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  • Digitale Medien  (9.752)
  • 1995-1999  (2.288)
  • 1990-1994  (7.464)
  • Analytical Chemistry and Spectroscopy  (9.750)
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  • Digitale Medien  (9.752)
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  • 101
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 300-302 
    ISSN: 0935-6304
    Schlagwort(e): Supercritical-fluid-extraction ; supercritical-fluid-chromatography ; vitamin E ; pharmaceuticals ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: No abstract
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 102
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 315-321 
    ISSN: 0935-6304
    Schlagwort(e): Glycopeptide antibiotics ; chiral selectors ; Teicoplanin ; enantioseparations ; CZE ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Baseline separation of the enantiomers of a number of negatively charged amino and mandelic acid derivatives was achieved in less than 10 min by capillary electrophoresis in a polyacrylamide coated capillary, using the “partial filling method” (PFM) with submillimolar concentration of Teicoplanin (TE) as the chiral selector. The influence of the charge and concentration of TE, electrolyte solution composition and pH, on the enantioresolution was examined. Further proofs were brought to corroborate the hypothesis that the enantiorecognition takes place at the D-Ala-D-Ala binding site, whose blockade is responsible for the antibacterial activity of glycopeptide antibiotics. While the dependence of the chiral recognition capabilities of TE on electrolyte solution composition and pH could limit its applicability, improved sensitivity, reduction of TE wall adsorption, resulting in a good efficiency, and high cost reduction, due to the very small amount of chiral selector required, were shown as advantages of the PFM adopted in this study.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 103
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 327-334 
    ISSN: 0935-6304
    Schlagwort(e): Large volume on-column injection ; partially concurrent solvent evaporation ; solvent trapping ; retaining precolumn ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---When 0.53 mm i.d. uncoated precolumns connected to a solvent vapor exit are used for sample introduction with partially concurrent solvent evaporation, substantial losses of volatile solutes are often observed. They were found to be the consequence of solute accumulation at the front end of the flooded zone, which in turn is the result of a strong pressure drop over the flooded zone owing to the formation of plugs of sample liquid. The pressure drop causes significant solvent evaporation at the front, which enriches the solute material there and causes its loss. The use of 0.32 mm i.d. restrictions between the uncoated precolumn and the vapor exit greatly reduced this problem.
    Zusätzliches Material: 10 Ill.
    Materialart: Digitale Medien
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  • 104
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 339-342 
    ISSN: 0935-6304
    Schlagwort(e): Chlorophyll ; SFC ; supercritical fluid chromatography ; vegetables ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Complex mixtures of chlorophyll degradation products may arise during processing and storage of vegetable oil and green plant materials like broccoli and spinach. Determination of these compounds is important in the area of food chemistry. Therefore a method using packed column supercritical fluid chromatography (SFC) has been developed. The method comprises chromatography using a simple gradient of methanol in carbon dioxide at constant column back pressure of 30 MPa and a column temperature of 40°C. Effects of pressure and mobile phase composition showed the importance of applying a modifier gradient for optimal separation of the chlorophyll products. The method permits separation of 15 chlorophyll derivatives including chlorophyll a and b, pheophytins, and pyropheophytins on a C18 column in about 20 minutes. Identifications of the individual peaks were based on reference compounds, the retention order of the compounds, and their absorption spectra.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 105
    ISSN: 0935-6304
    Schlagwort(e): Capillary gas chromatography ; gas chromatography-mass spectrometry ; essential oil analysis ; Lepechinia schiedeana ; antioxidant activity ; lipid peroxidation ; Ledol; Ledol HMQC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Steam distillation (SD), simultaneous distillation-solvent extraction (SDE), microwave-assisted solvent extraction (MWE), and supercritical (CO2) extraction (SFE) were used to isolate secondary metabolites from Lepechinia schiedeana. The various extracts were analyzed by capillary gas-chromatography, on poly (dimethylsiloxane) (DB-1) and poly(ethyleneglycol) (INNOWAX), 60 m columns, using FID or MSD (EI, 70 eV). Kováts indexes, mass spectra, or standard compounds were employed for compound identification. 43, 61, 67, and 79 compounds at concentrations above 0.01% were detected in the SD, SDE, MWE, and SFE extracts, respectively. Ledol, C15H26O, was the major constituent (20.04-36.87%) in all extracts. Oxygenated sesquiterpenes (24.36-43.14%), C10H16, monoterpenes (27.70-39.87%), and C15H24, sesquiterpenes (10.04-22.22%) were the main groups of compounds present in SD, SDE, MWE, and SFE extracts. Heavy hydrocarbons (Cn 〉 15), diterpenoids, and phytosterols were found only in MWE and SFE extracts. The antioxidant activity of Lepechinia schiedeana was measured by the HRGC quantification of the volatile carbonyl compounds, final products of lipoxidation, released in a model lipid system (sunflower oil) by the effect of the Fenton reagent. The concentration of volatile carbonyl compounds decreased by 65% when lipid oxidation was induced in the presence of macerated Lepechinia plant. The protection of polyunsaturated acids in sunflower oil was also studied by measuring their concentrations after heating of the oil (180°C, 2 h) with and without macerated Lepechinia plant.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 106
    ISSN: 0935-6304
    Schlagwort(e): Silver ion HPLC ; long chain polyunsaturated fatty acid ; isopropanol ; separation of positional isomers ; degree of unsaturation ; normal phase retention effect ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A high resolution approach to silver ion HPLC was studied for the separation of positional isomers of triacylglycerols (TAGs) containing long chain polyunsaturated fatty acids (PUFA) such as eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA), and docosapentaenoic acid (DPA) in enzymatically synthesized structured TAGs. Isopropanol was used as a novel modifier in a hexane-acetonitrile based mobile phase for silver ion HPLC. Peak identification was based on HPLC-mass spectroscopy and selectivities of lipases. Positional isomers of TAGs containing one molecule of EPA, DHA, or DPA with saturated fatty acids (FAs) such as caprylic acid and palmitic acid were separated within 13 min using a gradient of hexane-isopropanol-acetonitrile as mobile phase. TAGs containing two or more EPA, DHA, or DPA were also separated from each other within 25 min, but their positional isomers were unresolved. The retention characteristics of the TAG were found to be related to the number of carbon atoms in the FAs present in addition to the number of double bonds and their isomeric configuration. One isomer with an unsaturated FA in the sn-2 position eluted faster than the other with the unsaturated FA in the sn-1 or 3 position. Species with longer chain FAs attached to TAGs with the same degree of unsaturation eluted faster than those that have shorter chain FAs. For example, docosapentaenoylhexadecanoyloctanoin (DPA/C16/C8) was eluted faster than dioctanoyldocosapentaenoin (DPA/C8/C8).
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 107
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 373-378 
    ISSN: 0935-6304
    Schlagwort(e): Electrophoresis ; electrophoretic mobilities ; CZE ; MEKC ; peptides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A computer model is presented for the prediction of the electrophoretic mobilities of peptides from physical constants derived from their amino acid sequences. The model assumes that the electrophoretic mobility can be represented by a product of four functions according to the relation:  lcomp= l(L)w(W)q(Q)c(CC), where L (a length parameter) is represented by the number of amino acid residues of the peptide, W (a width parameter) is represented by the average residue mass, Q = the charge of the peptide, and CC = the position of the center of charge relative to the center of mass. The model was used to calculate the electrophoretic mobilities of peptides in a 50 mM phosphate buffer at pH 2.5. Sixty-four test peptides ranging in size from 2 to 39 amino acid residues were used for this study. The calculated mobilities show excellent correlation with experimental measurements with a correlation coefficient greater than 0.98.
    Zusätzliches Material: 5 Tab.
