of the developing limbs.
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  • 6
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    Development genes and evolution 198 (1989), S. 185-190 
    ISSN: 1432-041X
    Keywords: Drosophila ; Oogenesis ; Follicle cells ; Egg shell ; Ovarian tumor
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary The developmental potential of the cells of the somatic follicular epithelium (follicle cells) was studied in mutants in which the differentiation of the germ-line cells is blocked at different stages of oogenesis. In two mutants, sn 36a and kelch, nurse cell regression does not occur, yet the follicle cells around the small oocyte continue their normal developmental program and produce an egg shell with micropylar cone and often deformed operculum and respiratory appendages. Neither the influx of nurse cell cytoplasm into the oocyte nor the few follicle cells covering the nurse cells are apparently required for the formation of the egg shell. In the tumor mutant benign gonial cell neoplasm (bgcn) the follicle cells can also differentiate to some extent although the germ-line cells remain morphologically undifferentiated. Vitelline membrane material was synthesized by the follicle cells in some bgcn chambers and in rare cases a columnar epithelium, which resembled morphologically that of wild-type stage-9 follicles, formed around the follicle's posterior end. The normal polarity of the follicular epithelium that is characteristic for mid-vitellogenic stages may, therefore, be established in the absence of morphologically differentiating germ-line cells. However, the tumorous germ-line cells do not constitute a homogeneous cell population since in about 30% of the analyzed follicles a cell cluster at or near the posterior pole can be identified by virtue of its high number of concanavalin A binding sites. This molecular marker reveals an anteroposterior polarity of the tumorous chambers. In follicles mutant for both bgcn and the polarity gene dicephalic the cluster of concanavalin A-stained germ-line cells shifts to more anterior positions in the follicle.
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  • 7
    ISSN: 1432-1939
    Keywords: Drosophila ; Microbial associations ; Resource partitioning
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary The distributions of five Drosophila species and four components of the microflora have been compared across a total of 48 traps baited with four different fruit and vegetable substrates in two domestic compost heaps in Canberra (Australia). Large and consistent differences are found, both among the Drosophila and among the microbial classes, in their distributions across traps baited with different substrates. Moreover the distribution of each Drosophila species shows a unique set of strong associations with the microbial distributions. Thus the distributions of both D. simulans and D. melanogaster are found to be strongly negatively correlated with the abundance of bacteria while D. simulans is also strongly positively correlated with the titre of fermenter yeasts. D. immigrans is strongly positively correlated both with bacteria and with non-fermenter yeasts. D. hydei is positively correlated with nonfermentery yeasts and D. busckii is negatively correlated with fermenter yeasts. Moulds are the only microbial class not consistently associated with the distribution of any of the Drosophila species. The correlations with the other microbial classes are sufficient to explain the majority of the abundance differences of the Drosophila species among the trap types. It is therefore proposed that the clear partitioning of the fruit resources by the Drosophila is due to their differing primary interactions with the microflora.
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  • 8
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    Journal of comparative physiology 166 (1989), S. 179-187 
    ISSN: 1432-1351
    Keywords: Blowfly ; Drosophila ; Photoreceptor ; Lanthanum ; trp mutant
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary The effect of lanthanum on the light response of blowfly (Calliphora erythrocephala) photoreceptors was studied. The electrophysiological behaviour of the photoreceptors in the presence of La can be summarized as follows: 1. Upon long stimulation the photoreceptors responded with a ‘transient receptor potential’, i.e. the cells depolarized at the onset of the stimulus and then repolarized to (or below) the resting potential. This effect was dependent on stimulus intensity and occurred only at high intensities. During illumination membrane noise was reduced. 2. The light-induced changes in membrane potential were paralleled by changes in membrane resistance. 3. The time course of the receptor response was slowed down. 4. Light adaptation led to an increase in response latency. 5. The recovery of the receptor response after light adaptation was slowed down. 6. The sensitivity of the receptor cells measured by the response to short light stimuli was reduced. In summary, the electrophysiological behaviour of Calliphora photoreceptors in the presence of La was very similar to that of the photoreceptors of the trp (transient receptor potential) mutant of Drosophila melanogaster. This result suggests that La and trp mutation affect the same cellular processes in the photoreceptors.
