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  • Column liquid chromatography  (495)
  • photosynthesis  (262)
  • Springer  (757)
  • 2000-2004  (50)
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  • 1
    ISSN: 1570-7458
    Keywords: Vitis vinifera ; Empoasca vitis ; leafhopper ; photosynthesis ; transpiration ; stomatal conductance ; mesophyll conductance ; growth ; yield ; fruit quality ; starch ; carbohydrate reserves
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The impact of the grape leafhopper,Empoasca vitis, on leaf gas exchange, plant growth, yield, fruit quality and carbohydrate reserves of the grapevines,Vitis vinifera L., was studied. Gas exchange was measured on the discolored (red) and the green parts of infested main leaves and on leaves from uninfested vines. Photosynthesis and mesophyll conductance were severely reduced on main leaves showing leafhopper feeding symptoms. The stomatal conductance of the red leaf section of infested main leaves was lower than on undamaged control leaves. Additionally, the red leaf section of infested main leaves showed lower transpiration rates when compared to the green parts of the same leaves and to undamaged control leaves. Gas exchange processes of lateral leaves were not affected by leafhopper feeding. Leafhopperload on main leaves was correlated to visual damage symptoms. At 71.8 leafhopper-days per leaf up to 40% of the main leaf area of the infested plants was discolored from the borders towards the center. Lateral leaves showed no feeding symptoms. Shoot diameter, pruning weight and carbohydrate reserves in the wood were not affected by leafhoppers. Lateral leaf area growth was significantly stimulated on plants infested by leafhoppers. No decrease in yield and fruit quality with leafhopper-loads up to 71.8 leafhopper-days per leaf were observed.
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  • 2
    Electronic Resource
    Electronic Resource
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    Entomologia experimentalis et applicata 63 (1992), S. 101-102 
    ISSN: 1570-7458
    Keywords: Cnaphalocrosis medinalis ; rice leaffolder ; Oryza sativa ; rice ; photosynthesis ; transpiration
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
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  • 3
    ISSN: 1572-8773
    Keywords: Chorella vulgaris ; acid tolerance ; ATPase ; nickel toxicity ; nutrient uptake ; photosynthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract This study concerns the inhibitory effects of acid pH and nickel on growth, nutrient (NO3 - and NH4 +) uptake, carbon fixation, O2 evolution, electron transport chain and enzyme (nitrate reductase and ATPase) activities of acid tolerant and wild-type strains of Chlorella vulgaris. Though a general reduction in all these variables was noticed with decreasing pH, the tolerant strain was found to be metabolically more active than the wild-type. A reduced cation (NH4 +, Na+, K+ and Ca2+) uptake, coupled with a facilitated influx of anions (NH4 +, PO4 3- and HCO3 -), suggested the development of a positive membrane potential in acid tolerant Chlorella. Nevertheless, a tremendous increase in ATPase activity at decreasing pH revealed the involvement of superactive ATPase in exporting H+ ions and keeping the internal pH neutral. A difference in Na+ and K+ efflux of the two strains at decreasing pH suggests there is a difference in membrane permeability. The low toxicity of Ni in the acid tolerant strain may be due to the low Ni uptake brought about by a change in membrane potential as well as in permeability. Hence, the development of superactive ATPase and a change in both membrane potential and permeability not only offers protection against acidity, but also co-tolerance to metals.
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  • 4
    ISSN: 1420-9055
    Keywords: Phytoplankton ; primary production ; photosynthesis ; optics ; adaptation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract This tutorial was designed for nonbiologists requiring an introduction to the nature and general timescales of phytoplankton responses to physical forcing in aquatic environments. As such, an effort was made to highlight biological markers which might assist in identifying, measuring and/or validating physical processes controlling the variability in the distribution, abundance, composition and activity of phytoplankton communities. Given the recent advances in environmental optics and remote sensing capabilities, a special emphasis was placed on the nature and utility of phytoplankton optical properties in current bio-optical modelling efforts to predict temporal and spatial variability in phytoplankton productivity and growth.
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  • 5
    Electronic Resource
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    Springer
    BioMetals 5 (1992), S. 149-156 
    ISSN: 1572-8773
    Keywords: Hg2+ toxicity ; cyanobacterium ; Nostoc calcicola ; growth ; photopigments ; nucleic acids ; photosynthesis ; membrane integrity ; nutrient uptake ; enzymes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Toxicological responses of the filamentous N2-fixing cyanobacteriumNostoc calcicola Bréb. towards Hg2+ were studied to enumerate the decisive lethal events. In low-dose, long-term experiments (0.05–0.25 μm Hg2+, 10 days), photoautotrophic growth was severely inhibited with concurrent loss of photosynthetic pigments (phycocyanin〉chlorophyll α〉carotenoids) and nucleic acids. The termination of growth after a day 4 exposure to 0.25 μm Hg2+ has been attributed to the complete inhibition ofin vivo photosynthetic activity in the cyanobacterium (O2 evolution〉14CO2 incorporation). The elevated Hg2+ concentrations irreversibly damaged the cell membrance as observed under light microscopy, and as indicated by the leakage of intracellular electrolytes and phycocyanin. In high-dose, short-term experiments (0.5–20.0 μm Hg2+, up to 6 h), thein vivo activities of selected enzymes (glutamine synthetase 〉 nitrate reductase 〉 nitrogenase) were less inhibited by Hg2+ than the uptake of nutrient ions (NH 4 + 〉NO 3 − 〉PO 4 3− ).
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  • 6
    Electronic Resource
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    Aquatic sciences 54 (1992), S. 321-330 
    ISSN: 1420-9055
    Keywords: Algal pigments ; algal communities ; photosynthesis ; Lake Lugano (Lago di Lugano)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract A one-year study of phytoplankton, primary production and related physical and chemical factors was made in a Swiss basin of Lake Lugano (Lago di Lugano). The chlorophylls and 12 carotenoids were analyzed with a TLC technique. The carotenoid monitoring was considered to be particularly interesting, because the role of these pigments in freshwater algae is still very poorly documented by field studies. The dependence of photosynthesis on several factors was statistically evaluated. Evidence was found of light-adaptation phenomena. The variations of photosynthetic activity and efficiency largely depended on the light regime in the few days before the field observations and on the cellular content of chlorophylls and single carotenoids, whose concentrations in their turn were closely linked with light, temperature, average cell size, and with the actual species assemblage.
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  • 7
    ISSN: 1440-1703
    Keywords: Clethra barbinervis ; interspecific difference ; intraspecific variation ; photosynthesis ; SO2 resistance
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The effect of SO2 on the photosynthesis ofClethra barbinervis collected from a smoke-polluted area near the Ashio copper smelter in Tochigi Prefecture was compared withC. barbinervis collected from a nonpolluted district in Tsukuba, Ibaraki Prefecture andQuercus mongolica var.grosseserrata grown in a nonpolluted field in Nagano Prefecture. The plants were exposed to 0.5–1.5 p.p.m. SO2 for 90 min (short-term) and to 0.3 p.p.m. SO2 for 31–39 days (long-term). TheClethra plants from both sites had a lower intrinsic stomatal conductance and photosynthetic rate thanQuercus plants. Short-and long-term fumigation caused stomatal closure inQuercus plants, but had little effect on the stomatal conductance ofClethra plants. Under short-term fumigation, nonstomatal photosynthetic inhibition per unit of absorbed SO2 was smallest inClethra plants from Ashio. Long-term fumigation caused photosynthetic decline and visible foliar injury toQuercus plants, but had no effect onClethra plants from Ashio. Consequently,Clethra plants from Ashio had a higher photosynthetic rate thanQuercus plants after long-term fumigation. These results suggest thatC. barbinervis populations in the smoke-polluted area of Ashio had evolved high SO2 resistance connected with SO2 detoxification ability in mesophyll cells.
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  • 8
    ISSN: 1440-1703
    Keywords: photosynthesis ; Prunus avium ; relative growth rate ; shading ; total plant water use efficiency
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Cherry (Prunus avium L.) saplings were grown under natural sunlight (controls) or moderate shading (up to 30%, depending on the incident light intensity and the hour of the day). Reduced light intensity increased the dry mass of each of the plant components studied. Consequently, the total dry mass of shaded plants was significantly greater than that of controls at the end of the growing season. However, the diurnal trend in the level of photosynthesis (per unit of leaf area) of shaded plants was similar to the controls in August, but lower in September. As the growing season proceeded, reduced photosynthetic rates, thinner mesophyll and larger specific leaf area in the shaded plants indicated that leaf development had adapted to shaded conditions throughout the growing season. It is suggested that increased growth of shaded plants was caused by a higher initial relative growth rate and a greater whole-plant photosynthesis. Shading consistently reduced transpiration over the season, therefore improving water use efficiency of shaded leaves. Our results suggest that a moderate reduction in light intensity can be a useful method for improving growth and saving water in hot and dry environments.
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  • 9
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    Ecological research 8 (1993), S. 81-83 
    ISSN: 1440-1703
    Keywords: bract ; Carpinus laxiflora ; mast year ; photosynthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Light saturated net photosynthesis was measured in bracts and leaves ofCarpinus laxiflora, the major species in secondary forests in cool and intermediate temperate zones in Japan. The maximum net photosynthesis of leaves and bracts was essentially constant from May to early August and decreased gradually thereafter. For bracts, it was 3.2 μmol m−2s−1, approximately half that for the leaves. The photosynthesis of bracts would thus appear to contribute significantly to seed maturity. The estimated production of bract based on the photosynthesis would make seeds (3 mg dry weight) mature for 37 days, assuming all photosynthate of the bracts to have been distributed in the seeds only. This was quite consistent with the growth curve for the seeds. A mast year phenomenon is discussed in relation to bract photosynthesis and leaf number.
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  • 10
    ISSN: 1440-1703
    Keywords: Aucuba japonica ; photosynthesis ; Sea of Japan ; shading ; snow cover
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Aucuba japonica varieties are common evergreen understory shrubs in Japan.Aucuba japonica var.borealis is distributed on the Sea of Japan side of Honshu and Hokkaido where heavy snow cover lasts for more than 3 months in winter.Aucuba japonica var.japonica is distributed in areas with shallow or no snow on the Pacific Ocean side of Honshu and Shikoku. The ecophysiological characteristics of var.borealis were compared with those of var.japonica to examine the effects of heavy and long-term snow cover on the life cycle of var.borealis. Shoots of both varieties were shaded in crushed ice for 110 days, but their photosynthetic activities, chlorophyll contents and the chlorophylla/b ratio was not affected. The leaves of var.borealis were no less frost tolerant than those of var.japonica. In spite of the difference in environmental factors, both varieties had similar characteristics in seasonal changes of photosynthesis, respiration and chlorophylla/b ratio. These results suggest that var.japonica could survive in areas with heavy snow where it does not normally occur. Leaf net production (LNP) was estimated based on the microclimatic data and seasonal photosynthetic and respiration rates. The difference in the annual LNP between the two varieties was equivalent to the difference in the LNP during the snow season. One of the major effects of snow cover is to interrupt and reduce the production period of var.borealis.