    Materialart: Digitale Medien
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  • 108
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 386-390 
    ISSN: 0935-6304
    Schlagwort(e): Sulfur chemiluminescence detection ; sulfur simulated distillation ; boiling point distribution ; simultaneous FID/SCD analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A gas chromatographic system for the simultaneous acquisition of hydrocarbon and sulfur chromatograms was developed. Detection of sulfur compounds is achieved using a sulfur chemiluminescence detector (SCD) mounted in series with a flame ionization detector (FID). A constant fraction of the effluent of the FID is transferred to the SCD by means of a fixed restrictor. Unlike previous versions of this approach, the FID is not used to generate the chemiluminescent sulfur species. Rather, the FID is operated under optimum conditions for hydrocarbon analysis and a furnace is used to generate the chemiluminescent sulfur species. The system permits dual acquisition of the hydrocarbon and sulfur signals in a single analysis with a single column, since the detectors are operated in a serial fashion. The application of sulfur simulated distillation using this approach was examined, since this requires simultaneous universal and sulfur selective detection. Precision of absolute response of both the FID and SCD was typically less than 2% RSD for a standard reference material.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 109
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 391-394 
    ISSN: 0935-6304
    Schlagwort(e): REMPI-TOFMS ; laser mass spectrometry ; supersonic jet ; GC-MS ; interface ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The laser-based methods Laser Induced Fluorescence (LIF) and Resonance-Enhanced Multi-Photon Ionization (REMPI) can be used as highly selective detection modes for gas chromatography (GC). One major prerequisite for successful application of these detection methods is the availability of appropriate and reliable interfaces between the GC effluent and the molecular beam inlet. When a pulsed supersonic molecular beam (jet) source is used, the analyte molecules are efficiently cooled, allowing maximum selectivity of the laser spectroscopic detection methods. However, several technical problems have to be solved for practical realization of a GC-supersonic jet valve hyphenation. The pulsed jet interface should not interfere with the GC properties and the supersonic molecular beam properties. Further a good working cycle for the conversion from the continuously flowing GC current to the pulsed jet gas flow should be attained. This paper presents a novel setup of a GC-pulsed jet interface. The construction allows temporal and spatial compression of the analyte molecules in jet gas pulse and thus an increase of the detection sensitivity. Moreover, the GC effluent comes into contact only with glass surfaces and not with valve parts like plungers and seals. This reduces memory effects and sample decomposition. The valve setup is tested with a REMPI-TOFMS instrument.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 110
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 414-416 
    ISSN: 0935-6304
    Schlagwort(e): Selenium ; water ; SPME ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A method for the selective determination of Se4+ and Se6+ using solid phase microextraction (SPME) and GC/MS analysis is presented. Se4+ is selectively derivatized by reaction with 4,5-dichloro-1,2-phenylenediamine to form the corresponding piazselenolo complex, extracted by the SPME fiber, and determined by GC/MS. The RSD at a 5 μg/L concentration was 9.88% and the theoretical detection limit 6 ng/L. The method was employed to test real matrices; tap and river water were analyzed before and after spiking giving a recovery rate of 102% in river water and 97% in tap water.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 111
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 565-588 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Kovats retention index ; vapor pressure ; boiling point ; Wilson activity coefficient ; binary phase diagrams ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Non-ideal mixing in a dimethylsilicone stationary phase is modeled according to the Wilson activity coefficient. Pure liquid vapor pressures of alkylated compound series are calculated from capillary GLC retention with the functional group heat of solution in a polymer solvent. The new method uses the Kovats index, molar mass, and functional group to determine the bubble line of a compound. Boiling points at reduced and normal pressure are compared to literature values of 194 gasoline components. An unlike molecular pair interaction parameter is derived, using only bubble line data of the pure liquids. Binary phase diagrams are constructed and compared to vapor liquid equilibrium data.
    Zusätzliches Material: 22 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 112
    ISSN: 0935-6304
    Schlagwort(e): Computer modeling of GC ; computer simulation of GC ; computer-assisted GC analysis ; GC multicolumn analysis ; heart cutting GC analysis ; computer-assisted column design ; computer-assisted selectivity tuning ; retention index mapping ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The analysis of four components in a mixture containing many possible interferents is simplified by heart-cutting serially connected columns containing stationary phases of widely different polarities. The design of the proper lengths of the two columns and timing the heart-cuts is accomplished with the aid of a computer simulation of the problem. The computer program calculates the proper lengths of column to produce the shortest analysis time and also outputs the predicted chromatograms from both columns. The chromatogram from the first column is used to construct the timing gates for the heart-cuts and the chromatogram from the second or analytical column is used to set integration gates for the selected compounds of interest.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 113
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 609-612 
    ISSN: 0935-6304
    Schlagwort(e): Cyclodextrins ; 2-p-toluidinyl-6-naphthalenesulfonate ; indirect fluorimetric detection ; liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Cyclodextrins (CD's) were visualized by postcolumn mixing with 2-p-toluidinylnaphthalene sulfonate (TNS) in liquid chromatography. The indirect detection is based on fluorescence enhancement due to the formation of an inclusion complex between TNS and CD's. β-CD gave larger signal intensity than α- and γ-CD. Different selectivities were observed for alkyl-bonded silica stationary phases with different chain length.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 114
    ISSN: 0935-6304
    Schlagwort(e): Enantioselective multidimensional gas chromatography-mass spectrometry (enantio-MDGC-MS) ; methylcitric acid (MCA) ; inherited metabolic disease ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Methylcitric acid (2-hydroxybutane-1,2,3-tricarboxylic acid-MCA) is a structural analogue of citric acid, but due to an additional methyl group it is a chiral molecule with two stereogenic centers and thus four stereoisomers are conceivable. MCA occurs naturally as prominent metabolite in body fluids of patients with inherited metabolic diseases such as propionic acidemia, methylmalonic aciduria, or holocarboxylase synthetase deficiency. Therefore methylcitric acid is considered to be an important diagnostic marker for these diseases. MCA is most likely produced from accumulated propionyl-CoA in these diseases by the enzyme si-citrate synthase from the citric acid cycle; however, there are other enzymes known which could catalyze the same reaction with different stereoselectivity, such as re-citrate synthase or the more specific enzyme methylcitrate synthase, found in microorganisms. Almost all methods dealing with MCA in the literature are non-enantioselective. For that reason there is no information about occurrence of MCA enantiomers in healthy people, patients with propionic acidemia, methylmalonic aciduria, or holocarboxylase synthetase deficiency and about value of enantiomeric distribution for diagnosis and long-term treatment. The enantioselective analysis of MCA as corresponding trimethyl ester was achieved by enantioselective multidimensional gas chromatography coupled with mass spectrometry using heptakis-(2,3-di-O-methyl-6-O-tert-butyl-dimethylsilyl)-β-cyclodextrin as chiral stationary phase. The described method allows a reliable screening of MCA in complex matrices like urine without time consuming sample preparation and with mass selective detection. During this investigation urine samples from various patients and healthy controls were analyzed. As concluded, MCA is a good diagnostic marker and can be easily measured by the method presented. Only the two stereoisomers (2S,3R) and (2S,3S) were detectable in patients and healthy controls. The varying ratios of these stereoisomers cannot presently be correlated with the health status of patients, although there are some indications that this might be possible. However, the quantitative levels of MCA, determined as the ratio of MCA absolute peak area divided by 1,000 to the creatinine contents of urine samples in this investigation, showed a dependence on the state of health and MCA would thus also be a possible marker for long-term treatment. Such a substance is of major interest nowadays since there are different studies searching for such a long-term marker in propionic acidemia or methylmalonic aciduria.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 115
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 623-627 
    ISSN: 0935-6304
    Schlagwort(e): Supercritical fluid extraction ; hydrocarbons ; high temperature ; thermal desorption ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The extraction of n-alkanes, polyaromatic hydrocarbons (naphthalene, methylated naphthalenes, phenanthrene, methylated phenanthrenes, anthracene, and methylated anthracenes) and biomarkers (hopanes) from Posidonia shale by high temperature supercritical fluid (HT-SFE) carbon dioxide extraction has been evaluated, including the relative contributions from thermal desorption and relative comparisons to conventional Soxhlet extraction. These current results confirm those of previous studies indicating a widely differing extractability of strongly and weakly associated hydrocarbons in ancient sediments and the significantly higher recoveries possible using HT-SFE compared to conventional Soxhlet extraction. The present study also demonstrates that these high HT-SFE recoveries are due to true extraction rather than simple thermal desorption and that this procedure is a useful tool to study speciation as well as total extractable hydrocarbons from sediments.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 116
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 631-634 
    ISSN: 0935-6304
    Schlagwort(e): Dill ether ; stereoselective synthesis ; dill ether stereoisomers ; enantioselective multidimensional gas chromatography-mass spectrometry (enantio-MDGC/MS) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 117
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 639-643 
    ISSN: 0935-6304
    Schlagwort(e): Cyclodextrin ; Halowax ; hexachloronaphthalene ; PCN ; polychlorinated naphthalenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 118
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 501-508 
    ISSN: 0935-6304
    Schlagwort(e): Fast GC ; film inefficiency factor ; high pressure drop ; thick film columns ; thin film columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The negative effect of the liquid stationary phase film thickness on the column efficiency is strongest for peaks with retention factors, k, in the vicinity of k = 0.3-0.4 and rapidly diminishes with the departure of k from that region. Additionally, at the high pressure drop required for fast analysis of complex mixtures, the negative effect of the same film thickness diminishes with the increase in column length, regardless of the k values. In practice, it is recommended to ignore the film thickness and optimize the columns as thin film ones regardless of their actual film thickness. Accounting for the film thickness results only in a modest improvement in the resolution for a few affected peaks - those with k = 0.3-0.4. However, this improvement comes at the cost of a substantial increase in analysis time, and should be used only as the action of the last resort.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 119
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 514-520 
    ISSN: 0935-6304