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  • 9
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    Ecological research 4 (1989), S. 209-218 
    ISSN: 1440-1703
    Keywords: Annual life cycle ; Drosophila ; Fungus preference ; Nematode parasitism
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Food preferences and nematode parasitism were studied in natural populations of mycophagousDrosophila in and near Sapporo, northern Japan. Species which preferred fresh mushrooms showed species-specific responses toPleurotus mushrooms:D. pirka bred only onPleurotus cornucopiae, D. trivitata onP. cornucopiae andP. ostreatus, D. trilineata on these twoPleurotus mushrooms and some other mushrooms, whileD. sexvittata bred on a wide variety of mushrooms but seldom onPleurotus mushrooms. Species which preferred decayed mushrooms (D. quadrivittata, D. histrioides, D. testacea and species of thequinaria species-group) showed host preferences different from those of the above species. The rate of parasitism by nematodes was generally higher in species which prefer decayed mushrooms than in species which prefer fresh mushrooms. Among species which prefer fresh mushrooms, onlyD. trilineata was parasitized frequently by nematodes. It was not clear what factors determine the rate of parasitism in these mycophagousDrosophila. D. pirka, D. trivittata andD. trilineata passed through three or four generations per year and entered reproductive diapause in early September in and near Sapporo.
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  • 10
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    Molecular and cellular biochemistry 90 (1989), S. 27-35 
    ISSN: 1573-4919
    Keywords: zerknullt gene ; homeobox protein ; Drosophila ; filter binding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology , Medicine
    Notes: Summary The region upstream from the zerknullt (zen) gene contains three sites that specifically bind the zen protein product of the gene. Evidence for these binding sites was obtained by the filter binding technique and the DNase footprinting technique. The filter binding technique was used to scan various segments of DNA for the presence of possible specific binding sites. Segments that were selectively retained by the filter binding technique invariably contained one or more specific binding sites according to the DNase footprinting technique. Two of the zen protein binding sites were spaced only 30 base pairs apart. These sites could be separated without any loss in their specific binding properties. It is concluded that these two sites function independently in the binding of zen protein.
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  • 11
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    Biochemical genetics 27 (1989), S. 507-520 
    ISSN: 1573-4927
    Keywords: Drosophila ; sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) ; glue proteins ; glycosylation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The patterns of protein fractions from total salivary glands and from glue plugs were compared in seven members of theDrosophila nasuta subgroup by the use of sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). The glue protein patterns are member specific concerning the numbers and the electrophoretic mobilities of major and minor glue protein fractions. However, the major fractions of all subgroup members could be grouped into five SDS-PAGE domains according to the homologies of their electrophoretic mobilities, prominence of Coomassie blue staining, and PAS reaction. In all subgroup members, major fractions are involved in posttranslational modifications into larger protein molecules of the final glue. Quantitative estimations of the glue proteins inD. n. nasuta andD. n. albomicans reveal that they constitute between 55 and 60% of the total salivary gland proteins, whereas inD. melanogaster and inD. hydei the fraction is only 32 and 35%, respectively.
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  • 12
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    Biochemical genetics 27 (1989), S. 507-520 
    ISSN: 1573-4927
    Keywords: Drosophila ; sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) ; glue proteins ; glycosylation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The patterns of protein fractions from total salivary glands and from glue plugs were compared in seven members of theDrosophila nasuta subgroup by the use of sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). The glue protein patterns are member specific concerning the numbers and the electrophoretic mobilities of major and minor glue protein fractions. However, the major fractions of all subgroup members could be grouped into five SDS-PAGE domains according to the homologies of their electrophoretic mobilities, prominence of Coomassie blue staining, and PAS reaction. In all subgroup members, major fractions are involved in posttranslational modifications into larger protein molecules of the final glue. Quantitative estimations of the glue proteins inD. n. nasuta andD. n. albomicans reveal that they constitute between 55 and 60% of the total salivary gland proteins, whereas inD. melanogaster and inD. hydei the fraction is only 32 and 35%, respectively.