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  • 11
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    Journal of chemical ecology 19 (1993), S. 559-568 
    ISSN: 1573-1561
    Keywords: Juglone ; allelopathy ; allelochemical ; photosynthesis ; chioroplast ; mitochondria ; Lemna minor ; Glycine max
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The impacts of juglone on plant growth and several other physiological functions were evaluated in this study. Juglone inhibitedLemna minor growth, chlorophyll content, and net photosynthesis at treatments between 10 and 40μM. Soybean leaf disks vacuum infiltrated with as little as 10μM juglone had reduced photosynthesis. Oxygen evolution by chloroplasts isolated fromPisum sativum was inhibited by juglone with an I50 of 2μM. Micromolar treatments of juglone stimulated oxygen uptake in mitochondria isolated fromGlycine max. These data suggest perturbations of chloroplast and mitochondrial functions may contribute to plant growth reductions observed in juglone-mediated allelopathy.
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  • 12
    ISSN: 1573-5028
    Keywords: gene duplication ; photosynthesis ; RFLP ; Southern blots
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract A second locus (Lhb1B) encoding Photosystem II Type I chlorophyll a/b-binding (CAB) polypeptides was identified in Arabidopsis thaliana. This locus carries two genes in an inverted orientation. The predicted sequences of the polypeptides encoded by these two genes show substantial divergence in their amino termini relative to each other and to the proteins encoded by the three Lhb1 CAB genes previously characterized [10], but little divergence within the predicted primary structure of the mature protein. DNA probes derived from seven additional types of tomato CAB genes, encoding chlorophyll a/b-binding polypeptides of several antenna systems of the photosynthetic apparatus, were tested against A. thaliana. Each of these hybridized in Southern blots to unique DNA fragment(s), demonstrating the existence of each of these different types of CAB genes in the genome of A. thaliana. The number of genes encoding each CAB type in A. thaliana was estimated to be similar to that of tomato.
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  • 13
    ISSN: 1573-5028
    Keywords: carbonic anhydrase ; antisense ; over-expression ; tobacco ; photosynthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The activity and location of carbonic anhydrase has been modified by transformation of tobacco with antisense and over-expression constructs. Antisense expression resulted in the inhibition of up to 99% of carbonic anhydrase activity but had no significant impact on net CO2 assimilation. Stomatal conductance and susceptibility to water stress appeared to increase in response to the decline in carbonic anhydrase activity. An over-expression construct designed to increase cytosolic carbonic anhydrase abundance resulted in a significant increase in net activity, a small increase in stomatal conductance but little impact on CO2 assimilation. Chloroplastic carbonic anhydrase activity was enhanced by the expression of an additional construct which targeted the polypeptide to the organelle. The increase in chloroplastic carbonic anhydrase appeared to be accompanied by a concomitant increase in Rubisco activity.
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  • 14
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    Plant molecular biology 20 (1992), S. 481-491 
    ISSN: 1573-5028
    Keywords: photosynthesis ; cytochrome b 6 ; gene regulation ; genome mapping
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The genes encoding the photosynthetic cytochrome b 6 (petB) and subunit 4 (petD) have been cloned and sequenced from the unicellular, photoheterotrophic, transformable cyanobacterium Synechococcus sp. PCC 7002, formerly designated Agmenellum quadruplicatum. The gene arrangement was found to be similar to that reported in the cyanobacterium Nostoc PCC 7906. The DNA and derived protein sequences were compared to chloroplast and the other cyanobacterial sequences. By pulsed-field electrophoresis, the petBD operon and the petCA operon, encoding the Rieske iron-sulfur protein and cytochrome f, were found to be located on separate, unlinked,Not I-digested DNA fragments. ThepetBD operon was found on the third largest Not I fragment (NC-325) while the petCA operon was found on the second largest Not I fragment (NB-370). These results suggest the two operons are not in proximity. The 1.35 kb transcript was shown to be light-regulated. Transcripts from cells grown under constant illumination showed a decrease in petB transcript levels to undetectable levels within 2 h after the cells were placed in the dark. Upon reillumination, transcript levels rose to three-fold over that seen initially under constant illumination.
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  • 15
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    Bioscience reports 11 (1991), S. 539-571 
    ISSN: 1573-4935
    Keywords: proton translocation ; respiration ; photosynthesis ; quinones ; bc complexes ; cytochrome oxidase ; NADH-quinone oxidoreductase
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Detailed molecular mechanisms of electron transfer-driven translocation of ions and of the generation of electric fields across biological membranes are beginning to emerge. The ideas inherent in the early formulations of the chemiosmotic hypothesis have provided the framework for this understanding and have also been seminal in promoting many of the experimental approaches which have been successfully used. This article is an attempt to review present understanding of the structures and mechanisms of several osmoenzymes of central importance and to identify and define the underlying features which might be of general relevance to the study of chemiosmotic devices.
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  • 16
    ISSN: 1573-5028
    Keywords: chlorophyll-binding proteins ; photosynthesis ; photosystem II ; site-directed mutagenesis ; Synechocystis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract A mutant strain of the cyanobacterium Synechocystis sp. PCC (Pasteur Culture Collection) 6803 has been developed in which psbB, the gene coding for the chlorophyl a-binding protein CP47 in Photosystem II (PSII), has been deleted. This deletion mutant can be used for the reintroduction of modified psbB into the cyanobacterium. To study the role of a large hydrophilic region in CP47, presumably located on the lumenal side of the thylakoid membrane between the fifth and sixth membrane-spanning regions, specific deletions have been introduced in psbB coding for regions within this domain. One psbB mutation leads to deletion of Gly-351 to Thr-365 in CP47, another psbB mutation was targeted towards deletion of Arg-384 to Val-392 in this protein. The deletion from Gly-351 to Thr-365 results in a loss of PSII activity and of photoautotrophic growth of the mutant, but the deletion between Arg-384 and Val-392 retains PSII activity and the ability to grow photoautotrophically. The mutant strain with the deletion from Gly-351 to Thr-365 does not assemble a stable PSII reaction center complex in its thylakoid membranes, and exhibits diminished levels of CP47 and of the reaction center proteins D1 and D2. In contrast to the Arg-384 to Val-392 portion of this domain, the region between Gly-351 and Thr-365 appears essential for the normal structure and function of photosystem II.
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  • 17
    ISSN: 1573-5028
    Keywords: cyanobacterial mutant ; membrane assembly ; PsaE ; photosystem I ; photosynthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract We studied assembly of the PsaE subunit of photosystem I into photosynthetic membranes of cyanobacterial mutant strains that lack specific photosystem I subunits. Radiolabeled PsaE was incubated with photosynthetic membranes, and their binding and assembly were assayed by resistance to removal by chaotropic agents and proteolytic digestion. PsaE incorporated into the wild-type membranes was resistant to these treatments. In the absence of PsaD, it was resistant to proteolytic digestion, but was removed by NaBr. When the membranes were isolated from a mutant strain in which the psaF and psaJ genes have been inactivated, PsaE assembled in vitro could not be removed. PsaE could associate with the membranes of the strain DF in which the psaD, psaJ and psaF genes have been mutated. However, the radiolabeled PsaE associated with these membranes was removed both by the proteolytic as well as by the chaotropic agents. Characterization of PsaE present in vivo revealed similar results. These observations suggest that PsaD and PsaF/J may interact with PsaE and stabilize it in the photosystem I complex.
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  • 18
    ISSN: 1573-5028
    Keywords: gene expression ; photosynthesis ; protein turnover ; psbA ; tac promoter
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The unicellular cyanobacterium Synechococcus sp. PCC 7942 has three psbA genes encoding two different forms of the photosystem II reaction centre protein D1 (D1:1 and D1:2). The level of expression of these psbA genes and the synthesis of D1:1 and D1:2 are strongly regulated under varying light conditions. In order to better understand the regulatory mechanisms underlying these processes, we have constructed a strain of Synechococcus sp. PCC 7942 capable of over-producing psbA mRNA and D1 protein. In this study, we describe the over-expression of D1:1 using a tac-hybrid promoter in front of the psbAI gene in combination with lacI Q repressor system. Over-production of D1:1 was induced by growing cells for 12 h at 50 μmol photons m-2 s-1 in the presence of 40 or 80 μg/ml IPTG. The amount of psbAI mRNA and that of D1:1 protein in cells grown with IPTG was three times and two times higher, respectively. A higher concentration of IPTG (i.e., 150 μg/ml) did not further increase the production of the psbAI message or D1:1. The over-production of D1:1 caused a decrease in the level of D1:2 synthesised, resulting in most PSII reaction centres containing D1:1. However, the over-production of D1:1 had no effect on the pigment composition (chlorophyll a or phycocyanin/number of cells) or the light-saturated rate of photosynthesis. This and the fact that the total amounts of D1 and D2 proteins were not affected by IPTG suggest that the number of PSII centres within the membranes remained unchanged. From these results, we conclude that expression of psbAI can be regulated by using the tac promoter and lacI Q system. However, the accumulation of D1:1 protein into the membrane is regulated by the number of PSII centres.
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  • 19
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    Plant molecular biology 17 (1991), S. 641-652 
    ISSN: 1573-5028
    Keywords: F-ATPase ; cyanobacteria ; operon ; evolution ; photosynthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The two operons atp1 and atp2, encoding the subunits of the FOF1 ATP-synthase, have been cloned and sequenced from the cyanobacterium Synechocystis sp. PCC 6803. The organization of the different genes in the operons have been found to resemble that of the cyanobacteria Synechococcus sp. PCC 6301 and Anabaena sp. PCC 7120. The Synechocystis FOF1 ATP-synthase has nine subunits. A tenth open reading frame with unknown function was detected at the 5′ end of atp1, coding for a putative gene product similar to uncI in Escherichia coli. A promoter structure was inferred for the Synechocystis atp operons and compared to other known promoters of cyanobacteria. Even though the operon structure of atp1 and atp2 in Synechocystis resembles the corresponding operons of Synechococcus, the amino acid sequences of individual gene products show marked differences. Genetic distances between cyanobacterial genes and genes for ATP-synthase subunits from other species have been calculated and compiled into evolutionary trees.