    Schlagwort(e): Solid-phase extraction ; high temperature - gas chromatography ; gas chromatography - mass spectrometry ; wax esters fennel seed oil ; caraway seed oil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A rapid method for the isolation and quantitative determination of wax esters in vegetable oils was developed. For the first time wax esters in oils were separated from the triglyceride matrix by means of solid-phase extraction, which allows rapid sample preparation in parallel and therefore a high sample throughput. The thus obtained wax ester fractions of fennel and caraway seed oils were analyzed by high temperature gas chromatography. GC-MS analyses were carried out using electron impact ionization in order to characterize the wax ester fraction. With respect to the results of the GC-MS analyses different isomers of saturated wax esters with the same carbon number were observed. Additional monounsaturated wax esters with an unsaturated fatty acid moiety were identified.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 120
    ISSN: 0935-6304
    Schlagwort(e): Clusia criuva Cambess ; counter-current chromatography ; flavonoids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The family Guttiferae belongs to the superorder Theiflorae, order Theales and according to Dahlgren's system of classification, it is equivalent to Hypericaceae (=Clusiaceae) [1]. This family consists of 49 genera encompassing over 1000 species of wide distribution in the tropics as shrubs and trees [2]. Plants of the genus Clusia have been used in folk medicine for the treatment of different kind of illness such as: febrifuge, anti rheumatic, purgative, for stomach problems and, in Brazil, they are very commonly used to heal wounds [3]. The key of any study of material from natural sources is the availability of suitable separation methods for the isolation of pure products [4-6]. Tentatives for separations using chomatography on solid support phases were not very efficients in the fractionation of Clusia criuva Cambess methanolic/ethyl acetate extracts. However, the use of counter-current chromatography, an all liquid technique, showed advantages in comparison with the more traditional liquid-solid separation methods and even with HPLC. In this sense it was possible to isolate flavonoid glycosides from ethyl acetate extract of Clusia criuva, in a very short operation time.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 121
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 541-546 
    ISSN: 0935-6304
    Schlagwort(e): Solvating gas chromatography ; gas chromatography ; fast separation ; pesticides ; herbicides ; aldehydes ; packed capillary columns ; polymer-encapsulated silica ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Rapid separations of selected environmentally important polar compounds using polymer-encapsulated silica stationary phases and a carbon dioxide mobile phase under solvating gas chromatography (SGC) conditions are reported. Ten underivatized short chain aldehydes and ten nitrogen-containing herbicides were separated within 1 min and 5 min, respectively, using a 30 cm×250 μm i. d. column packed with diol-bonded, polyethylenimine (PEI)-coated, and hexamethyldisilazane (HMDS)-end-capped silica particles (5 μm, 120 Å). Seven organophosphorus pesticides were resolved in less than 5 min using a 30 cm×250 μm i. d. column packed with polymethylhydrosiloxane-deactivated and SE-54 encapsulated silica particles. Separation numbers per unit time increased with pressure and temperature ramps. Both rapid pressure and temperature programming can be used to increase the speed of SGC. The effects of pressure and temperature on apparent retention factors of solutes with various polarities were investigated using diol-PEI-HMDS silica particles in SGC.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 122
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 559-564 
    ISSN: 0935-6304
    Schlagwort(e): Liquid chromatography ; dead time ; multiparametric least-squares adjustment ; homologous series ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In reversed phase liquid chromatography (RP-HPLC), the validity of a multiparametric non-linear least-squares regression iterative method for the determination of the column dead time tM and the regression parameter (slope b), based on the use of alkan-2-ones, alkyl aryl ketones, and 1-nitroalkanes has been evaluated. The determination of tM and b has been extensively studied for two mobile phase systems acetonitrile-water and methanol-water on seven octadecyl-C18 and one octyl C8 analytical columns. The calculated tM and b values were compared with those obtained by Guardino's and Grobler's methods. The influence exerted thereon by the nature of the homologous series, the mobile phase composition, and the packing materials were investigated.
    Zusätzliches Material: 5 Tab.
    Materialart: Digitale Medien
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  • 123
    ISSN: 0935-6304
    Schlagwort(e): SFE ; experimental design ; additives ; recycling ; polyolefins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The performance and feasibility of supercritical fluid extraction (SFE) applied to the extraction of some antioxidants (Irganox 1076, Irgafos 168) and one UV-stabilizer (Chimassorb 81) from both virgin and recycled low density polyethylene (LDPE), and virgin high density polyethylene (HDPE) are studied. Due to the high number of variables a full-factorial design has been applied to minimize the number of experiments required to reach the optimum extraction conditions. Further analysis has been carried out off-line by reversed-phase HPLC. Modification of the physical properties of the polymeric matrix and increased number of recycling cycles as well as the influence of physical properties on the efficiency of SFE are also discussed.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 124
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 595-598 
    ISSN: 0935-6304
    Schlagwort(e): Xylitol ; samarium ; weak association ; equilibrium constant ; capillary electrophoresis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 125
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 599-603 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrochromatography ; retention ; mixed stationary phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Most commercially available instruments for capillary electrochromatography (CEC) have a fixed configuration and lack the flexibility to use shorter columns. Applying a blended stationary phase (a phase consisting of a given ratio of bare silica and reversed phase material) can simulate columns of different length in CEC. The goal of this work was to examine the effect of the degree of blending of reversed-phase columns (with bare silica) on the speed of the separation of neutral compounds in CEC. Optimum column packing mixture was determined from the variation of the solute retention factors as a function of the ratios of blending of reversed-phase and bare silica. By adjusting the column composition, solute retention factors and the analysis run time were halved when compared to a pure reversed-phase column of the same length. Stationary phase blending can be considered as an additional parameter to mobile phase variation, column temperature and applied electric field for the optimization of selectivity and analysis time. By adjusting the stationary phase composition, mobile phase composition, column temperature and applied electric field, the analysis run time of neutral components was decreased more than 75% when compared to a separation obtained on neat reversed-phase column of the same dimensions. The linear dependence of the retention factors as a function of the blend ratio (reversed phase/bare silica) offers a framework for designing a “blended” packed capillary column for CEC separations.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 126
    ISSN: 0935-6304
    Schlagwort(e): Liquid chromatography ; retention index ; multiparametric least-squares adjustment ; homologous series ; nitramines ; nitroaromatics ; aminoaromatics and nitrophenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In reversed phase liquid chromatography, the retention indices of some neutral and acidic explosives and related compounds (nitramines, nitroaromatics, aminoaromatics, and nitrophenols) based on the alkan-2-one, alkyl aryl ketone, and 1-nitroalkane retention index standards have been determined by the application of a new mathematical adaptation method, viz. a multiparametric least-squares regression iterative method. This method was applied to two types of columns. The first group includes six octadecyl-C18 columns with different packing materials and obtained from different manufacturers, while the second group comprises one octyl-C8 column. The retention indices have been extensively studied using either methanol-water or methanol-phosphate buffer mobile phase systems. The calculated multiparametric retention indices values were compared with those obtained by Guardino's, Grobler's, and Kovàts' methods. The influences of the concentration of the organic modifier in the mobile phase, aqueous mobile phase pH, and the column packing material on the retention indices of the explosives were also investigated. Good agreement was observed between the retention indices calculated by the use of the four mathematical methods for both neutral and acidic explosives.
    Zusätzliches Material: 4 Tab.
    Materialart: Digitale Medien
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  • 127
    ISSN: 0935-6304
    Schlagwort(e): Organochlorine compounds ; pesticides ; food analysis ; tomatoes ; GLC-ECD ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A method is described for the simultaneous extraction and determination of twenty organochlorine pesticides residues [hexachlorocyclohexane (HCH) isomers (α, β, γ, δ), aldrin, dieldrin, endrin, heptachlor and its epoxide (HE), hexachlorobenzene (HCB), α-endosulfan, o,p′-DDD, p,p′-DDD, o,p′-DDE, p,p′-DDE, o,p′-DDT, p,p′-DDT, dicofol, methoxychlor, and mirex] that were spiked in tomatoes. Samples were extracted with ethyl acetate, and the extract was subjected to a rapid clean-up using a Florisil column. The residues were determined by GLC-ECD using two columns of different polarity. The calibration graph correlation coefficient ranged from 0.9903 to 0.9990. The recoveries ranged from 95 to 99% with relative standard deviation ranging from 0.5 to 14.7% in the concentration range 0.005 to 0.2 μg/g. The limits of detection ranged from 0.004 to 0.05 μg/g and the limits of quantification ranged from 0.005 to 0.174 μg/g.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 128
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 628-630 
    ISSN: 0935-6304
    Schlagwort(e): p-Nitrophenol ; urine ; SPME ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 129
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 635-638 
    ISSN: 0935-6304
    Schlagwort(e): High resolution gas chromatography ; thermal desorption ; archeological cosmetic powders ; PTV injector ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 130
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 666-670 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrochromatography ; mixed packing technique ; electroosmotic flow ; retention mechanism ; fast analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Mixed packing capillary electrochromatography (MP CEC) with the stationary phase comprising a physical mixture of strong cation exchange (SCX) phase and octadecysilyl (ODS) phase was developed. With the existence of a sulfonic acid group on the surface of SCX, not only could the electroosmotic flow (EOF) remain high at low pH, but also the hydrophilicity of the stationary phase was increased greatly, leading to broad adaptable ranges of both pH and organic modifier concentration in the mobile phase. At the same time, with the coexistence of C18 on the surface of ODS, both the retention and the resolution of samples were improved. Accordingly, MP CEC combined the advantages of both SCX and ODS columns. Effects of operation parameters on EOF and the capacity factors of solutes as well as the retention mechanism of such a column were studied systematically. In addition, MP CEC columns were used in the analysis of strong polar solutes as well as for the high speed separation of acidic, basic, and neutral compounds in a single run.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 131
    ISSN: 0935-6304
    Schlagwort(e): Enantioselective capillary gas chromatography ; chiral stationary phase ; chiral recognition mechanism ; cholic acid ; cyclocholates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The suitability of cyclocholates as chiral selectors in gas chromatography has been evaluated. We present the synthesis and characterization of two cyclocholates, viz. 3α,7α-diacetoxycyclo[3]cholate and 3α,7α-diacetoxycylo[4]cholate. Mixtures of these new selectors with polysiloxanes were tested as chiral stationary phases in capillary gas chromatography. Several enantiomer separations of common racemates were achieved with the 3α,7α-diacetoxycyclo[3]cholate at 10% in OV-1701 (w/w). It was shown that column efficiency was strongly dependent on temperature and that enantioselectivity was very sensitive to column conditioning. This chromatographic behavior suggested that cyclocholates were only dispersed in polysiloxane. Thus, it was assumed that chiral discrimination occurred via enantioselective adsorption interactions of enantiomers at the surface of the solid chiral selector dispersed in the polysiloxane matrix OV-1701.