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  • 13
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    Biochemical genetics 27 (1989), S. 263-277 
    ISSN: 1573-4927
    Keywords: Drosophila ; kinetic plate reader ; enzyme polymorphism
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Techniques for performing numerous enzyme kinetic assays with minimum time and effort would be valuable to studies of the evolutionary genetics of metabolic control and the quantitative genetics of determinants of kinetic parameters. Microtiter plate readers have been used for a variety of repetitious analytical techniques, and instruments are available that can take repetitive readings with sufficient speed to perform kinetic assays. The ability of these instruments to assay rapidly the kinetic properties of small samples makes them potentially useful for a number of problems in population genetics. While the ability to handle large numbers of samples is very attractive, the small sample volumes and optical imprecision of microtiter plates result in some sacrifice in accuracy. This paper presents methods for performing kinetic assays on individual field-caughtDrosophila, quantifies the precision of these methods, and characterizes differences amongDrosophila melanogaster andD. simulans from samples caught in California and Pennsylvania. Comparisons between field-caught and laboratory rearedD. melanogaster show that most of the characters are very similar, with the exception of αGPDH, which has a threefold higher mean activity among field-caught flies. The phenotypic correlations are presented with a brief discussion of their relevance to assessing the evolution of metabolic control of these enzymes.
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  • 14
    ISSN: 1573-4927
    Keywords: Drosophila ; aldox-2 ; molybdoenzymes ; sulfite oxidase ; molybdenum ; tungsten
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Mutation at thealdox-2 locus inDrosophila melanogaster affects the specific activities of four molybdoenzymes differentially during development. Sulfite oxidase activity is normal during late larval and pupal stages but is reduced during early adult stages inaldox-2 organisms. There was complete concordance among the effects ofaldox-2 on sulfite oxidase, aldehyde oxidase, xanthine dehydrogenase, and pyridoxal oxidase, when 38 stocks were analyzed which were derived from single recombination events betweenc andpx, markers which flankaldox-2. Several different biochemical analyses indicate that the active molybdoenzymes present in thealdox-2 strain are normal with respect to size, shape,pH-activity profile,K m , and molecular weight. Significant differences were found between thealdox-2 strain and the OR control strain in their responses to dietary Na2MoO4 and Na2WO4. The mutant strain is much more resistant to the effects of dietary Na2WO4 and much more responsive to the administration of Na2MoO4 than the OR control strain when these effects are quantitated by measurements of molybdoenzyme specific activities. This evidence suggests that thealdox-2 + gene product has a molybdenum binding site which can also bind tungsten and that this site is altered in the mutant strain. The hypothesis presented explains the observed effects of thealdox-2 mutation and relates them to the other mutations reported in this gene-enzyme system.
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  • 15
    ISSN: 1573-3297
    Keywords: Drosophila ; circadian clock ; ultradian oscillations ; disconnected mutant ; visual system
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Psychology
    Notes: Abstract Free-running locomotor activity and eclosion rhythms ofDrosophila melanogaster, mutant at thedisconnected (disco) locus, are substantially different from the wild-type phenotype. Initial periodogram analysis revealed little or no rhythmicity (Dushayet al., 1989). We have reanalyzed the locomotor activity data using high-resolution signal analysis (maximum-entropy spectral analysis, or MESA). These analyses, corroborated by autocorrelograms, uncovered significant residual circadian rhythmicity and strong ultradian rhythms in most of the animals tested. In this regard thedisco mutants are much like flies expressing mutant alleles of theperiod gene, as well as wild-type flies reared throughout life in constant darkness. We hypothesize that light normally triggers the coupling of multiple ultradian oscillators into a functional circadian clock and that this process is disrupted indisco flies as a result of the neural lesion.
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  • 16
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    Theoretical and applied genetics 77 (1989), S. 123-127 
    ISSN: 1432-2242
    Keywords: Inbreeding depression ; Drosophila ; Natural selection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary This experiment was designed to study the relationship between rate of inbreeding and observed inbreeding depression of larval viability, adult fecundity and cold shock mortality in Drosophila melanogaster. Rates of inbreeding used were full-sib mating and closed lines of N=4 and N=20. Eight generations of mating in the N=20 lines, three generations in the N=4 lines and one generation of full-sib mating were synchronised to simultaneously produce individuals with an expected level of inbreeding coefficient (F) of approximately 0.25. Inbreeding depression for the three traits was significant at F=0.25. N=20 lines showed significantly less inbreeding depression than full-sib mated lines for larval viability at approximately the same level of F. A similar trend was observed for fecundity. No effect of rate of inbreeding depression was found for cold shock mortality, but this trait was measured with less precision than the other two. Natural selection acting on loci influencing larval viability and fecundity during the process of inbreeding could explain these results. Selection is expected to be more effective with slow rates of inbreeding because there are more generations and greater opportunity for selection to act before F=0.25 is reached. Selection intensities seem to have been different in the three traits measured. Selection was most intense for larval viability, less intense for fecundity and, perhaps, negligible at loci influencing cold shock mortality.