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  • 20
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    Plant molecular biology 17 (1991), S. 289-293 
    ISSN: 1573-5028
    Keywords: cytochrome b 6-f complex ; photosystem II (Synechocystis PCC 6803) ; photosynthesis ; Rieske Fe-S sequence ; apocytochrome f sequence
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
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  • 21
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    Plant molecular biology 19 (1992), S. 217-230 
    ISSN: 1573-5028
    Keywords: chlorophyll a/b-binding protein genes ; Glycine ; LHCP II ; photosynthesis ; soybean ; ribulose-1,5-bisphosphate carboxylase genes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The levels of chlorophyll a/b-binding protein (Cab) gene polysomal poly(A)+ mRNA were quantitated throughout the development of Glycine max L. Cab mRNAs were abundant in young expanding leaves, representing 6.1% of the leaf mRNA population. Lower Cab mRNA levels were present in embryos, stems, and cotyledons of developing seedlings; the lowest levels were found in roots where they accounted for 0.04% of the polysomal poly(A)+ mRNA of this organ. To determine the contribution of different members of the Cab gene family to the Cab mRNA populations, a quantitative S1 nuclease reconstruction assay was developed. Cab3, Cab4, and Cab5 mRNAs were detected in all stages examined during soybean development but their levels underwent differential changes. Cab3 encodes the most abundant Cab mRNA in young leaves, developing embryos, and in Stage VII cotyledons from the developing soybean seedling. The levels of Cab mRNAs were compared to the levels of ribulose-1,5-bisphosphate carboxylase small subunit gene mRNA and differences in their patterns of accumulation were noted. Collectively these data indicate that during soybean embryogenesis developmental control mechanisms supersede light-regulatory signals.
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  • 22
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    The journal of membrane biology 126 (1992), S. 265-275 
    ISSN: 1432-1424
    Keywords: photosynthesis ; thylakoids ; electrochromism ; gramicidin ; conductance ; dimerization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Summary The effect of the pore-forming antibiotic gramicidin on pure lipid membranes is well characterized. We studied its action in protein-rich thylakoid membranes that contain less than 25% (wt/wt) acyl lipids. A transmembrane voltage was induced by flashing light, and its decay was measured and interpreted to yield the distribution of gramicidin over thylakoids, its dimerization constant and its single-channel conductance in this membrane. The distribution of gramicidin over the ensemble of thylakoids was immediately homogeneous when the antibiotic was added under stirring, while it became homogeneous only after 20 min in a stirred suspension that was initially heterogeneous. The dimerization constant, 5×1014 cm2/mol, was about 10 times larger than in pure lipid membranes. This was attributed to the upconcentration of gramicidin in the small fractional area of protein free lipid bilayer and further by a preference of gramicidin for stacked portions of the membrane. The latter bears important consequences with regard to bioenergetic studies with this ionophore. As gramicidin was largely dimerized from a concentration of 1 nm (in the suspension) on, the membrane's conductance then increased linearly as a function of added gramicidin. When the negative surface potential at the thylakoid membrane was screened, the conductance of a single gramicidin dimer agreed well with figures reported for bilayers from neutral lipid (about 0.5 pS at 10 mm NaCl). The modulation of the conductance by the surface potential in spinach versus pea thylakoids and between different preparations is discussed in detail.
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  • 23
    ISSN: 1871-4528
    Keywords: water-stress ; photosynthesis ; yield
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary Relations between measurements of the slow kinetics of chlorophyll fluorescence and growth and yield were examined in seven potato genotypes grown either fully irrigated or droughted from the time of plant emergence. Drought reduced total dry matter production and yields and increased tuber dry matter concentration. Drought increased harvest index in cv. Spunta, but decreased it in cv. Pentland Crown. Total dry matter production was correlated with each of constant fluorescence, variable fluorescence and the half life of the decay in variable fluorescence. These correlations were determined largely by the effect of treatment, and did not discriminate effectively between genotypes within a treatment.
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  • 24
    ISSN: 1871-4528
    Keywords: water-stress ; photosynthesis ; leaf water potential
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary The slow kinetics of chlorophyll fluorescence were examined in seven potato genotypes grown either fully irrigated or droughted from the time of plant emergence. Constant and variable fluorescence (F o andF v respectively) declined with time in plants from both irrigated and droughted treatments, but the decline was greater in droughted than irrigated plants. However, the yield of variable fluorescence (F v/(F o+F v)) was unaffected by the drought treatment. The main effect of drought was upon the quenching of variable fluorescence. Both the half life of the decay of variable fluorescence (q1/2) and the secondary maximum (M) were significantly greater in the droughted plants than in those from the irrigated treatment. Significant differences between genotypes were found forF v/(F o+F v),M andq 1/2. Genotype-by-treatment interactions were non-significant for all the variables examined. Changes in chlorophyll fluorescence transients were not closely related to changes in leaf water potential.
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  • 25
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    Russian journal of marine biology 26 (2000), S. 389-398 
    ISSN: 1608-3377
    Keywords: hermatypic coral ; zooxanthella ; photosynthesis ; respiration ; energy budget
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract We analyzed the recent data on the distribution of the photosynthetic energy of zooxanthellae in corals and the models of interactions between the plant and animal cells in the course of matter and energy exchange developed based on this information. The models of energy exchange of animals symbiotic with zooxanthellae are characterized by the following features: (1) A flow chart of carbon or energy fluxes is the main form of representation of the energetics in native symbiotic organisms. (2) The relations between the symbionts are relatively adequately revealed and correspond to the modern notions; however, the intensities of the energy fluxes ascribed to these relations are dependent on the experimental and design methods used by the authors. (3) The inputs into the energy budget consist of the autotrophic production of zooxanthellae and the heterotrophy of the polyp. The energy expenditures comprise excretion, respiration, development, and growth of the animal and algae. (4) The differences between the species, genera, and phyla of animals that develop symbiotic relations with zooxanthellae are confined to the absolute values of energy fluxes in the organism.
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  • 26
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Bovine milk ; Multivariate optimization ; Glycerophospholipids ; Molecular species separation ; Chemometrics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The molecular species profile, representing the fatty acid combinations on the glycerol backbone, is the most fundamental description of an intact glycerophospholipid class and provides a key to understanding its functional characteristics. We have developed a powerful RP-HPLC method for the separation of molecular species, including so-called “critical pairs”, of natural mixtures of 1,2-diacyl-sn-glycero-3-phosphocholine 1,2-diacyl-sn-glycero-3-phosphoethanolamine from bovine milk and other natural sources. We have used a novel multivariate development and optimization strategy to locate the region of optimum separation conditions within a prechosen domain of the chromatographic parameter space.
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  • 27
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Open tubular columns ; Cross-linked polyacrylate stationary phase ; Photopolymerization ; Antracene derivatives
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Polyacrylate films containing a lauryl moiety were fabricated on about 12 μm I.D. fused silica capillaries by in-situ photopolymerization of acrylates. Relatively thick films up to 1 μm were obtained by the technique. The films were tested as retentive layers for reversed phase open tubular liquid chromatography (OTLC). Due to the presence of the incorporated lauryl moiety in the layer considerable retention could be achieved for polar compounds with aqueous mobile phases. The efficiency of the prepared columns approximates to the theoretical value. The polyacrylate films appear to be extremely stable even under strong basic conditions. The films swell considerably in the presence of nonpolar solvents resulting in more favourable retention and a significant improvement of the chromatographic performance.
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  • 28
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    Chromatographia 35 (1993), S. 627-630 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fatty acid analysis ; Fish oils
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A chromatographic method has been developed for the determination of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) in fish oil dietary supplements containing triglycerides rich in (n−3) polyunsaturated fatty acids (PUFAs). Following the ester saponification, free fatty acids were resolved by TLC into two fractions: i) a more mobile group of saturated and monounsaturated fatty acids and ii) a less mobile group containing PUFAs. The PUFA fraction was further analyzed by HPLC to determine the levels of EPA and DHA in the fish oil sample.
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  • 29
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carbidopa and levodopa in plasma ; Electrochemical detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A validated reversed-phase high-performance liquid chromatographic procedure employing electrochemical detection (LCEC) for the analysis of carbidopa and levodopa in human plasma is reported. The method is sensitive and specific with amperometric detection at a glassy carbon working electrode with Eapp=0.75 V vs. Ag/AgCl. The retention times of levodopa, internal standard, and carbidopa are 3.3, 4.5, and 9.7 minutes, respectively, with an overall chromatographic run time of 12.0 minutes. The peak height ratio versus plasma concentration is linear over the range of 5.0 to 500 ng/mL for each analyte and exhibits correlation coefficients of 0.9957 or better (n=9). The mean absolute recovery of carbidopa and levodopa using the described assay is 36.6 and 66.0%, respectively. The inter- and intra-day accuracy and precision are within 11.8% of the actual values for all concentrations. Also, due to the demonstrated instability of carbidopa and levodopa in plasma a procedure is provided to circumvent this. Blood collected in pre-treated Vacutainer tubes can be stored in an ice bath for up to 4 hours without any significant degradation, thereby providing a practical means for processing several clinical samples simultaneously.
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  • 30
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fullerenes ; FullereneSep® ; Separation factor ; HPLC-particle beam mass spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary High-performance liquid chromatographic separation of fullerene mixtures in the range C60 to C100 can be achieved using a novel stationary phase which rivals the performance of the more expensive ‘Pirkle-type’ columns currently employed.
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  • 31
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    Chromatographia 35 (1993), S. 675-678 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion chromatography ; Trace metal determination ; Sample contamination ; Human hair
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The dynamic ion-exchange chromatographic analysis of bivalent ions, such as Cu, Pb, Zn, Ni, Co and Mn in resistant organic matrices needs preliminary wet ashing with oxidizing acids (HNO3 and HClO4). Such treatment may lead to an increase in the amounts of metals present in the sample due to their release from containers or equipment used in an acidic environment and to metal impurities contained in the acids. The effect of these interferences in the determination of trace metals in human hair was studied.