    Zusätzliches Material: 11 Ill.
    Materialart: Digitale Medien
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  • 132
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 683-686 
    ISSN: 0935-6304
    Schlagwort(e): Vacuum gas oils ; packed column chromatography ; n-paraffins ; carbon number distribution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Gas chromatographic methods are of widespread use in the petroleum industry for assessing petroleum and derivatives quality. The feedstocks for catcracking processes are very sensitive to the n-paraffin contents, which can be accurately determined using capillary column chromatography. Nevertheless, packed column chromatography does have potential advantages, viz. sometimes shorter analysis times, lower costs, higher column capacity, for vacuum gas oil analysis. This paper presents a method for such a determination using a Dexsil-300 packed column. The results obtained (n-alkane contents, carbon number distribution) agree fairly well with those obtained on a 30 m × 0.25 mm DB-1 fused silica capillary column.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 133
    Digitale Medien
    Digitale Medien
    Springer
    Space science reviews 84 (1998), S. 199-206 
    ISSN: 1572-9672
    Schlagwort(e): Nuclear reactions ; Nucleosynthesis ; Abundances ; Stars:Evolution ; Interior ; Rotation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Physik
    Notizen: Abstract We first recall the observational and theoretical facts that constitute the so-called 3He problem. We then review the chemical anomalies that could be related to the destruction of 3He in red giants stars. We show how a simple consistent mechanism can lead to the destruction of 3He in low mass stars and simultaneously account for the low 12C/13C ratios and low lithium abundances observed in giant stars of different populations. This process should both naturally account for the recent measurements of 3He/H in galactic HII regions and allow for high values of 3He observed in some planetary nebulae. We propose a simple statistical estimation of the fraction of stars that may be affected by this process.
    Materialart: Digitale Medien
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  • 134
    ISSN: 0935-6304
    Schlagwort(e): Epoxytriacylglycerols ; high temperature gas chromatography ; hydroxytriacylglycerols ; ketotriacylglycerols ; lipids ; negative chemical ionization mass spectrometry ; SOP-50 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Five seed oils consisting of unusual triacylglycerols have been examined by high temperature gas chromatography using glass capillary columns coated with the stationary phase SOP-50 (50%-diphenyl-50%-dimethylpolysiloxane, methoxy-terminated). The investigated hydroxy, epoxy, and ketokonjuene triacylglycerols were first derivatized in order to permit analysis by high temperature gas chromatography. Structural elucidation of the intact triacylglycerols was performed with high temperature gas chromatography/negative chemical ionization-mass spectrometry using NH3 as a reagent gas. Individual derivatized lipid species with a molecular weight up to 1176 g/mol could be identified.
    Zusätzliches Material: 10 Ill.
    Materialart: Digitale Medien
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  • 135
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 169-174 
    ISSN: 0935-6304
    Schlagwort(e): CZE ; detection limit ; signal-to-noise ratio ; correlation chromatography ; reproducibility ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Poor signal-to-noise ratios and analytical reproducibility in capillary electrophoresis were improved by application of multiple injections of the same sample at (pseudo) randomly chosen time moments. One order of signal-to-noise ratio improvement was achieved in practice using an in-house developed computer-controlled pneumatic sampler. However, it is demonstrated here that better implementation of the capabilities of multiple input requires that the detector signal noise be “pre-whitened”, i.e. spikes, baseline drift, oscillations etc. must be removed from the detector signal before transforming it to the electropherogram in the common form. Such filtering of the detector signal was realized by implementing iterative, menu-driven software written in Matlab, a high-level programming language.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 136
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 181-184 
    ISSN: 0935-6304
    Schlagwort(e): Trace analysis, atmospheric ; digital signal processing ; signal to noise reduction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 137
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 189-192 
    ISSN: 0935-6304
    Schlagwort(e): Chiral stationary phases ; pyrethroic acids ; enantiomer separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 138
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 193-196 
    ISSN: 0935-6304
    Schlagwort(e): capillary electrophoresis ; dissolving solvent selection ; optimization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 139
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 201-208 
    ISSN: 0935-6304
    Schlagwort(e): PAN ; peroxyacetyl nitrate ; alkyl nitrate ; chlorinated hydrocarbons ; halocarbons ; capillary GC-ECD ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A cryogenic preconcentration/high-resolution gas chromatographic technique has been developed for the rapid, simultaneous quantitation of C1-C4 organic nitrates and halocarbons in ambient air. Whole-air samples are collected in TedlarTM bags by an evacuated-chamber method. Samples were stable in 0.010-cm-thick bags for 24 h if they were immediately stored in a freezer at -25°C. Analytes in a 50-cm3 air sample were efficiently preconcentrated on fused-silica beads at -180°C and thermally desorbed at 30°C. High-resolution gas chromatography with a cross-linked polydimethylsiloxane fused-silica capillary column and an electron-capture detector were used for separation and quantitation of the analytes. An analysis time of about 12 min was facilitated by sample cryofocusing at -180°C and oven temperature programming. Recoveries of the analytes by the evacuated-chamber method were better than 95%. The sensitivity of the technique for sample volumes of 50 cm3 is in the sub-parts-per-trillion by volume (ppt[v]) range for many of the analytes, with an average precision of about ±5% for analytes at levels of about 10 ppt(v).
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 140
    ISSN: 0935-6304
    Schlagwort(e): capillary electrophoresis ; enantiomer separation ; hydroxypropyl-β-cyclodextrin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Following an extended screening project, 86 racemic drugs were investigated by capillary zone electrophoresis in the presence of the chiral solvating agent (CSA) hydroxypropyl-β-cyclodextrin. A total of 42 drugs out of 86 tested was thereby separated into enantiomeric pairs. Statistical analysis of the numerous experiments performed un der identical conditions reveals a loose correlation of the migration separation factor (αm) with the migration retardation factor (Rm). For a subset of 23 drugs, a drop in the concentration of the CSA was also studied, showing the way to further optimization.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 141
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 253-257 
    ISSN: 0935-6304
    Schlagwort(e): Edible oils ; lipids in foods ; HPLC ; Polycyclic Aromatic Hydrocarbons (PAHs) ; off line LC-LC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 142
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 234-240 
    ISSN: 0935-6304
    Schlagwort(e): Micellar electrokinetic capillary chromatography ; electroosmotic migration ; electrophoretic migration of micelle ; retention mechanism ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In the present work, four organic modifiers, viz. urea, dioxane, methanol, and tetrahydrofuran, were comparatively and systematically studied in terms of their effects on electrokinetic migration behavior and the retention mechanism of homologous solutes in MECC. The results showed that the electroosmotic mobility, μeo, and the electrophoretic mobility of a micelle, μep,mc, decrease linearly with increasing organic modifier concentration. The ability of organic modifiers to lower μeo is greater than their ability to lower μep,mc. The negative values of the slopes of these linear relationships, Deo and Dep,mc, increase along the series the order urea 〈 methanol 〈 dioxane 〈 tetrahydrofuran. The logarithm of the capacity factor (ln k′) of uncharged homologous solute, which is mainly determined by the hydrophobic interaction, decreases linearly with increasing organic modifier concentration, due not only to the decrease in the partition coefficient but also to the decrease in the phase ratio. A linear relationship was observed between the slope of the plot of ln k′ vs. organic modifier concentration and the carbon number of homologous compound. The slope of such a relationship can characterize the hydrophobicity of the organic modifier. The hydrophobicity of such organic modifiers is also found to increase along the series urea 〈 methanol 〈 dioxane 〈 tetrahydrofuran.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 143
    ISSN: 0935-6304
    Schlagwort(e): Fluoroquinolone ; ASTED ; HPLC fluorescence ; sarafloxacin ; flumequine ; oxolinic acid ; chicken liver ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A recently introduced programmable fluorescence detector was compared with a single wavelength fluorescence detector for quantification of fluoroquinolone (FQ) antibacterial agents, which have widely varying spectral characteristics. The two detectors were connected in parallel to an HPLC system to test their performance characteristics. With single wavelength detection, two FQs, flumequine and oxolinic acid could be detected at an emission wavelength of 368 nm in a single chromatogram while a third FQ, sarafloxacin, was not observed at that wavelength. Similarly, when the detector was optimized for sarafloxacin emission at 440 nm, the other two compounds were undetected. In contrast, all three FQs were quantified at their individual maxima in a single run using the programmable fluorescence detection. The applicability of an HPLC - programmable fluorescence detector, in combination with on-line microdialysis, also was evaluated using chicken liver fortified at low ppb levels with the three FQs. After on-line microdialysis sample clean up, the resultant HPLC chromatograms were free of background interference enabling the programmable detector to optimize the quantitation of the three analytes in a single run. The limit of quantification (LOQ) determined for each FQ was 1.0 ppb and the limit of detection (LOD) was 0.2 ppb, an order lower in magnitude than was obtainable with single wavelength detection.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 144
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 267-281 
    ISSN: 0935-6304
    Schlagwort(e): Chemically bonded phases, CBPs ; liquid chromatography, HPLC ; preparation; surface characterization ; column evaluation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In order to increase chromatographic selectivity and to extend the analytical capability of reversed phase liquid chromatography (RP HPLC) many investigators have concentrated on the preparation of silica based column packings with chemically bonded phases (CBP). These phases have also been successfully used in sample preparation techniques, mainly in solid phase extraction (SPE). Although alkyl bonded phases (e.g., C2, C8, and C18) are the most widely used packings in RP HPLC and SPE, various specific applications require CBPs with polar functional groups (e.g., -NH2, -NO2, -CN, and/or -OH). The solution of problems with separation of complicated chiral compounds was attempted by applying stationary phases with chiral selectors (e.g., cyclodextrins, Pirkle phases, crown ethers, etc.). On the other hand, packings with pseudo-membrane or liquid crystal properties have been utilized for the separation of various substances of natural origin. Porous silica is commonly used as a support in the preparation of CBPs. Its physico-chemical characteristics, such as: type and structure of siliceous matrix, porosity, type and concentration of silanol groups, as well as surface purity, strongly influence the density and structure of chemically bonded phases. Recognition of these properties is helpful in optimizing separation processes based on RP HPLC elution and/or extraction of substances with polar character.