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  • 17
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    Theoretical and applied genetics 77 (1989), S. 253-259 
    ISSN: 1432-2242
    Keywords: Heterosis ; Selection ; Drosophila ; Genotype x environment
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Experiments were designed to examine whether heterosis would occur in crosses of Drosophila melanogaster populations adapted to 18 °C or 28 °C environments. Crosses were examined in parental environments, an intermediate environment (23 °C) and a mixed environment (alternating 18°/28°C). Parental populations did not show divergence for larval viability, cold shock or high temperature mortalities when tested in a common environment. However, the 28 °C population was less fecund than the 18 °C population, but had higher larval competitive ability and higher adult longevity. Heterosis for viability, cold shock mortality and high temperature mortality occurred in crosses between a population adapted to 18 °C and another adapted to 28 °C, but not in crosses between two populations adapted to the same temperature. The results suggest that, in the absence of drift, heterosis is expected in crosses between lines or populations with different histories of selection but not between lines with the same selection histories.
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  • 18
    ISSN: 1617-4623
    Keywords: Drosophila ; Vestigial ; Dihydrofolate reductase ; Aminopterin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Vestigial (vg) mutants of Drosophila melanogaster are characterized by atrophied wings. In this paper we show that: (1) aminopterin an inhibitor of dihydrofolate reductase (DHFR) and fluorodeoxyuridine (FUdR), an inhibitor of thymidylate synthetase induce nicks in the wings of wild-type flies and phenocopies of the vg mutant phenotype when vg/+ and vg B/+ flies are reared on these substances (vgB is a deficiency of the vg locus). Only thymidine and thymidylate can rescue the flies from the effect of aminopterin. We propose that the vg phenotype is due to a decrease in the dTMP pool in the wings. (2) Mutant vg strains yield more offspring on medium containing aminopterin than on normal medium. The resistance of vg larvae to the inhibitor seems specific to the gene. This is the first case of aminopterin resistance in living eucaryotes. In contrast sensitivity of the vg larvae to FUdR is observed. (3) An increase in the activity and amount of DHFR is observed in mutant strains as compared with the wild-type flies. Our data suggest that the vg + gene is a regulatory gene acting on the DHFR gene or a structural gene involved in the same metabolic pathway.
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  • 19
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    Molecular genetics and genomics 218 (1989), S. 118-126 
    ISSN: 1617-4623
    Keywords: Drosophila ; Regulation ; yellow gene ; Germline transformation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary We have assessed the DNA sequence requirements for the correct spatial pattern and phenotypic expression of y in the late embryo/larvae. The wild-type larval phenotype requires both the regions between-294 bp and-92 bp and a portion of the intron; the sequence element(s) located within the intron can act in a position independent manner to effect the wild-type larval phenotype. The larval expression pattern was examined by tissue experiments in situ and by staining germline transformants derived from various y/lacZ fusion constructs. The larval expression of y is restricted to the mouthparts, microsetae and anal plates. While the-495 bp to+194 bp region alone cannot effect a wild-type larval expression pattern, this region in conjunction with the intron appears to be sufficient to drive β-gal expression in an essentially wild-type pattern. Our data further suggest that the-294 bp to-92 bp region contains elements which specify the larval pattern and that the element(s) in the intron normally act to enhance the level of expression necessary for the wild-type larval phenotype. We also present a phenotypic analysis of the adult cuticle structures of germline transformants derived from a variety of deletion and rearrangement constructs of the y gene. This analysis has revealed several new features associated with the regulation of y expression.