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  • 32
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Normal phase separations ; Cyanopropyldimethyl silica ; Chloro-added polycyclic aromatic hydrocarbons ; Environmental samples
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    Topics: Chemistry and Pharmacology
    Notes: Summary Retention characteristics in normal phase HPLC of highly biologically active chloro-added polycyclic aromatic hydrocarbons (PAHs) were studied. Silica, cyanopropyldimethylsilyl- and aminopropylsilyl- modified stationary phases were investigated. Retention properties of chloroadded PAHs on these phases were shown to be strongly influenced by the number of chloro-additions. This is due to the strong polarity of the methylene carbon at the chloro-addition site. Active silica had a strongly degrading effect on the unstable chloro-added PAHs during separation. Aminopropylsilica did not exhibit sufficient selectivity towards chloro-added PAHs when compared to chlorosubstituted PAHs. Cyanopropyldimethylsilica was shown to be applicable to a group separation of chloro-added and chloro-substituted PAHs. A fast clean-up procedure for chloro-added PAHs in complex samplesis outlined. It involves an initial elimination of more polar substances on a short open column with strongly deactivated silica and a subsequent separation on a cyanopropyldimethylsilyl HPLC column in normal phase mode.
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  • 33
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    Chromatographia 32 (1991), S. 345-349 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column packings ; Pore size distribution ; Diffusion and adsorption ; Band broadening
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    Topics: Chemistry and Pharmacology
    Notes: Summary The complex intraparticle structure typical of chromatographic column packings has been analyzed by use of an equivalent network model which emphasizes pore size distribution and connectivity. Special attention is given as to the way in which diffusion and adsorption interact and display modified peak spreading characteristics according to the morphology of the pore space. This study reveals a very significant increase in the column band broadening over that expected from physical adsorption which can arise from particular distributions of pore sizes. This has implications for designing packings which take advantage of the separating power due to adsorption but do not compromise the resolution of the chromatographic system.
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  • 34
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; GC/ECD detection ; PCBs, ortho and non-ortho ; Chromatographic separation ; Congener determination ; FTIR identification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An analytical procedure for the individual determination of ortho and non-ortho PCB congeners in sediments, using high performance liquid chromatography (HPLC) preseparation and gas chromatography/ECD detection, is described. Gas chromatography/FTIR spectrometry (GC/FTIR) and gas chromatography/mass spectrometry (GC/MS) were employed for individual congener identification and determination. Sample extraction, clean-up of extract and selective elution procedures were optimized by using reference certified marine sediment samples. Recovery and precision were typically 83% and 16% respectively at 2 ng/g of total PCB content. The proposed procedure, tested by analyzing real sediment samples, showed a reproducibility better than 20% at 13 ng/g PCB level.
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  • 35
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Glutamine ; Pyroglutamic acid ; Amino acids formulations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The aminoacid glutamine in aqueous solution and in conditions of high temperature and long term storage is partly transformed into pyroglutamic acid which exhibits potential neurotoxic effects. Commercially available aminoacid mixtures supplemented with glutamine are heat-sterilized and some losses of glutamine and formation of pyroglutamic acid may occur. The aim of the work was to set up an easy and reliable HPLC method which allows the determination of pyroglutamic acid as a degradation product of glutamine. The column was a 5 μm Hypersil ODS (100×4.6 mm) and the mobile phase 100% 0.007 M phosphate buffer pH 3.5. Stability studies in different conditions of temperature and time of storage were performed on aminoacid mixture available in the commerce.
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  • 36
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carbonyl compounds ; Luminarin hydrazides ; Fluorescence detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Fluorogenic reagents (luminarin 3, luminarin 11 and luminarin 12), having a quinolizinocoumarin moiety as fluorophore and a carboxylic acid hydrazide function as reacting group, have been developed. These reagents were found to be highly sensitive fluorescence derivatization reagents for aldehydes and ketones in high-performance liquid chromatography. The reagents readily react with carbonyl compounds in aqueous sulphuric acid solution (0.1 M) at room temperature to produce the corresponding hydrazone derivatives, which can be separated on both reversed or normal-phase column. The structures of the derivatives were studied, together with their properties in reversed and normalphase chromatographic systems. UV absorbance, corrected fluorescence spectral data and quantum yields of luminarin 3, luminarin 11 and luminarin 12 are presented. The detection limits (signal to noise ratio=3) for aldehydes and ketones were in the sub-pmol range. Luminarin 3 was also applied to the determination of hydroxymethylfurfural (HMF) in orange juices and concentrates. The method for HMF involves the solid-liquid extraction of the juice by using a C-18 cartridge prior to derivatization and normal-phase separation of the derivative with fluorimetric detection at 387 nmex., 444 nm em. The calibration curve was linear for amounts of HMF ranging from 0.1 to 10 nmol. Intrarun relative standard deviation was 12.8% for 0.1 nmol and 2.6% for 1 nmol. Recovery studies indicated an average of 98.7±1.9% for juice concentrate and 99.8±3.2% for pasteurized juice.
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  • 37
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Method development ; Chemometrics ; Response criteria ; Analysis of drug purity
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    Topics: Chemistry and Pharmacology
    Notes: Summary Optimization procedures require adequate response criteria to assess the quality of each chromatogram obtained during the process. The objective of this paper is to evaluate the possibility of using different resolution functions, in the chromatographic separation of a drug and its impurities (particularly the impurity just eluted after the drug). This study shows the limits of some resolution expressions. The interest of the simple Δt criterion, the difference between retention times, is presented in this paper.
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  • 38
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    Chromatographia 36 (1993), S. 147-151 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polarity ; Retinoids
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    Topics: Chemistry and Pharmacology
    Notes: Summary The retention of retinoids in reversed-phase liquid chromatography was studied using aqueous mobile phases of different composition (methanol 94–86% and acetonityrile 92–82%) at five temperatures (40–60 °C). With both organic modifiers the effect of the molecular structure increased as the water content and the polarity of the mobile phase increased. The temperature-dependence increased in the same manner with aqueous acetonitrile mobile phases. The π-π interactions between the retinoids and acetonitrile diminish when the water content of the mobile phase is increased, as happens also to the hydrophobic interactions with both organic modifiers. The net effect of these changes depends on the composition of the mobile phase. There was excellent correlation of retention with all polarity parameters studied(ϕ, P′, xe, xd, xn, E T N , δT, δ, δo and δd), when the calculations were made separately with methanol and acetonitrile. The volume fraction of the organic modifier, ϕ, was the only parameter describing the retention well in both organic modifiers simultaneously.
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  • 39
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Aromatic amines ; Arylbenzylamide methylthioether derivative ; SL 85.1016 ; Pharmacokinetics
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    Topics: Chemistry and Pharmacology
    Notes: Summary An HPLC method has been developed for the determination of SL 85.1016, a new calcium antagonist arylbenzylamide methylthioether derivative. SL 85.1016 and the internal standard, SL 87.0210, are extracted from alkaline human plasma withn-hexane and back extracted into 0.05 M phosphate buffer (pH 2.5; 0.2 ml). Acetonitrile (50 μl) is added to the final aqueous extract in order to prevent absorption of the compounds of interest onto the walls of the glass tube; this solution then is partially processed by HPLC on a C18 column with UV detection (254 nm). The determination limit of the method is 2 ng.ml−1 of SL 85.1016 in human plasma; the response to the drug is linear in the range 2–200 ng.mg−1.
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  • 40
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    Chromatographia 36 (1993), S. 347-350 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Allium ; Derivatization ; S-alk(en)yl-L-cysteine sulfoxides ; Sulfur amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two pre-column derivatization procedures coupled with reversed phase HPLC have been compared for the analysis ofS-Alk(en)yl0L-cysteine sulfoxides in variousAllium species. In order to establish external standards some (+/-) sulfoxides were synthesized, using a new method to enhance asymmetric synthesis of the diastereoisomers. The first derivatization method is the formation ofo-phthaldialdehyde/tert.-butylthiol derivatives which can be analyzed using UV detection. The second, presently used for amino acid analysis, is the Waters Pico-Tag method, which employs phenylisothiocyanate as derivatization reagent. As the Pico-Tag method was found to be the most efficient for determination ofS-alk(en)yl-L-cysteine sulfoxides it was used to determine the alliin content of various samples of garlic.
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  • 41
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fatty acids and bile acids ; Fluorogenic precolumn derivatization ; 2-Bromoacetyl-6-methoxynaphthalene
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    Topics: Chemistry and Pharmacology
    Notes: Summary The use of 2-bromoacetyl-6-methoxynaphthalene as a fluorogenic labelling reagent in pre-column derivatization for the HPLC separation of biologically active carboxylic acids (fatty acids and bile acids) has been investigated. The compound reacts (30 min. at 70°C) with carboxylic acids to give fluorescent esters that can be separated by reversedphase HPLC and detected at λ ex. 300 nm, λ em. 460 nm. The experimental conditions for the derivatization and chromatographic separation are discussed. Applications to the determination of valproic acid and chenodeoxycholic acid in pharmaceutical formulations are described.
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  • 42
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Valproic acid ; Simultaneous determination of anticonvulsants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The derivatizing procedure of Moody et al. [20] for valproic acid has been simplified and applied to the simultaneous HPLC determination of valproic acid (VPA), barbital (B), primidone (PRM), phenobarbital (PB) and carbamazepine (CBZ) in serum or plasma of epileptic patients. The sample is deproteinized with acetonitrile containing esterification agents and an aliquot of the supernatant is heated to 70°C for 15 min with 4-bromophenacyl bromide. The reaction mixture is analysed on a C18 column at ambient temperature, with gradient elution and with detection at 205 nm. The time required for the chromatographic analysis is 13 min; identification is based on retention time and quantification is by peak area determination with an internal standard. The calibration curves show good linearity in the range 6.25 to 100 mg/L. The detection limits at a signal: noise ratio ≥3, ranged from 1 mg/L for B and CBZ to 2–3 mg/L for PRM, PB and VPA. The method described for the simultaneous determination of the five drugs in the same plasma pool, correlated well with isocratic HPLC methods specific for each drug. The simultaneous procedure described allows a reproducible (CVs≤6.5% within run) and rapid (25 min for sample preparation: 13 min for chromatographic run) therapeutic monitoring of patients treated with VPA and two or more antiepileptic drugs.
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  • 43
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous polymer spherical packings ; Vinyl ether ; Alkali resistance ; No abnormal adsorption
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    Topics: Chemistry and Pharmacology
    Notes: Summary Spherical, porous-polymer particles for column packing in high-performance liquid chromatography were prepared by suspension copolymerization of alkylvinyl ether with triethyleneglycol divinyl ether. The hydrophobicity of the packings was easily adjusted by changing the monomer ratio. The packings showed the usual reversed-phase liquid chromatographic properties, but did not sho abnormal retention, tailing and broadening of peaks and irreversible adsorption of ionic and aromatic substances, owing to the lack of ionic or aromatic groups. In addition, the packings were stable in alkaline solutions because of the relative alkali stability of C−O−C bonds as compared with CO−O and Si−O−C bonds in conventional packings.