    Zusätzliches Material: 12 Ill.
    Materialart: Digitale Medien
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  • 145
    ISSN: 0935-6304
    Schlagwort(e): capillary gas chromatography ; microplasma mass spectrometry ; radio frequency plasma ; element-selective detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Capillary gas chromatography was performed with mass spectrometric detection using a novel microplasma ion source for operation in an element-selective mode. The ion source was a 350 kHz radio frequency helium plasma, which was sustained inside the 4 cm end of a 0.32 mm i.d. fused silica capillary column, and located inside the high vacuum chamber of the quadrupole mass spectrometer. Due to the low volume of the ion source, a stable low pressure discharge was produced utilizing only the 2.25 mL min-1 of GC carrier gas (helium) for plasma support. Small amounts of oxygen (0.1-0.2% v/v) were added to the plasma gas in order to prevent carbon deposits and to enhance signal-to-noise ratios. Chlorine and bromine were selectively detected at the 5-20 pg s-1 level (S/N = 2), and both produced a response that was linear within 3 orders of magnitude.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 146
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 315-316 
    ISSN: 0935-6304
    Schlagwort(e): Tertiary amine ; ruthenium ; chemiluminescence ; photochemical oxidation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 147
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 303-307 
    ISSN: 0935-6304
    Schlagwort(e): gas chromatography ; modified silica gel ; gaseous standard mixtures ; FID calibration ; carbon monoxide and carbon dioxide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Quartz rods coated with a thin layer of chemically modified silica gel have been used for the generation of a two-component gaseous standard mixture containing carbon monoxide and carbon dioxide. A new method based on thermal decomposition of immobilized compounds chemically bonded to the surface of silica gel has been used in the generation process. The oxalic acid moiety bonded to the glycydoxypropylsilylated surface of silica gel underwent decarbonylation and decarboxylation at 300°C, yielding carbon monoxide and carbon dioxide. On-line connection of a thermal desorber with the GC/FID enabled calibration of the detector following the process of methanization of CO and CO2. The following amounts of CO and CO2 were generated per unit length of the rod: 15.1 × 10-8 Mol cm-1 (RSD = 5.71%) for CO and 34.2 × 10-8 Mol cm-1(RSD = 5.16%) for CO2.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 148
    ISSN: 0935-6304
    Schlagwort(e): Large-volume on-column injection ; gas chromatography ; infrared spectrometry ; microcontaminants ; solid-phase extraction ; open-split interface ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A large-volume on-column GC-cryotrapping-IR system was developed for injections of up to 100 μl of organic extracts. Considerable reduction of the solvent-and-water background and enhanced analyte detectability was achieved by using an open-split interface between the GC column and the IR detector and improving the leak-tightness of the system. The system was combined with solid-phase extraction to yield on-line SPE-GC-IR. With this set-up, sample volumes of only 20 ml sufficed to detect, and identify, microcontaminants in tap and surface water at the 0.1-1 μg/L level. Detection limits were on the order of 15 ng/L for tap water when using appropriate functional-group chromatograms. Or, in other words, SPE-GC-IR is a suitable technique for the screening of environmental water samples for functional groups, i.e. classes of compounds, of interest.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 149
    ISSN: 0935-6304
    Schlagwort(e): Adsorption/thermal desorption sampling instrument ; capillary gas chromatography ; electrolytic conductivity detector ; photoionization detector ; environmental air monitoring ; hazardous air pollutants ; volatile organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 150
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 475-476 
    ISSN: 0935-6304
    Schlagwort(e): Scent glands ; defense substances ; n-alkanes ; furanones ; 2-alkenals ; 2-alkenyl acetates ; 2-decenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 151
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 491-497 
    ISSN: 0935-6304
    Schlagwort(e): Fast GC ; narrow-bore columns ; trace analysis ; splitless injection ; on-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The use of hot splitless, cold splitless, and on-column injections for trace analysis in narrow-bore capillary GC is evaluated. Despite the low flow rates for the columns used, the required splitless times for splitless injections can be surprisingly short if liners with a small inside diameter are used. On-column injection can be applied by using an appropriate normal-bore precolumn coupled to the narrow-bore analytical column using a specially designed low dead volume column connector. The effects of the experimental conditions such as sample volume, injection temperature, and initial oven temperature on peak focusing and the discrimination and degradation behavior of the analytes are discussed. The possibilities to obtain sensitive and fast separations are illustrated by various applications.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 152
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 505-508 
    ISSN: 0935-6304
    Schlagwort(e): capillary electrophoresis ; inorganic ions ; polyethyleneimine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A capillary zone electrophoresis (CZE) method for the simultaneous assay of bromide, iodide, nitrite, nitrate, and thiocyanate using direct UV detection is reported. The method is based on the separation of anions in a capillary coated with a cationic polymer, polyethyleneimine (PEI). The minimum detection limits, reproducibility of peak areas, and migration times were determined at the optimal condition. The method was applied to the analysis of tap water and human urine. The changes in separation selectivity of the anions resulting from addition of the cationic polymer to the buffer were investigated.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 153
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 523-526 
    ISSN: 0935-6304
    Schlagwort(e): High-performance liquid chromatography ; gardenia constituent separation ; genipin gentiobioside ; geniposide ; crocin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 154
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 435-439 
    ISSN: 0935-6304
    Schlagwort(e): Micellar Electrokinetic Chromatography (MEKC) ; counter pressure moderated MEKC ; migration time window ; peak resolution and peak capacity in MEKC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The influence of a hydrostatic counter pressure on basic mobility equations in MEKC was analyzed theoretically and investigated experimentally. Taking into account the influence of counter pressure, the modified mobility equations predict a decreased migration time ratio t0/tMC, which was confirmed by results obtained in SDS-MEKC separation of a homologous series of n-alkyl phenyl ketones. As a result, the migration time window could be enlarged in a simple way without having to change the chemistry of the system. Although counter pressures reduce peak efficiency in MEKC by disturbing the plug profile, the concomitant enlargement of the migration time window compensates for this effect. Especially for later migrating compounds, peak resolution could be enhanced at moderate counter pressures. The overall peak capacities within the whole migration window increases slightly when applying counter pressures up to 10 mbar.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 155
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 445-449 
    ISSN: 0935-6304
    Schlagwort(e): chiral separation ; organic cation effect ; ethylamines ; ethanolamines ; basic drugs ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---This paper addresses the influence of small organic cations in the background electrolyte (BGE) on chiral separation by capillary zone electrophoresis (CZE). Seven basic drugs, viz. alprenolol, amphetamine, anisodamine, isoprenaline, pinacidil, synephrine, and verapamil were used as test compounds with hydroxylpropyl-β-cyclodextrin (HP-β-CD) as the chiral selector. Resolution of the chiral test compounds was studied at pH 2.5 in the presence of Tris, ethanolamine, diethanolamine, triethanolamine, diethylamine, and triethylamine, which exist in their cationic forms at this pH value. Among the six cationic additives studied, triethylamine is most effective in enhancing resolution. A tentative mechanism of the effect is proposed.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 156
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 569-573 
    ISSN: 0935-6304
    Schlagwort(e): Chinese herbal preparation ; Shao-yao-tang ; pharmaceutical analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A high-performance liquid chromatographic method for the separation of twenty one constituents of Shao-yao-tang including six flavonoids, six alkaloids, three anthraquinones, three carboxylic acids, one monoterpene, one saponin, and one aldehyde was developed. Detection at 275 nm with a linear gradient elution system consisting of tetrabutylammonium bromide (TBA) and acetic acid solution was found to be suitable for determination of nineteen marker substances in an unpretreated Shao-yao-tang extract within 75 min. This method can also be used to analyze 11-14 components in a number of Chinese herbal preparations such as San-huang-hsieh-hsin-tang, Ching-chieh-lien-chiao-tang, San-tsung-kuei-chien-tang, Chai-hu-ching-kan-tang, and Ching-yin-li-ke-tang.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 157
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 575-576 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrochromatography (CEC) ; chiral separations ; Vancomycin stationary phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 158
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 577-581 
    ISSN: 0935-6304
    Schlagwort(e): Volatiles ; Bromeliaceae ; Bromelia plumieri ; glycosidically bound volatiles ; aroma precursors ; glucoconjugates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 159