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  • 20
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    Molecular genetics and genomics 215 (1989), S. 281-285 
    ISSN: 1617-4623
    Keywords: Drosophila ; achaete-scute complex ; myc ; Protein domains ; Genomic search
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Several genes of the achaete-scute complex (ASC) of Drosophila melanogaster encode a 60 amino acids long conserved domain which shares a significant homology with a region of the vertebrate myc proteins. Based on these results, the existence of a family of Drosophila genes that would share both this conserved domain and the neurogenic function of the AS-C has been postulated. To test this proposal, we have searched a D. melanogaster genomic library with a probe that encodes the conserved domain. Only under very low stringency hybridization conditions, clones not belonging to the AS-C cross-hybridized with the probe. Those that gave the strongest signals were characterized. Sequencing of the cross-hybridizing regions showed that they had no significant homology with the conserved domain, the sequence similarity extending at the most for 37 nucleotides. Although our results do not conclusively disprove the existence of a family of AS-C-like genes, they indicate that the conservation of the domain would be lower than that found for shared motifs in other families of Drosophila developmental genes.
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  • 21
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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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  • 22
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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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  • 23
    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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  • 24
    ISSN: 1573-8477
    Keywords: Genetic elements ; isozymes ; life span ; Drosophila
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Analysis of electrophoretic loci shows that at least four differences exist in isozymes of long- and short-lived populations ofD. melanogaster, descended by selection from a common ancestral stock. Adults of longlived populations differ in gene dosage of phosphoglucomutase (PGM), NAD malate dehydrogenase (MHD), NADP malic enzyme (ME) and by additional mobility variants of glucose-6-phosphate dehydrogenase (G6PD). Larvae, however, differ only by variants of G6PD. The differences in these enzymes, considered together with the greater flight endurance that long-lived populations have shown elsewhere, suggest that increased glycogen synthesis plays a significant role in the improved life span of selected populations. Adaptation to selection for increased life span may, therefore, derive from an improved ability to use dietary sucrose in the media provided. The distribution of electrophoretic loci agrees with the results of a study indicating the position of genetic elements contributing to life span.
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  • 25
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    Evolutionary ecology 3 (1989), S. 189-201 
    ISSN: 1573-8477
    Keywords: Developmental homeostasis ; life history traits ; Drosophila ; breeding site variation ; cactus ; Sonoran desert
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Variation in life histories among populations of cactophilicDrosophila mojavensis has been hypothesized to be a by-product of a shift to one of two alternate host plants. When cultured on the ancestral and a secondary host cactus, a Baja population expressed shorter development times and smaller thorax sizes than a mainland population, but viability did not differ. Comparisons with all reciprocal F1 and F2 crosses between populations revealed that genetic differences in development time and thorax size were largely additive. Homeostasis in these life history traits was population specific, except for viability. Homeostasis in development time was greater in the Baja population than in the other crosses, suggesting dominance for decreased homeostasis in the mainland population. Underdominance in viability homeostasis of the F1 hybrids suggested some incompatibility between populations. Homeostasis in thorax size was greater in females than in males and differed among parental populations. Maintenance of heritable differences and genetic variation for homeostasis in these traits suggested a role for cactus-specific differences in environmental uncertainty caused by variation in breeding site duration and abundance in nature.
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  • 26
    ISSN: 1617-4623
    Keywords: Chromosomal walking ; Cut locus ; Drosophila ; Unstable mutations
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    Topics: Biology
    Notes: Abstract We have cloned from the Oregon R strain of Drosophila melanogaster a 240 kb segment of DNA that contains the cut (ct) locus, and characterized the region for the presence of repetitive elements. Within this region at least five copies of the suffix element were detected, as well as several putatively novel mobile elements. A number of mutations obtained from the unstable ct MR2 strain and its derivatives were mapped within the cut locus. Comparison between parental and daughter strains indicates that frequently two or more independent transposition events involving the cut locus occur simultaneously within a single germ cell, thus providing a molecular basis for the transposition explosion phenomenon.