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  • 44
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion exchange ; Indirect photometric and direct conductivity detection ; Naphthalenesulfonate ; Inorganic anions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Indirect photometric and unsuppressed direct conductivity detection modes are examined using naphthalene mono-, di-, and tri-sulfonate as mobile phases for the separation of several anions such as F−, Cl−, NO2 −, Br−, NO3 −, SO4=,I−, and SCN− using a commercial anion exchange column. With all three mobile phases, conductivity detection shows better sensitivities and detection limits than indirect photometry. Conductivity detection is 5 to 16 times more sensitive than indirect photometry for all analytes. Detection limits achieved using these mobile phases are, for example, 0.04 ng and 0.1 ng for chloride ion with conductivity and indirect photometry, respectively. Both detection modes give wide linear ranges extending from at least 100 ppm to the detection limit of each anion which is generally about 0.02 ppm. Sulfur oxide anions such as dithionate and tetrathionate are separated using flow programming with naphthalenetrisulfonate as the mobile phase in less than 20 minutes. With both detection modes, desired chromatographic performance of these three eluents is achieved without pH adjustment of the mobile phase.
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  • 45
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Heat-treated milk ; Milk quality indicators ; 5-Hydroxymethyl-2-furfuraldehyde
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An enhanced method of HPLC for the determination of 5-Hydroxymethyl-2-furfuraldehyde (HMF) in fluid milk was perfected. Its resolving capacity permitted the specific separation of this compound. The real concentration (μmol/l) of HMF was determined and not the HMF value, as in the colorimetric analysis, where an intermediary coloured compound (HMF-TBA) is utilised. The optimum pH condition (pH=4.0–4.2) for the mobile phase to prevent overlapping between the HMF peak and the peaks of the other compound (α and β) that coeluted with the HMF and also the optimum organic solvent content (3% or 7%) were established. This is a sensitive, quick and safe method for the determination of HMF in fluid milk.
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  • 46
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chlortetracycline ; Reversed-phase silical gel ; C8 bonded phase ; Collaborative study
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An established method for the analysis of chlortetracycline by liquid chromatography using octylsilylated silica gel as the stationary phase was examined in a multicentre study involving five laboratories and a total of six columns. Three chlortetracycline hydrochloride samples were analysed. The main component and the impurities were determined. An analysis of variance, treating each column as a different laboratory, showed an absence of consistent between-laboratory bias and the presence of a significant laboratory-sample interaction. The repeatability and the reproducibility of the method, expressed as relative standard deviations of the result of the determination of chlortetracycline hydrochloride, were calculated to be 0.9% and 1.1% respectively.
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  • 47
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    Chromatographia 37 (1993), S. 627-634 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; ODS phases ; NMR and FTIR characterization ; Stationary phase functionality
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two spectroscopic methods, solid state NMR and diffuse reflectance FTIR, have been used in conjunction with liquid chromatographicretention data to identify and distinguish the functionality of octadecylsilica (ODS) stationary phases. NMR and FTIR spectra are indicative of various features of the different functionalities of the phases and this information can be used to elucidate the configuration of the organosilyl moiety in the ODS on the silica surface and explain why DSS phases have different molecular shape (mainly planarity) recognition capability.
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  • 48
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    Chromatographia 37 (1993), S. 423-428 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polymer-modified silica ; Polypyrrole cloride ; Polypyrrole dodecylsulfate ; Small molecules ; Polyaromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Polypyrrole chloride and polypyrrole dodecylsulfate coated-silica packing materials have been synthesized. Reverse-phase chromtographuy was employed to characterise both packings. A series of test compounds with known properties was used as molecular probes. They included benzene and derivatives, basic drugs, and polyaromatic hydrocarbons. A commericial C18 column was also used for the purpose of comparison in some cases.
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  • 49
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Arsenic compounds ; Polymeric styrene divinylbenzene phase ; Ion-pairing
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The resolving power of an ion-pair reversed-phase liquid chromatography method, on a polymeric stationary phase (PRP-1) with an alkaline aqueous mobile phase (pH=9) containing tetrabutylammonium cation as ion-pairing agent, is compared with a traditional ion-pairing system using an octadecyl-modified silica column and a neutral aqueous mobile phase (pH=7.3). This chromatographic system (PRP-1 column) provides a rapid means for the determination of two of the most important arsenic species, arsenobetaine and arsenite. Addition of methanol (5%) to the aqueous mobile phase allows the differentation of arsenobetaine from the system peak when using UV detection.
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  • 50
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gravity-flow column chromatography ; Provitamin A determination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The provitamin A content of some food samples was determined by methods involving MgO: Hyflosupercel gravityflow column chromatography (GFCC) and reversed phase high performance liquid chromatography (HPLC), the quantitation being done by external standardization (HPLC-ES) or internal standardization (HPLC-IS) with Sudan. The results obtained with α- and β-carotene in carrots, β-carotene and β-cryptoxanthin in papaya and β-carotene in tomato and kale agreed well, showing that any of the these techniques can be used, provided the analysis is done under optimum conditions. Good separation of the different provitamins using GFCC depends on the analyst's skill and visual acuity. HPLC-ES required a constant supply of provitamin standards, thus the varying purity of commercially available standards and the high instability of these compounds could pose grave problems. Due to the stability of Sudan, HPLC-IS appeared to be the method of choice although passage of the extract through a MgO: Hyflosupercel minicolumn was required prior to injection to separate chlorophylls, dihydroxy- and polyoxycarotenoids which would otherwise elute with Sudan. Nonconformity of the Sudan structure to those of the provitamins did not effect the quantitative results. The chromatographic separation, identity and quantification of the provitamins could be more easily established by using HPLC-IS, complemented with GFCC.
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  • 51
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    Chromatographia 33 (1992), S. 103-112 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Chiral separations ; Allethrin ; Cypermethrin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Liquid and gas chromatographic separations of the pyrethroid insecticides allethrin and cypermethrin have been investigated with various achiral and chiral stationary phases. Diastercomeric and enantiomeric selectivity was observed for cypermethrin on a Pirkle-type chiral LC stationary phase, but very strong interactions and therefore long retention times prevented the separation of allethrin on this phase. Trans-allethrin isomers were separated on a chiral β-cyclodextrin RP-HPLC column while cypermethrin showed some difficulties on this phase due to isomerization. Diastereomeric but no enantiomeric selectivity by GC was achieved for cypermethrin with an apolar DB 5 capillary. GC separation of the diastereomers was used to study the selective photodegradation of cypermethrin isomers after forestry applications. Chiral β-cyclodextrin-based GC phases showed some enantioselectivity for cis- and trans-allethrin isomers. A separation of the eight isomers into six partially resolved peaks was achieved by GC with a coupled column consisting of chiral permethylated β-cyclodextrin and DB 1701 as stationary phases. This combination was used to characterize allethrin formulations intended for indoor use and to investigate allethrin products formed by ozonolysis of thin films of the insecticide.
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  • 52
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiralcel OD ; N-Alkyl-N-methylanilineN-oxide enantiomers ; Chiral nitrogen centre ; Flavin-containing monooxygenase
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A high-performance liquid chromatographic method for the resolution of the enantiomers of a series ofN-alkyl-N-methylanilineN-oxides is reported. The resolutions were achieved using a Chiralcel, OD chiral stationary-phase with a mobile-phase of hexane and ethanol in varying proportions. The chromatographic order of elution of the enantiomers ofN-ethyl-N-methylanilineN-oxide was determined to be (+)-(R) before (−)-(S).
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  • 53
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    Chromatographia 37 (1993), S. 539-542 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Sotolon ; Vin jaune ; Flor-sherry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Sotolon (4,5-dimethyl-3-hydroxy-2(5H)-furanone) is a key flavour compound in the french flor-sherry “Vin jaune”. This compound was determined quantitatively by extraction of 25 ml of wine on a XAD-4 resin, elution with diethyl ether, separation by HPLC on a Lichrospher 100 Diol column, elution with dichloromethane/hexane (60/40) and UV detection at 232 nm. The amount of sotolon in “Vin jaune” (120 to 268 μg/l) was related to the development of the yeast film over a period of 6 years. Only 6 to 51 μg/l were found in the “Vin de paille” which is made with overmaturated grapes of the same Savagnin vine-plant but without development of yeasts, and 80 to 140 μg/l in “Tokai” which are partly grown under a yeast film.
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  • 54
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column-switching ; Determination of triamterene ; Fluorescence detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A liquid chromatographic method incorporating column-switching and fluorimetric detection for the determination of triamterene in untreated urine, is described. The urine samples (5 μL) were directly introduced onto an Hypersil ODS-C18, 30 μm (20 mm×2.1 mm I.D.) pre-column. Polar urinary compounds were removed by flushing the pre-column with water for 1 min, and the analyte was then switched onto an HP-LiChrospher RP C18,5 μm (125 mm×4mm ID) analytical column using an acetonitrile/phosphate buffer gradient elution. Fluorescence detection was performed at 230 nm excitation and 430 nm emission wavelengths. The recovery of drug was 102±2% in the 0.10–20.0 μg/mL concentration range, the limit of detection being 5 ng/mL. A validation of the usefulness of this procedure was accomplished by analysing urine extracts obtained from real samples.
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  • 55
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Characterization of reversed phases ; Column hydrophobicity ; Column hydrophylicity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The validity of a method for characterizing stationary phases for reversed-phase, liquid chromatography, based on the use of homologous series, has been evaluated. The method is based on a retention model which describes the dependence of the logarithm of the capacity factor on mobile phase composition and the carbon number of specific homologous series. A first-order as well as a second-order version of this model was investigated. The second-order model proved to be a significant improvement on the first-order model, even for smaller mobile-phase ranges. Nevertheless both models showed a significant lack of fit, reflecting the incompleteness of these models. Therefore, it is very questionable whether this method is suitable to describe HPLC-column characteristics like hydrophobicity and hydrophylicity.