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 587-591 
    ISSN: 0935-6304
    Schlagwort(e): capillary GC ; polymethoxyflavones ; citrus oil ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The cold pressed peel oils of three species of citrus fruit, viz. sweet orange, tangerine, and grapefruit, have been examined for polymethoxyflavones by GC and GC-MS. Four GC column stationary phases were compared and separation of the six predominant orange oil polymethoxyflavones was obtained isothermally at 310°C in under ten minutes, including the resolution of the polymethoxyflavones from β-sitosterol. The nature of the stationary phase and the analysis temperature exercise dramatic effects on the resolution and elution order of the components, DB-35ms providing the best overall separation. A temperature programmed separation is also presented and the polymethoxyflavone composition of all three oils, as determined by GC-MS, is described. This is the first reported GC-MS study of the PMFs of these citrus species. While tangerine oil is as rich in polymethoxyflavones as orange oil, they are less abundant and occur at lower concentrations in grapefruit oil. Hydroxy-polymethoxyflavones were identified by GC-MS in tangerine oil. One hydroxy-pentamethoxyflavone, M+ = 388, identified in tangerine was also present at low levels in both orange and grapefruit oils. These results are compared with previous studies utilizing HPLC and GC.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 160
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 605-607 
    ISSN: 0935-6304
    Schlagwort(e): Reversed-flow MEKC ; separation according to polarity ; organic modifiers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Reversed-flow MEKC, i.e. MEKC at low pHs to suppress the electroosmotic flow, was evaluated for the separation of some homologous series. At low pHs compared to MEKC, the elution order reverses and normal phase type migration is obtained. Moreover, the elution window is nearly infinite. Efficiencies are very high and reproducibilities in absolute migration times are acceptable (%RSD 〈 5). The influence of a series of alcohol modifiers was investigated.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 161
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 597-604 
    ISSN: 0935-6304
    Schlagwort(e): high temperature gas chromatography ; atomic emission detection ; microwave induced plasma ; compound independent calibration ; non-ionic surfactants ; alcohol ethoxylates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---High temperature gas chromatography (HT-GC) coupled to atomic emission detection (AED) has been applied for the determination of alkyl chain distribution, mole average degree of ethoxylation and weight percent distribution of the corresponding homologues of alcohol ethoxylates without all the actual homologues being available as pure references. Based upon its constant elemental response, the HT-GC-AED system has been evaluated for its applicability to compound independent calibration within the homologous series of the alcohols and alcohol ethoxylates. Discrimination against high molecular weight components by gas chromatography requires conversion to the acetyl or trimethylsilyl derivatives. The latter includes introduction of the hetero atom silicon and thus allows monitoring of the silicon trace. Thus selectivity will be enhanced by excluding detection of compounds which do not react with the derivatization reagent. The method has been validated with the analysis of the technical product Brij 30, consisting of a mixture of alcohol ethoxylates with a vendor-specified mole average degree of ethoxylation of four. The experimental result yields a mole average degree of 4.0 ± 0.1 in the carbon, silicon and oxygen traces.
    Zusätzliches Material: 12 Ill.
    Materialart: Digitale Medien
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  • 162
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 608-612 
    ISSN: 0935-6304
    Schlagwort(e): propolis ; profiling ; CZE ; MEKC ; flavonoids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The usefulness of capillary electrophoresis (CE) with diode array detection for the profiling of Propolis, a hive product, is investigated. Water extracts of Propolis were analyzed with both capillary zone electrophoresis (CZE) at pH 7.0 and 9.3, and micellar electrokinetic chromatography (MEKC) with sodium dodecyl sulfate at pH 9.3. Characteristic profiles were obtained and several organic acids and preservatives could be identified by means of library comparison of the recorded UV spectra combined with addition of reference compounds to the extracts. The selectivity of the CZE and MEKC system differed considerably but the information obtained with both methods was similar. The dry residues of the water extraction were extracted with ethanol-water (70 : 30, v/v) and analyzed with the MEKC system to enable the separation of the more hydrophobic constituents of the Propolis samples. Complex profiles containing various well separated peaks were obtained allowing the identification of some interesting flavonoids. On the basis of the recorded CZE and MEKC profiles, the Propolis samples could be divided into two clearly different groups which are probably from a different origin.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 163
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 625-627 
    ISSN: 0935-6304
    Schlagwort(e): End-closure ; end-seal ; static coating ; glass and fused silica capillaries ; press-fit cap ; polyethylene closure ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 164
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 633-639 
    ISSN: 0935-6304
    Schlagwort(e): capillary gas chromatography ; microplasma mass spectrometry ; radio frequency plasma ; element-selective detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Simultaneous element-selective detection of the halogens and carbon was accomplished with capillary gas chromatography coupled with microplasma mass spectrometry. The microplasma ion source was a radio frequency plasma contained inside the last 4-5 cm of the 0.32 mm i.d. fused silica capillary column. The ion source was located inside the high vacuum housing of the MS, and only the GC carrier gas (2.3 mL min-1 of helium) was used for plasma generation. Atomic ions were detected in the positive mode. Detection limits were in the low picogram area, and the selectivity to carbon ranged from 8×102 for fluorine to higher than 104 for the other halogens. By introduction of both hydrogen and oxygen as reagent gases, peak tailing was avoided by suppression of analyte reactions with the silica walls of the ion source. Special attention was given to the fluorine-selective detection due to an interfering background species at m/z 19, assumed to be H3O+ originating from the reagent gases. The background signal was minimized by careful control of the power level.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 165
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 554-560 
    ISSN: 0935-6304
    Schlagwort(e): LC stationary phases ; octadecyl and octylsilica characterization ; cyclodextrins ; partially methylated cyclodextrins ; heptakis(2,6-di-O-methyl)-β-CD ; evaporative light scattering detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In order to establish guidelines to help the analyst in the choice of the most suitable octadecyl or octyl bonded phase for the LC analysis of a given partially methylated β-CD sample, analyses of four commercially available dimethyl-β-cyclodextrins (DM-β-CDs) have been carried out on nine octyl (C8) or octadecyl (C18) silica bonded or polymeric bonded phases which differ significantly in their hydrophilic and hydrophobic properties. Chromatograms show that the nature of the packing materials has considerable influence on the resolution of complex mixtures composed of closely related compounds such as partially methylated β-CDs. Among various kinds of C8 and C18 bonded phases, silica based and monomeric phases which present both reinforced hydrophobic and polar interactions showed the best performance. Whatever the complexity of the commercial DM-β-CD, the richest chromatographic fingerprints, which best depict the complexity of the mixture, are obtained with Nucleosil 50-5-C8 column. For the simplest mixtures, Nucleosil 50-5-C8 column with acetonitrile-water (34:66) as mobile phase is the most suitable chromatographic system and leads to the best resolution between heptakis (2,6-di-O-methyl)-β-CD and hexakis (2,6-di-O-methyl)-mono(2,3,6-tri-O-methyl)-β-CD (14 OCH3 and 15 OCH3). This chromatographic system might enable an LC-MS coupling for direct identification of the different components in the mixture as well as control of batch to batch variations.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 166
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 565-568 
    ISSN: 0935-6304
    Schlagwort(e): capillary gas chromatography ; precalculation of retention indices ; boiling points ; two- and multidimensional taxonomic groups of organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---It was shown that reciprocally unambiguous conformity between GC retention indices (at least for the commonly used standard nonpolar polydimethylsiloxane liquid phases) and boiling points of organic compounds is typical not only within one-dimensional taxonomic groups (homologous series and/or groups of congeners), but also within two- and multidimensional taxonomic groups (with simultaneous variations of some structural fragments). In all cases, this conformity is described by three-parameter non-linear equations log RI = a log Tb + b (n1 + Σ ki ni) + c, where n1 is the serial number of homologue within corresponding series and ni is the number of other structural fragments in the molecules. The coefficients ki in this equation reflect the relative alterations of molecular polarizabilities and may be estimated as ratios of refractions ki = RD(X)/RD(CH2), where X are variable structural fragments within a group of congeners, RD(CH2) = 4.647 cm3mol-1. The approach under discussion permits precalculation of the retention indices of any organic compounds with known boiling points. The precision of proposed method of RI precalculation is comparable with the contemporary level of interlaboratory reproducibility of experimental RI determination with standard nonpolar liquid phases (5-10 i.u.).