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  • 27
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    Molecular genetics and genomics 219 (1989), S. 397-403 
    ISSN: 1617-4623
    Keywords: Drosophila ; Pyrimidine biosynthesis ; Dihydroorotate dehydrogenase ; Molecular mapping
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    Topics: Biology
    Notes: Summary The dhod locus encodes dihydroorotate dehydrogenase, the fourth enzymatic step of de novo pyrimidine biosynthesis. This locus was cloned previously by a chromosome walk in cytogenetic region 85A. The location of dhod within 85A DNA has been determined by mapping two rearrangement mutations to a small DNA region. A nearly full-length cDNA clone of the dhod transcript was isolated and partially sequenced, to confirm its identity. The cDNA clone was also used to map the transcribed DNA. A 1.5 kb dhod RNA is described which is most abundant in embryos and displays minor length heterogeneity in pupae and adults. The developmental expression of this transcript is discussed relative to the expression of dihydroorotate dehydrogenase activity and other genes of the pyrimidine biosynthetic pathway.
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  • 28
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    Molecular genetics and genomics 215 (1989), S. 190-199 
    ISSN: 1617-4623
    Keywords: Mutagen sensitivity ; Recombination ; Gene structure ; Drosophila ; mei-41
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    Topics: Biology
    Notes: Summary The mutagen-sensitive mutant mus(1)104 D1 of Drosophila melanogaster maps to a position on the X chromosome very close to the meiotic mutant mei-41 D5 . Both mutants have been characterized as mutagen-sensitive and defective in post-replication repair. In the present report we show by complementation studies that mus(1)104 and mus(1)103 are allelic with mei-41. In addition, two reported alleles of mus(1)104 lie between the mei-41 alleles A10 and D5. The size of the mei-41 locus is estimated to be about 0.1 centimorgans (cM). Because several alleles of mei-41 have been shown to reduce recombination and increase meiotic chromosome loss and nondisjunction, mus(1)104 D1 females were examined for defects in meiosis. Although there was no evidence for reduced recombination on the second chromosome in homozygous mus(1)104 D1 females, heterozygous mus(1)104 D1 /mei-41 〉D5 and mus(1)104 D1 /deficiency females showed reduced levels of recombination. However, there was no evidence of an increase in nondijunction in these females.
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  • 29
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    Molecular genetics and genomics 215 (1989), S. 257-265 
    ISSN: 1617-4623
    Keywords: Drosophila ; Maternal effect ; Syngamy ; Embryonic development ; Molecular cloning
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    Topics: Biology
    Notes: Summary The maternal effect locus fs(1) Ya is required for the fusion of the apposed sperm and egg pronuclei (syngamy) following fertilization in Drosophila. It is tightly linked to another complementation group, fs(1) Yb, needed for both oogenesis and embryogenesis. We have isolated a set of overlapping cloned sequences in the 3B4-6 region of the X chromosome encompassing the fs(1) Ya-fs(1) Yb region. A single 2.4 kb maternal transcript is encoded with-in this region, and an 8.5 kb DNA fragment that contains this transcript complements both fs(1) Ya and fs(1) Yb mutations. Northern and in situ hybridization analyses show that the maternal transcript is only present in nurse cells and oocytes beginning in previtellogenic stages, and is evenly distributed in the cytoplasm of 0–2 h syncytial embryos. The transcript is not detected in later stages of embryonic development. This expression pattern correlates closely with the genetic and developmental characteristics expected of the fs(1) Ya gene product.
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  • 30
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    Molecular genetics and genomics 215 (1989), S. 469-477 
    ISSN: 1617-4623
    Keywords: Drosophila ; Y chromosome ; Repetitive DNA ; Testis RNA ; Transposable elements
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    Topics: Biology
    Notes: Summary A cDNA clone bank was constructed from testis poly(A)+ RNA of Drosophila hydei and screened for clones which hybridize to Y chromosomal DNA sequences. The insert of clone cDhT14 hybridizes to a family of repeated DNA sequences with members distributed within the Y chromosome and elsewhere in the genome. This type of sequence has earlier been described as the Y-associated class of DNA. Southern blot analysis of DNA from different wild-type strains of D. hydei suggests that members of the T14 family of repeated DNA sequences are parts of a family of transposable elements. The genomic localization of the T14 family of repeated DNA sequences was revealed by in situ hybridization to metaphase and polytene chromosomes, and to transcripts of Y chromosomal lampbrush loops. Approximately 10–15 members (20%–30%) of the T14 sequence family reside in 8.3 kb PstI restriction fragments. A genomic clone of one of these DNA fragments, DhT14-8.3, hybridizes to transcripts on the Y chromosomal lampbrush loop “cones”, and in conventional in situ hybridization experments to region 12D/13A of the X chromosome and to region 112 of chromosome 5. The cDNA clone cDhT14 represents a part of an abundant testis RNA species of 5.0 kb. This RNA is also present in ovaries and in 0–3 h, 3–6 h and 6–12 h embryos, but less abundantly than in testes. Both the Y chromosomal site of the 8.3 kb PstI fragments and sites elsewhere in the genome are actively transcribed. At least one of the latter genomic sites is transcribed into the 5.0 kb RNA species. This poly(A)+ RNA is present in the cytoplasm of primary spermatocytes as shown by transcript in situ hybridization. The potential function of transcripts from Y chromosomal lampbrush loops is discussed.