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  • 56
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Copoly(styrene/acrylonitrile) ; Gradient elution ; Precipitation chromatography of polymers ; Solubility of polymers
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    Topics: Chemistry and Pharmacology
    Notes: Summary Copolymers from styrene and acrylonitrile could be separated according to composition by gradient elution through methanol after injection inton-heptane and sudden addition of 50, 60, or 70 vol% tetrahydrofuran. The peak sequence was the same as with a common binary gradientn-heptane/tetrahydrofuran, i.e., retention increased with acrylonitrile content of the samples. With copolymers containing 37, 31, or 26% acrylonitrile, the elution characteristics in the ternary systems could be logically extrapolated towards the points measured in the corresponding binary gradient system.
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  • 57
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral recognition ; Aminoalkylphosphonic acid derivatives ; β-cyclodextrin bonded phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An acetylated β-cyclodextrin column was used to analyse the enantiomeric resolution of a number of aminophosphonic acids. Effects of the structure of these compounds on the extent of separation was examined. Molecular modelling studies were also carried out in an attempt to relate any interaction between the amino and phosphonic acid groups to chiral recognition by the stationary phase.
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  • 58
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    Chromatographia 33 (1992), S. 177-185 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Diuretics ; Screening and determination of diuretics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This critical review of different methods proposed for the determination and screening of diuretics is directed mainly, because of its potential application, towards highperformance liquid chromatography.
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  • 59
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    Chromatographia 33 (1992), S. 218-224 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Peak ; Pattern recognition ; Prediction interval
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary It is still difficult to determine peaks and peak boundaries properly, though peak recognition is very important for the precision of quantitative data. A new computer program overcomes these problems using a method which is adapted from human judgements. The algorithm was developed for HPLC but can also be used in other fields of analytical chemistry.
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  • 60
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral separation ; Association constants ; Frontal analysis ; Cyclodextrin bonded-phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The interaction between cyclodextrin and the drug (1R,2S,3S,4S)-(5Z)-7-(3-((phenylsulfonyl)amino)bicyclo[2.2.1]hept-2-yl)hept-5-enoic acid ((+)-S-145), was studied using α-, β-, and γ-cyclodextrin bonded-phase columns. Retention behavior of (+)-S-145 on these columns revealed that the strength of inclusion was β→γ→α-cyclodextrin. Interaction between β-cyclodextrin and (+)-S-145 was found to increase as the proportion of carboxylic ion in the (+)-S-145 molecule increased. Comparison of binding capacities of these bondedsilica gels obtained by frontal analysis and surface coverage indicated that availability of the immobilized β- and γ-cyclodextrin was 20–25%. The synthesized β-cyclodextrin bonded-phase column was superior to that of commercial columns in terms of chiral separation of (±)-S-145. A typical usage of the β-cyclodextrin column is discussed for separation of (±)-S-145 in plasma samples.
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  • 61
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Primary and secondary aliphatic alcohols ; Aqueous derivatization ; Phthalic acid monoesters
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    Topics: Chemistry and Pharmacology
    Notes: Summary Determination of primary and secondary aliphatic alcohols in aqueous and nonaqueous solutions by high-performance liquid chromatography (HPLC) is described. The alcohol is derivatized with phthalic anhydride to yield the corresponding monophthalate. Separation of the derivative is achieved on an ODS-10 reverse phase (RP) column by elution with an appropriate isocratic mobile phase of acetonitrile and aqueous phosphoric acid (0.1%). Detection is accomplished by UV absorption at 230 nm or 280 nm giving linear calibration plots, for alcohols in aqueous solution from 0.05% to 0.50% (w/v) and in pyridine solution from 0.0025% to 0.0250% (w/v).
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  • 62
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hybrid mobile phases containing alcohols ; Solute-micelle association constants ; Polynuclear aromatic hydrocarbons
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    Topics: Chemistry and Pharmacology
    Notes: Summary The interaction between some polynuclear aromatic hydrocarbons of environmental concern, and sodium dodecylsulphate and hexadecyltrimethylammonium bromide in the presence of methanol, 2-propanol and n-butanol has been evaluated by high-performance liquid chromatography using micellar mobile phases. Solute-micelle association constants have been determined for the compounds investigated. The results show that the addition of the alcohol to the mobile phase decreases the association constant values, methanol 〈2-propanol 〈n-butanol, relative to those in the absence of any additive.
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  • 63
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    Chromatographia 38 (1994), S. 571-578 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Wine ; Biogenic amines ; Solid-phase extraction ; Derivatization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method suitable for the determination of 19 biogenic amines in wine has been developed. The method involves derivatization of amines by treatment with dansyl chloride and solid-phase extraction of the derivatives. Prior to the derivatization procedure, clean-up of the wine sample with polyvinylpyrrolidone is carried out. Reversed-phase gradient elution HPLC with UV detection at 250 nm was used to determine these compounds. Some consideration was given to the effect of temperature on the separation process. Linearity of derivatization was obtained for amounts of all the biogenic amines ranging from 500 μg·L−1 to 20 mg·L−1. Limits of detection (signal-to-noise ratio=3) of the amines were similar for all the dansylderivatives (between 50 and 150 μg·L−1). Addition of standard amines was used for the determination of amine recoveries. These were better than 85% for ethanolamine, tryptamine, phenetylamine, putrescine, cadaverine and histamine. The overall process was succesfully applied to identify and quantify biogenic amines in white and red wines.
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  • 64
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral/enantiomeric iseparation ; Cellulose-based chiral phases ; Tifluadom analogues ; 2-acylaminomethyl-1,4-benzodiazepines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The resolution of nine recamic mixtures of tifluadom analogues has been evaluated using the chiral stationary phases Chiralcel OD and Chiralcel OJ. The separation was performed on an analytical scale to optimize the conditions for chiral resolution, approaching baseline separation, of the two enantiomers. Eight racemates were baseline separated on Chiralcel OJ using a mobile phase of hexane/2-propanol.
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  • 65
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Diol silica gels ; Carbohydrates ; Evaporative light scattering detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Bonded silica columns have been evaluated for their ability to separate carbohydrates and polyols. Mobile phases consisting of dichloromethane/methanol produced the best separations in comparison with the acetonitrile/water mixtures commonly used with amino columns. Of all the bonded phases tested, LiChrospher Diol silica provided the best separations, and selectivities were not very different from those obtained on the most popular system using an amino bonded phase and acetonitrile/water as eluent. In addition, diol columns with a dichloromethane/methanol eluent offer excellent stability with no Schiff’s base formation of reducing sugars. Using an evaporative light scattering detector, low limit detection is obtainable (20 ng of glucose from a column) and gradient elution is quite feasible.
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  • 66
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenolic compounds ; Ion-pair solid-phase extraction ; Comparison of sorbents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A comparative study of the solid phase extraction of phenolic compounds in water was carried out. Three different sorbents, C18, CH and PLRP-S, were tested for the preconcentration process in order to determine phenolic compounds in water at μg l−1 levels by reversed-phase LC separation and diode-array detection. The addition of an ion-pair reagent in the extraction process was also studied in order to increase the breakthrough volume of some compounds. Using the optimized conditions the limit of detection was less than 0.5 μg l−1, the maximum admissible concentration (MAC) in drinking water. The method was applied to determine phenolic compounds in Ebro river water however no phenols were found within the detection limits of the method.
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  • 67
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Extraction-determination ; Basic drugs ; Blood
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method for the extraction of basic drugs from whole blood based on the use of a buffered protein precipitating reagent at pH9, to form NiWO4 in biological fluids and a ternary organic extracting phase of density below 1 is proposed. The extract is analysed by high performance liquid chromatography using a Hypersil C8 column and detection at 230 nm; the mobile phases used consist of binary mixtures of acetonitrile and aqueous solutions containing 20 mmol/l ofn-propylamine at pH 5 andn-hexylamine at pH 4, as blockers of the free silanol groups. The proposed method was applied to the determination of 16 basic drugs including narcotics, analgesics, cocaine-related compounds and adulterants, as well as 8 benzodiazepines, in whole blood.
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  • 68
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    Chromatographia 39 (1994), S. 62-66 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column switching ; Imidazolinone herbicides in soil ; Imazethapyr ; Imazapyr
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A column-switching method using two separation columns combined with UV detection at 260 or 236 nm has been used to determine the imidazolinone herbicides imazethapyr and imazapyr in soils. The residues were extracted from the soil with 0.1 M aqueous sodium carbonate solution and, after adjusting the pH to 2.0, the solution was partitioned with dichloromethane. Limits of determination for imazethapyr and imazapyr were 3 μg/kg. Recoveries were from 55 to 75% for both imidazolinone herbicides in the range 3–100 μg/kg in soil.
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  • 69
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous graphitized carbon ; Ring-substituted aniline derivatives ; Electronic interactions ; Principal component analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention characteristics of 22 aniline derivatives were determined on a porous, graphitized-carbon column in unbuffered acetonitrile-water and methanol-water mixtures. Each aniline derivative gave symmetrical peaks in each eluent without buffers. Good linear correlations were found between the log k′ and the concentration of the organic component in the eluent. The slope and intercept values differed according to the type of organic modifier and the charcter, number and position of substituents, indicating the different selectivities of methanol and acetonitrile and the good separating power of the column. Multivariate mathematical-statistical calculations proved that the retention of ring-substituted aniline derivatives is mainly governed by electronic parameters and the hydrogen acceptor capacity of substituents.
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  • 70
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-pairing ; Furosine ; Pyridosine ; Milk
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An ion-pair, reversed-phase, liquid chromatographic procedure using UV detection for quantitation of furosine is described. The standard plot was linear (r〉0.999) over a 5 ng range. An authentic synthesised sample of furosine was used for calibration. Commerical milk samples were analyzed by the described procedure.
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  • 71
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Automated peak detection ; Discrete Fourier transform ; Frequency acquisition and filtering ; Peak detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The principle of automated chromatographic peak detection and analysis software is summarized, and critical steps are systematically studied. As the only parameter to be entered is the acquisition frequency, evaluation of its effect on software performance is discussed. In the case of relatively noisy chromatograms, it is shown experimentally that numerous points per peak have to be taken, leading to quite fast computer acquisition procedures. The use of discrete Fourier transform filtration techniques can modify peak shapes and a comparative study evaluates the relative errors induced in the shapes and characteristics of the chromatographic profiles. Optimisation of filtering conditions is achieved and it is shown that for a filter position only 2% of the Nyquist frequency no deformation occurs in the chromatographic profile. Detection of the start and finish of chromatographic peaks is optimized according to a simple four step iterative procedure. In the case of simulations, the difference between the values used to simulate peaks and those calculated by the software are less than 1%.