    Zusätzliches Material: 1 Tab.
    Materialart: Digitale Medien
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  • 167
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 583-586 
    ISSN: 0935-6304
    Schlagwort(e): Fast gas chromatography ; narrow-bore columns ; flash-2D-GC ; dedicated fast GC instrumentation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Savings in analysis time in capillary GC have always been an important issue for chromatographers since the introduction of capillary columns by Golay in 1958. In laboratories where gas chromatographic techniques are routinely applied as an analytical technique, every reduction of analysis time, without significant loss of resolution, can be translated into a higher sample throughput and hence reduce the laboratory operating costs. In this contribution, three different approaches for obtaining fast GC separations are investigated. First, a narrow-bore column is used under conventional GC operating conditions. Secondly, the same narrow-bore column is used under typical fast GC conditions. Here, a high oven temperature programming rate is used. The third approach uses a recent new development in GC instrumentation: Flash-2D-GC. Here the column is placed inside a metal tube, which is resistively heated. With this system, a temperature programming rate of 100°/s is possible. The results obtained with each of these three approaches are compared with results obtained on a column with conventional dimensions. This comparison takes retention times as well as plate numbers and resolution into consideration.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 168
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 592-596 
    ISSN: 0935-6304
    Schlagwort(e): capillary gas chromatography ; new chiral selectors anchored to polysiloxane ; t-leucine derivatives ; immobilization ; radical-induced cross-linking ; low racemization of the phases ; high enantioselectivity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---New chiral polysiloxanes have been prepared as stationary phases for gas chromatography, with (S)-(-)-t-leucine-t-butylamide, (S)-(-)-t-leucine-(S)-(-)-1-phenylethylamide, (S)-(-)-t-leucine-(S)-(-)-1-(α-naphthyl)ethylamide, (S)-(-)-t-leucine-(R)-( + )-1-phenylethylamide, and (S)-(-)-t-leucine-(R)-( + )-1-(α-naphthyl)ethylamide as selectors. Immobilization is achieved by radical-induced cross-linking with 1,3,5,7-tetravinyl-1,3,5,7-tetramethylcyclotetrasiloxane (V4) and dicumyl peroxide (DCUP) as cross-linking reagents and cured at 170°C. Under these conditions, racemization of (S)-(-)-t-leucine is less than 4.5% (R) for 1 h curing, while for polysiloxanes with the conventional (S)-(-)-valine selectors about 20% of R-enantiomers are formed by racemization. In the presence of 5% (w/w) V4 and 6% of DCUP with regard to the phases, 70-80% immobilization is achieved; without V4, the degree of immobilization is about 50% for both the (S)-(-)-t-leucine and (S)-(-)-valine selectors. As the size of the amide moieties of the selectors increases from t-butyl to 1-(α-naphthyl)ethyl, the degree of immobilization decreases. If the curing time is prolonged to 2 h, the extent of racemization increases. The selectivity factors achieved for amino acid enantiomers and similar pharmaceuticals are generally higher than those obtained with the corresponding non-immobilized Chirasil-Val phases.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 169
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 620-622 
    ISSN: 0935-6304
    Schlagwort(e): Multidimensional gas chromatography ; comprehensive two-dimensional gas chromatography ; kerosene analysis ; cryogenic modulation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 170
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 617-619 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrochromatography ; cellulose acetate fiber ; microcolumn liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 171
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 613-616 
    ISSN: 0935-6304
    Schlagwort(e): Micro LC ; FID detection ; superheated water ; alcohols ; aldehydes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In the current study, an HPLC-FID system using superheated water as the eluent is constructed and further improved. Signal stability during temperature programmed operation was improved by using separate thermostatting of the 50 μm capillary restrictor. Operating the restrictor at 75°C prevented the superheated water from sputtering in the restrictor. Conventional octadecyl-modified silica, thermostable polymeric reversed phase and carbon type HPLC columns were used. The feasibility of the system is demonstrated by the analysis of a variety of compounds such as alcohols and aldehydes. It is shown that increased temperatures decrease elution times and, in addition to this, frequently improve peak shapes and column efficiencies. The separation of lower aldehydes is performed at 175°C with a detection limit in the low μg/ml range. The possibility of temperature programming is demonstrated for the separation of a range of alcohols. Furthermore, it is shown that temperature programming can be used for sample enrichment. Large volume injection with low temperature enrichment resulted in good peak shapes and a significant improvement of the detection limit. In this way, detection limits of 0.2 μg/ml (ppm) could be obtained for the aldehydes studied. Finally, the possibilities of using mobile phase additives as, e.g., buffers were briefly examined.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 172
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 623-624 
    ISSN: 0935-6304
    Schlagwort(e): Sulfur compounds ; waste paper ; chemiluminescence detector ; food packaging ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Tab.
    Materialart: Digitale Medien
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  • 173
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 640-644 
    ISSN: 0935-6304
    Schlagwort(e): chiral separation ; uncharged and charged cyclodextrin ; borate complexation ; capillary electrophoresis ; propranolol and its metabolites ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A buffer system of borate with charged (carboxymethyl-β-CD) and uncharged (β-CD) cyclodextrins (CDs) was employed in the chiral resolution and separation of propranolol and its selected major metabolites. By appropriate choice of buffer and additive conditions, chiral resolution of all of the compounds studied was achieved in a single analysis, where near baseline resolution was found for the difficult to resolve propranolol-glycol (Pr-glycol). This has not been observed in previous studies of propranolol and its metabolites.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 174
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 645-648 
    ISSN: 0935-6304
    Schlagwort(e): gas chromatography (GC) ; nitrogen-phosphorus detection (NPD) ; sorptive extraction/thermal desorption (SE/TD) ; amines ; in-situ derivatization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The use of sorptive extraction/thermal desorption (SE/TD) for the enrichment of amines from aqueous samples was investigated. The amines were derivatized in situ in the water sample by pentafluorobenzoyl chloride and subsequently enriched onto the SE cartridge. Two SE/TD cartridges were used, a commercially available polydimethylsiloxane (PDMS) packed cartridge and a similar cartridge prepared with newly synthesized poly(butyl acrylate) (PBA). Blank profiles of PBA were not as good as those obtained from the PDMS phase. A complex chromatogram was obtained using mass spectrometric detection. Fortunately, the use of a nitrogen-phosphorus detector (NPD) resulted in clean blanks. The PBA phase showed superior performance for the enrichment of the polar amine derivatives from water samples compared to the PDMS material. Using a CGC-NPD set-up and only 1 mL samples, detection limits are in the sub-ppb range.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 175
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 661-664 
    ISSN: 0935-6304
    Schlagwort(e): SPME ; AED ; metazachlor ; pesticides ; waste water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 176
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 658-660 
    ISSN: 0935-6304
    Schlagwort(e): 1,3-Dioxolanes ; acetals ; ketals ; coffee-like flavorings ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---This paper concerns a number of commercially available coffee-like flavoring preparations, identifying certain dioxolane structures of particular interest. The research was carried out by GC/MS, and spectral characterization was performed of the compounds in question, and especially of the acetals and ketals produced from compounds with carbonyl functions and 1,2-propylene glycol. Some determinations by means of chiral gas chromatography and by Isotope Ratio Mass Spectrometry (IRMS) have been useful in improving the analytical characterization of certain dioxolanes.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 177
    ISSN: 0935-6304
    Schlagwort(e): PAHs ; on-line SPE ; disk extraction ; RPLC ; water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 178
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 11-17 
    ISSN: 0935-6304
    Schlagwort(e): Acridine-modified HPLC stationary phases ; ligand mobility ; fluorescence spectroscopy ; time-resolved fluorescence anisotropy ; solid state NMR spectroscopy ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Ligand mobility of silica-based HPLC stationary phases modified by various surface coverages of acridine-9-carboxy(N-aminoethylaminopropyl)amide ligands was investigated by fluorescence spectroscopy, time-resolved fluorescence anisotropy measurements, as well as solid-state 13C-CP/MAS- and 1H-MAS-NMR spectroscopy. Rotational correlation times, τR, of the bound acridine fluorophore obtained from fluorescence anisotropy measurements are significantly longer in the bound phase, than in solution. Also, in time-resolved experiments anisotropies do not decay to zero. These results are interpreted in terms of wobble-in-cone ligand motion. The mobility of the fluorophore in the presence of liquid phase correlates strongly with the solubility of the model compound acridine-9-carboxy-n-butylamide in the same solvent. In the good solvent acetonitrile τR = 3.2 ns is found, whereas in methanol, τR 〉 80 ns is obtained. NMR measurements of the dry phase yield large linewidths, cross polarization constants, TCH, and spin-lattice relaxation times, T1ρH, shifting around the minimum in the correlation time curve. Both fluorescence and NMR data indicate medium to low ligand mobility. No difference in the mobilities of alkyl spacer and aromatic group is observed, probably due to the rigidity of the amide group.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 179
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 18-24 