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  • 31
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    Journal of comparative physiology 159 (1989), S. 237-242 
    ISSN: 1432-136X
    Keywords: Amylase ; Mosquitofish ; Rat ; Drosophila ; Structure ; Function
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    Topics: Biology , Medicine
    Notes: Summary Amylases from the mosquitofish (Gambusia affinis holbrooki, Pisces: Poeciliidae) and rat were purified and compared withDrosophila amylases in terms of structure and function. At the structural level, amino acid compositions of the three amylases were compared. At the functional level, amylase activities were compared on various substrates and in the presence of inhibitors. While the amylases from all three organisms had properties typical of alpha-amylases, both structural and functional differences were observed. Using resemblance coefficients of distance and similarity from numerical taxonomy, it was determined that the amylases from the rat andDrosophila were more similar to each other than either was to amylase from the mosquitofish, and that structural differences between the amylases did not reflect functional differences, i.e. there was no correlation between amylase structural and functional distances.
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  • 32
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Microcrystalline cellulose triacetate ; Molecular modeling ; Computer graphics
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    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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  • 33
    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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  • 34
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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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  • 35
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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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  • 36
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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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    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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  • 38
    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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  • 39
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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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  • 40
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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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  • 41
    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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  • 42
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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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  • 43
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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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  • 44
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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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  • 45
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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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  • 46
    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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  • 47
    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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  • 48
    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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  • 49
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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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    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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  • 51
    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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    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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  • 53
    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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    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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  • 55
    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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  • 56
    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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  • 57
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    Chromatographia 28 (1989), S. 129-132 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carotenoids ; Paprika, Rose hips, Marigold
    Source: Springer Online Journal Archives 1860-2000
    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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  • 58
    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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  • 59
    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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  • 60
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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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  • 61
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Optical resolution ; Polymeric adsorbents ; Penicillin sulfoxide ; Substituent effect
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    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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  • 62
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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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  • 63
    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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  • 64
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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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  • 65
    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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  • 66
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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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  • 67
    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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  • 68
    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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  • 69
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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
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    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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  • 70
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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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  • 71
    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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  • 72
    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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  • 73
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Normal phase elution ; Silica and cyano columns ; Flavonoid compounds
    Source: Springer Online Journal Archives 1860-2000
    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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  • 74
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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
    Source: Springer Online Journal Archives 1860-2000
    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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  • 75
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    Chromatographia 27 (1989), S. 325-327 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carotenoid ; Xanthophyll ; Broccoli ; Paprika
    Source: Springer Online Journal Archives 1860-2000
    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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  • 76
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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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  • 77
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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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  • 78
    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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  • 79
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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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  • 80
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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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  • 81
    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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    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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  • 83
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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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  • 84
    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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  • 85
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Molecular interactions ; Association effects ; Analyte solvation
    Source: Springer Online Journal Archives 1860-2000
    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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  • 86
    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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  • 87
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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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  • 88
    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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  • 89
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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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  • 90
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion-exchange ; Mobile phase optimisation ; Egg-white proteins
    Source: Springer Online Journal Archives 1860-2000
    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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  • 91
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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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  • 92
    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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  • 93
    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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  • 94
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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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  • 95
    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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  • 96
    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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  • 97
    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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  • 98
    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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  • 99
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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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  • 100
    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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