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  • 72
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    Chromatographia 39 (1994), S. 246-248 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mercury ; Diphenylethynylmercury
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new procedure for derivatisation of inorganic mercury(II) to diphenylethynylmercury with simultaneous extraction into dichloromethane is proposed. The organomercury derivative is effectively analysed by HPLC using UV detection. The calibration curve is linear over three orders of magnitude (0.02–50 mg L−1 Hg); the detection limit is 0.1 ng Hg. A preliminary study of the effect of potential interfering agents, in particular Cu(II), Zn(II), Cd(II), Pb(II), and cysteine, and applications of the present methodology to real environmental samples are presented.
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  • 73
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fluoropyrimidine drugs ; Pharmacokinetics of doxifluridine ; Chemotherapy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed phase high performance liquid chromatographic method has been developed for the simultaneous determination of the pro-drug 5′-deoxy-5-fluorouridine (5′-dFUR), its metabolite 5-fluorouracil (5-FU) and some fluorinated pyrimidines involved in the metabolic activation process of 5-FU. The method has been used to monitor the bioavailability of 5′-dFUR and 5-FU in patients undergoing anticancer chemotherapy. Serum sample treatment involves addition of internal standard (5-bromouracil), protein precipitation with saturated ammonium sulphate solution and liquid-liquid extraction with ethyl acetate-isopropanol (90 ∶ 10 v/v). Urine is simply diluted with mobile phase and injected. The average recovery from serum (at 0.5 μg/mL level) was 95.0%±1.4 for 5′-dFUR and 86.3%±3.5 for 5-FU. A linear response extending over four decades of concentration was observed. Detection limits in the low ng/ mL range were obtained using a 250 μL sample size and a 20 μL injection volume. Within-day and between-day coefficients of variation were below 4 and 10%, respectively.
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  • 74
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flow injection analysis ; Combined flow injection/HPLC ; Carbamate pesticides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An integrated flow injection (FI)/HPLC system for the total and individual determination of carbamate pesticides (propoxur, carbofuran and carbaryl) is proposed. The determination is based on the alkaline hydrolysis of the analytes and subsequent coupling with diazotized sulphanilic acid to yield the monitored dyes with or without a prior separation step by HPLC in a C18 column. The calibration curves obtained are linear in the μg/ml range and r.s.d. values are between 0.5 and 3.7% in all instances. Injection of the sample into the FI manifold allows the total pesticide content in the sample to be screened. The manifold thus acts as a post-column reactor/detector of the chromatograph for samples with high overall carbamate content, which are also injected into the HPLC instrument. The performance was checked with contaminated water samples.
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  • 75
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; α1 glycoprotein ; Enantioseparation ; β-blocking agents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The enantioselectivity of the α1 glycoprotein chiral stationary phase, Chiral AGP® has been evaluated for a number of β-blocking agents. A correlation has been found between the retention behaviour on this stationary phase and the hydrophobicity of the compounds. The separation factor α is higher for compounds that are well retained. Retention, and thus α, are also controlled by pH and the percentage of organic modifier in the mobile phase.
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  • 76
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Perfluoroalkylated polymer-gel packings ; Aromatic and fluorine-containing compounds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Porous, perfluoroalkylated polymer-gels for column packings in high-performance liquid chromatography (HPLC) were prepared by suspension polymerization of heptadecafluorodecyl arcylate and ethylene glycol dimethacrylate. The packings showed no abnormal retention for ionic or aromatic compounds, due to the lack of ionic or aromatic groups. In addition, the packings showed no excessive retention for strongly hydrophobic compounds which is often the case with long-chain, alkylated silica gels and polymer gels. This is due to the extremely low surface energy of perfluoroalkyl groups. Therefore, perfluoroalkylated polymer gels enable isocratic HPLC separation of solutes with significantly different hydrophobicity.
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  • 77
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous glass ; Surface free energy ; Film pressure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
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  • 78
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    Chromatographia 33 (1992), S. 478-484 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous glass adsorbents ; Surface free energy ; Oriented adsorption of hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The relationship between the specific capacity factor (k/S, where k is the capacity and S is the surface area of the sorbent, in m2) in the liquid chromatography of aromatic hydrocarbons and the adsorption energy (-°GA) has been investigated. The previously published results, based on the calculation of the work of adhesion (WSA) from contact angles, were re-examined and a new hypothesis on interactions at interfaces was employed. Direct proportionality has been found between k/S and-°GA, which allows prediction of the chromatographic behavior of adsorbates on sorbents. The surface free energy components were calculated in order to determine-°GA in terms of the work of adhesion. The dispersion component of the surface free energy of glass was obtained from the adsorption isotherm of n-octane and it was found that the hydrocarbon molecules are adsorbed in an oriented position. The contact angles of liquids on the outer surface of porous solids do not yield reliable values of WSA and of the surface free energy components. A higher intermolecular attraction increases WSA and decreases the contact angle in pores.
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  • 79
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Adenosine and some metabolites ; Extraction from brain tissue ; Quantitative determination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An analytical procedure has been developed for the assay of adenosine and some metabolites in brain tissue extracts of rats. This paper reports the extraction method, the technique adopted to avoid enzymatic transformations and the chromatographic conditions for the identification and quantitation of these nucleosides and bases. Peaks in the chromatograms of brain tissue extracts were identified by retention times, absorbance ratios of reference compounds and by enzymatic peak-shift.
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  • 80
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    Chromatographia 34 (1992), S. 573-580 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemically bonded phases (CBP) ; Surface heterogenity ; Surface purification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The surface chemistry of eight silica-gels with different siliceous matrix structures have been described. The influence of surface impurities on the chemical modification process (coverage density) with monooctadecylsilane has been studied. The surfaces of the adsorbents, before chemical modification, were cleaned by extraction with 20% HCl. Bare and modified materials were characterized using different physico-chemical methods e.g.: SIMS, CP/MAS NMR, porosimetry, pH measurement, elemental analysis and chromatography (GC & HPLC). The presence of trace amounts of different metallic elements creating new adsorption centers on the surfaces of the packings, have been demonstrated. Moreover, it has been shown that washing of silica gel adsorbents increases the coverage density of alkylsilyl ligands and improves the chromatographic properties of prepared packings.
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  • 81
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Zone-electrophoretic sample treatment ; Basic and acidic compounds ; Biological samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A modified valve arrangement for zone-electrophoretic sample treatment (ZEST)-which is coupled on-line with column liquid chromatography — is used to pretreat biological (plasma) samples. Carry-over of plasma proteins depends on the pH of the electrophoresis buffer. The determination of propranolol, metoprolol, cromolyn and salicylic acid demonstrates that both basic and acidic analytes can be isolated from the plasma matrix with high selectivity. Analogous piperazines, with different protein binding properties, were used to study the influence of protein binding on the recovery. It is shown that high protein can cause a decreased recovery.
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  • 82
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    Chromatographia 34 (1992), S. 597-600 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Oxindole alkaloids ; Uncaria tomentosa
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The main oxindole alkaloids from the root bark ofUncaria tomentosa were separated by reversed phase HPLC with an acetonitrile/methanol/phosphate buffer solvent gradient. UV detection was carried out at 245 nm. The chromatographic parameters for the separation of the alkaloids were optimized by studying the impact of the pH value of the mobile phase and the column temperature on the separation efficiency of the analytical system. The best separation was achieved with a mobile phase pH of 6.6 and a column temperature of 15°C. The method developed is suitable for the qualitative characterisation and quantitative determination of oxindole alkaloids in crudeUncaria tomentosa extracts and phytopharmaceuticals.
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  • 83
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Enantiomers of furprofen ; Human plasma
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A sensitive and stereoselective liquid chromatographic (HPLC) assay for the S and R enantiomers of furprofen in human plasma has been developed. The assay is based on derivatization with S(−)-1-phenylethylamine with formation of two diastereoisomeric derivatives and on their separation and quantitation using HPLC with uv detection. The method is linear from 25 to 600 ng ml−1 of both enantiomers, with a variation coefficient below 10.8%, and a detection limit of 20 ng ml−1. This procedure is suitable for pharmacokinetic studies.
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  • 84
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micelle-solute association constants ; Polynuclear aromatic hydrocarbons ; Octanol/water partition coefficients
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Sodium dodecyl sulphate, hexadecyltrimethylammonium bromide and polyoxyethylene(23) lauryl ether were investigated as mobile phases in the micellar liquid chromatography of polycyclic aromatic hydrocarbons of environmental concern. A wide range of surfactant concentrations were used and the retention parameters and distribution coefficients calculated. The trends in the retention data for the PAHs are discussed and several conclusions are presented concerning the partition coefficients when these surfactants are present in the mobile phase. Comparisons are made between the structural features of the compounds and their capacity factors, and the octanol/water partition coefficients are correlated with hydrophobicity for the PAHs studied.
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  • 85
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Normal phase separations ; Chloro-substituted polycyclic aromatic hydrocarbons ; Coupled column system ; Environmental samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention behaviour of chloro-substituted PAHs on several commercial normal bonded phase HPLC columns has been investigated. Chloro-substitution was shown to generally decrease the retention on stationary phases like amino-, diol- and nitrophenylpropyl-modified silica. Dimethylaminosilica exhibited more complex retention characteristics towards chloro-substituted PAHs. On this stationary phase, the position of the chlorine substituents on the aromatic solute seemed to be of greater importance for retention than on the amino-, nitro- and diolsilica. For some chloro-PAHs, the retention was shown to increase with the number of chloro-substitutions, probably due to the large affinity of the electron-rich nitrogen in the stationary phase for the electron deficient π-system of the chloro-PAHs. Chloro-substituted PAHs were strongly retarded on the electron donating 2-(1-pyrenyl)-ethylsilica (PYE) stationary phase. However, the molecular shape of the chloro-derivatives had a large influence on retention, which was considerably decreased for some nonplanar chloro-derivatives of chrysene and benz(a)anthracene. A two-dimensional back-flush HPLC method, consisting of a combination of a nitrophenylsilica column and a PYE column of matched lengths, was shown to be useful for clean-up of chloro-substituted PAHs in environmental samples.
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  • 86
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column switching ; Lidocaine ; Horse urine analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid method is described for the determination of lidocaine and its metabolites in horse urine using a column switching technique and HPLC analysis. This procedure offers a sensitive assay without the need for time consuming extractions.
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  • 87
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    Chromatographia 34 (1992), S. 132-136 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Cysteine, cystine ; Phenylthiocarbamyl derivatives ; Protein hydrolyzates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new approach is described, and a novel explanation presented, for the high performance liquid chromatographic analysis of cystine and cysteine as their phenylthiocarbamyl derivatives. PTC cystine and cysteine have been eluted with the same retention times and molar responses, most probably due to electrophilic attack of phenylisothiocyanate on cystine resulting in the scission of the disulfide bond yielding two moles of cysteine. Further, total PTC cystine and cysteine have been measured both in model solutions and in standard protein hydrolyzates (lysozyme, bovine albumin, ribonuclease) with the same linearity as the other ineteen amino acids. The reproducibility of the measurements, at the 250–750 pmole level, proved to be 4.1% (Relative Standard Deviation %) or less.
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  • 88
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    Chromatographia 34 (1992), S. 155-158 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Retention ; Crown ethers ; Actinomycin D ; Metal cation complexation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Retention of crown ethers in reverse-phase HPLC has been determined by their bonding ability with cations present in the eluent. The dependence of retention of crown ethers on cation concentration exhibits an inflection and makes it possible to calculate stability constant for the crown ether-cation complex. It is shown that in 75% MeOH retention of antitumor antibiotic, actinomycin D, depends on [Na+] and not on [K+] at concentrations of K+ from 5×10−7 to 10−1 mol l−1. Hence, actinomycin D may be classified as an ionophore-antibiotic.
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  • 89
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenolic compounds ; Optimisation of isocratic separations ; River water samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Isocratic column liquid chromatographic systems with UV absorbance detection at 280 nm have been developed for the separation of 29 phenolics and related compounds. The selectivity was investigated on silica-, carbon- and polymer-based separation columns for the separation of phenolic type of components. The effects of various acetonitrile/buffer mixtures, and pH of the mobile phase, and their impact on the retention of the phenols was assessed. Tables of retention times on the four columns for the 29 phenols with two different acetonitrile/buffer mixtures, together with the retention times at three pHs from 6.5 to 2.3 with varying levels of organic modifier on the LiChrospher RP 18 column are presented. As an application, the analysis of real river water samples from the Ebro river is described using a solid phase extraction step prior to injection into the chromatographic system.
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  • 90
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    Chromatographia 34 (1992), S. 173-176 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carbon packing materials ; Aromatic compound separation ; Eluent effect
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention volume dependences on the molar volume were found for aromatic compounds using liquid microcolumn chromatography. The contributions of the functional groups in molecules of these compounds to the total retention value were calculated from the capacity factor values. The comparison of capacity factor values for carbon sorbents and octadecyl-silicagel has shown that for several microcolumn separations the carbon sorbent column has a better selectivity and resolution than the octadecyl-silicagel column.
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  • 91
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    Chromatographia 34 (1992), S. 177-181 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Synthesis of bonded stationary phases ; Acceptor ligands ; Normal phases ; PAHs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The synthesis of several electron-acceptor stationary phases has been reviewed the materials evaluated for their capacity to separate polyaromatic hydrocarbons (PAHs). Chemically bonded phases were obtained by the same procedure; the organosilane moiety is monofunctional and the HPLC behaviour is compared under identical conditions. Examples of PAHs separations are given.
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  • 92
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    Chromatographia 34 (1992), S. 182-184 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; C18 bonded phase ; Residual silanol groups ; Metal 5-Br-PADAP complexes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary If any residual (free) silanol groups remain at the surface of silica gel after bonding treatment, they may affect the retention of solutes since the dissociated groups (≡SiO−) will attract cations. The silanol group effect on the retention of cationic solutes will increase with increasing pH of the mobile phase but the effect will decrease with increasing hydrophobic-ion concentration at the C18 surface because such ions can mask the residual silanol groups. A method for the separation of metal complexes with 2-(5-bromo-2-pyridylazo)-diethylaminephenol (5-Br-PADAP) has been developed. The hydrophobic ion in the MeOH/H2O mobile phase was tetrabutylammonium (TBA).
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  • 93
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    Chromatographia 34 (1992), S. 342-346 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; History of chromatography ; Calcium carbonate stationary phase ; Chlorophyll
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Although Michael Tswett is the originator of chromatography, little is known about the performance of his chromatographic systems. His descriptions of the separation of plant pigments are detailed but nevertheless difficult to interprete by today's chromatographic theory. By our own experiments with the system calcium carbonate/benzene it was found that the separation factor of chlorophyll a and b is approx. 1.6 which means that less than 100 theoretical plates are necessary for separation. Tswett's columns with 50 μm particles and 2–3 cm of bed height presumably exceeded this plate number. His separations could have been impaired by mass overload and by a volume flow rate which was two orders of magnitude faster than the optimum.
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  • 94
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Isomeric substituted alkylbenzenes ; Retention and resolution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention data of isomeric xylenes, ethyltoluenes and diethylbenzenes, and of mesitylene, benzene, toluene and ethylbenzene were obtained on a reversedphase column using methanol-water and ethanol-water mobile phases at four different temperatures. This database was used to relate the dependence of solute retention and resolution on the polarity of the mobile phase, solute dipole moment, and column temperature. The additivity of the free energy of the transfer of solute molecules or solute segments from the stationary phase to the mobile phase, was examined for the isomeric compounds. For this, the logarithm of the net retention volume was substituted for the free energy. Deviations from the additivity of free energies indicate that the separation of isomeric substituted alkylbenzenes is governed by their differential interactions with both the polar mobile phase and nonpolar stationary phase. Among the disubstituted alkylbenzenes,ortho-isomers favor the mobile phase more andpara-isomers tend to prefer the stationary phase more. Themeta-isomers are found to follow the additivity rule closely. These trends are amplified as the polarity of the mobile phase is increased indicating that these isomers are resolved better in water-rich mobile phases. These findings are substantiated by analogous results from gas-liquid chromatographic retention data, estimation of dipole moment effects, and examination of the entropic and enthalpic contributions to the net retention volume.
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  • 95
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column switching ; Polycyclic aromatics ; Oil distillates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A selective and sensitive HPLC method for the determination of Benzo[a]pyrene (B[a]p) in oil fractions by means of column switching is described. The diluted oil samples were injected directly onto a silica column with isooctane as eluent. After fast elution of the main part of the sample matrix, the B[a]p containing fraction was transferred on-line to a dinitro-aryl-modified silica column for final separation with isooctane/tetrahydrofuran. A detection limit of 50 ppt B[a]p was found when using fluorescence detection.
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  • 96
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Precipitation chromatography of polymers ; Block copolymers of styrene-butyl methacrylate ; Association phenomena
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Block copolymers of styrene andt-butyl methacrylate can be analysed by methanol/tetrahydrofuran gradients on C18 or phenyl bonded phase columns. On both of these columns, retention increases with styrene content of the samples. At 50°C, the retention of PS or a block copolymer containing 45% styrene was longer on the phenyl than the C18 columns. This indicates the contribution of adsorption to retention on phenyl bonded phase columns. Lowering the temperature from 50 to 30°C caused earlier elution of part of the sample from the phenyl phase. On a C18 phase the same drop in temperature improved the shape of the peak, which also started later than at 50°C. This effect of temperature is generally observed in polymer retention due to an adsorption mechanism, whereas increasing retention with decrease in temperature is characteristic of a precipitation mechanism. The block copolymer investigated contained 15% free polystyrene precursor which could not be separated from the block copolymer under the conditions employed. The addition of 20% PS homopolymer with a molecular weight similar to that of the styrene block in the copolymer showed that the polystyrene eluted together with the block copolymer, whereas the addition of PS homopolymer with a much higher molecular weight caused an extra peak at the expected elution time.
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  • 97
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Molecular recognition ; Multidentate phenyl-bonded phases ; PAHs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary New multidentate phenyl-bonded phases (MPBPs) were synthesized and evaluated the chromatographic retention behaviour with polycyclic aromatic hydrocarbons as sample probes in high-performance liquid chromatography. The new MPBPs show different retention characteristics from the previously synthesized MPBP, designated TP. Nevertheless, the results indicate that the retention mechanism is still the same as the TP phase: the size and shape of the solute molecule can be recognized by a cavity-like space formed by the methyl groups and phenyl rings of MPBPs.
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  • 98
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    Chromatographia 34 (1992), S. 391-397 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hydrophobic interaction ; Stationary phases ; Salt effect ; Proteins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Retention and selectivity in hydrophobic interaction chromatography (HIC) depend both on the type of stationary phase and on the mobile phase. In the last few years various high performance packing materials and columns have been introduced for HIC resulting in a range of different retentions and selectivity. We have investigated the effect of the stationary phase on the retention of various proteins. The retention of some solutes of different hydrophobicities were measured on three commercial HIC columns (TSK-Phenyl, Synchropack-Propyl, CAA-HIC) under isocratic conditions using water-methanol mixtures as eluent. The log kw values determined according to the literature were devalues determined according to the literature were dependent on the type and structure of the stationary phase and indicated a much less hydrophobic character for these columns than that obtained for reversed phase columns. Gradient separations were then carried out on a standard protein mixture using ammonium sulfate and sodium citrate to change the gradient time. In order to compare the effect of the stationary phase and the two salts investigated apparent capacity factors (kg) were determined and plotted against the gradient time obtained for the three columns in the two eluent system. It was shown that the type of stationary phase had a significant effect on the retention of proteins. In addition, the effect of the mobile phase composition, i.e. salt type, was considerably different on the various stationary phases. In order to exploit the potential of HIC to modulate selectivity for the separation of proteins, the combined effect of the stationary phase and the type of salt should be taken into account.
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  • 99
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    Chromatographia 34 (1992), S. 431-432 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thin-layer chromatography ; Porphyrine ether glycerides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Efficient TLC and HPLC conditions for the separation of a newly synthesized class of compounds, porphyrine ether glycerides, have been established. Supplementary physico-chemical characteristics are given for this group of solutes.
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  • 100
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flow injection analysis ; Combined methods ; Transition metal ions ; Aqueous samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An automatic method based on the combination of a flow injection (FI) manifold with a liquid chromatograph has been developed for the enrichment and determination of transition metal ions in water samples. Alternatively, the FI configuration can be used as a screening system for the determination of the total concentration of heavy metals. Two-parameter expressions for calibration graphs involving preconcentration time and concentration of the analytes were established for both the FIA and the integrated FIA/HPLC methods. The preconcentration time depends on the concentration level of the analytes in the samples. The method is linear in the range 2–200 ng/ml, with r.s.d. values between 1.5 and 5.0. It has been applied to the determination of copper, lead, zinc, nickel, cobalt, cadmium and manganese in synthetic water samples.
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