    ISSN: 0935-6304
    Schlagwort(e): Reversed-phase HPLC ; capillary electrophoresis ; MALDI-MS ; whey proteins ; multiple peaks ; bovine serum albumin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Elution of a commercial sample of bovine serum albumin (BSA) in a reversed-phase (RP) HPLC system at room temperature gives a distorted peak. If a shallow gradient is used during elution a split peak is observed. The nature of the several parts of this multiple peak is studied using sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE), size-exclusion chromatography (SEC), amino acid analysis, re-elution in RP-HPLC of collected fractions, capillary electrophoresis (CE), and matrix assisted laser desorption ionization-mass spectrometry (MALDI-MS). This study demonstrates that the split peak of BSA observed in these chromatographic conditions is due to the monomer, dimer and other aggregates existing in the commercial sample of the BSA used. Moreover, it is proved that typical RP-chromatographic conditions do not cause aggregation of BSA.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 180
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 59-62 
    ISSN: 0935-6304
    Schlagwort(e): capillary electrophoresis ; mass spectrometry ; MALDI ; CE-MALDI ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 181
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 55-58 
    ISSN: 0935-6304
    Schlagwort(e): liquid chromatography-mass spectrometry ; electrospray ionization ; haloacetic acids ; trace analysis of environmental water samples ; waste water samples ; river water samples ; seawater samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Negative ionization electrospray liquid chromatography mass spectrometry was developed for the simultaneous determination of all nine haloacetic acids containing bromine and chlorine. Haloacetic acids were separated on a crosslinked polystyrene resin column using 3% acetic acid dissolved in acetonitrile:water (20:80) as mobile phase. The precision of this method varied from ±2.2 to ±7.1% for nine haloacetic acids. In addition, quantitative results obtained with spiked water samples at three different concentrations are described. The limit of detection of the proposed method using 200 mL of water samples was between 0.003 and 0.070 μg/L. This method was successfully applied to the trace determination of haloacetic acids in waste water, river water, and seawater.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 182
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 63-64 
    ISSN: 0935-6304
    Schlagwort(e): Injection port performance ; comprehensive two-dimensional GC ; GC× ; GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 183
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 65-68 
    ISSN: 0935-6304
    Schlagwort(e): GC-MS ; rain ; roof runoff ; fatty acids ; phenols ; alkanes ; chlorinated compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 184
    ISSN: 0935-6304
    Schlagwort(e): gas chromatography, helium ionization detector (HID) ; formaldehyde ; atmospheric oxygenates ; volatile organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Two different gas chromatographic detectors, the helium ionization detector (HID) and the more commonly used flame ionization detector (FID), were used in parallel to compare their responses to a number of organic compounds. Atmospherically important oxygenated species were analyzed, as well as hydrocarbons and chlorinated and sulfur containing organics. The HID exhibited the better response to all compounds investigated, most notably to formaldehyde and higher oxygenates. A gas chromatographic system was developed to trap and analyze atmospheric organic compounds with HID detection. This required careful choice of the adsorbent material and removal of inorganic components (namely nitrogen and oxygen) before analysis. Real air samples were then taken and analyzed qualitatively for a range of olefinic and aromatic compounds.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 185
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 81-86 
    ISSN: 0935-6304
    Schlagwort(e): Available niacin ; capillary electrophoresis ; total niacin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Available and total niacin content in lentils and faba beans have been analyzed by capillary electrophoresis (CE), and the results compared with those obtained by high performance liquid chromatography (HPLC). Acidic and enzymatic hydrolysis have been carried out for available niacin determination, and an alkaline extraction performed for total niacin. The extracts were subsequently purified using a strong anion exchanger resin. Precise conditions for purification had to be worked out for each one of the two analytical methods (HPLC and CE). The HPLC analysis for available and total niacin was carried out in an ion-pair reverse phase column with UV detection at 261 nm. For the CE separation, the following conditions were employed: a 20 mM sodium tetraborate; 15 mM sodium dodecyl sulfate and 20% isopropyl alcohol solution as separation buffer; 30 kV and 25 or 30°C. Separation was carried out in a 70 cm effective length × 75 μm i.d. fused-silica capillary using on-column UV detection at 254 nm. The results obtained by CE for lentils and faba beans were similar to those obtained by HPLC.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 186
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 94-102 
    ISSN: 0935-6304
    Schlagwort(e): supercritical fluid chromatography ; experimental design optimization ; Diesel fuel ; group-type analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---An optimization procedure is presented for group-type analysis of diesel fuel by supercritical fluid chromatography using packed silica column and a mixed mobile phase. A set of five responses, four values of resolution of a performance mixture and analysis time, was modeled using a Doehlert matrix for experimental design. Optimized experimental conditions for the five responses were obtained from a response surfaces optimization, taking into account various constraints on SF6 content in mobile phase and analysis time. The predicted and experimental resolutions were in good agreement for the different optimized conditions and one of them was selected to for application to a given diesel fuel for comparison with the results obtained by SFC using pure CO2 and by HPLC. The conditions found in this study provide an alternative method for the determination of mono-, di-, and polyaromatic compounds in middle distillates.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 187
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 107-112 
    ISSN: 0935-6304
    Schlagwort(e): Linalool; linalyl acetate ; enantioseparation by enantioselective gas chromatography ; enantiomer distributions in natural products obtained by different extraction processes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The enantiomeric distributions of linalool and linalyl acetate in various natural products are measured by enantioselective gas chromatography on alkyl-substituted cyclodextrins. Different plant cultivars were investigated by four extraction processes: steam distillation, solvent extraction, supercritical fluid extraction, and headspace analysis. Careful attention must be paid to linalool which undergoes partial racemization under certain processing conditions. In most cases, enantiomeric distribution is a powerful tool for authenticity testing.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 188
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 121-123 
    ISSN: 0935-6304
    Schlagwort(e): gas chromatography ; capillary columns ; column efficiency ; column comparison ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The correct meaning of the the term “utilization of the theoretical efficiency” vs. the “coating efficiency” is explained.
    Zusätzliches Material: 1 Tab.
    Materialart: Digitale Medien
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  • 189
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 125-127 
    ISSN: 0935-6304
    Schlagwort(e): multidimensional gas chromatography ; self-made connectors ; effluent splitting ; press fit connectors ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 190
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 133-136 
    ISSN: 0935-6304
    Schlagwort(e): GC ; analysis of vegetable oil ; petroselinic acid ; butyl esters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 191
    ISSN: 0935-6304
    Schlagwort(e): Enantioselective multidimensional capillary gas chromatography (enantio-MDGC) ; stable isotope ratio mass spectrometry (IRMS) ; multidimensional gas chromatography coupled on-line with isotope ratio mass spectrometry (MDGC-IRMS) ; calibration; isotope discrimination ; authenticity control ; authentication of genuine flavor components ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Multidimensional gas chromatography coupled on-line with isotope ratio mass spectrometry (MDGC-IRMS) is presented as a powerful method for origin-specific analysis. Scope and limitations of this sophisticated coupling technique are discussed with regard to accuracy and precision.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 192
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 161-168 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrochromatography ; optimization ; mixture design ; DUP 654 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Capillary Electrochromatography (CEC) offers a rapid, economical, and efficient means for resolving nonionic compounds in the reversed phase mode on octadecylsilane (ODS) columns. A CEC optimization on a Hypersil ODS capillary column was employed to identify a suitable mobile phase for the pressure-driven (reversed phase ODS) separation of the anti-inflammatory 2-phenylmethyl-1-naphthol (DUP 654), and its related substances. The proportions of mobile phase modifiers methanol, acetonitrile, and water as well as pH were employed as variables in a stacked mixture design. Comparable response surface profiles were obtained for the CEC separations at pH 4 and pH 8. However, subtle differences were evident in the quality of separations obtained in the liquid chromatographic (LC) mode when using a specially-prepared column packed with exactly the same stationary phase as used in the CEC experiments. A mapping of the response surface for separations on a commercially available Hypersil ODS LC column revealed obvious differences. The differences indicate that the transfer of ODS based separation methods between CEC and LC involves more than simply transferring the conditions from one mode to the other.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 193
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 175-180 
    ISSN: 0935-6304
    Schlagwort(e): Supercritical Fluid Extraction (SFE) ; supercritical fluid chromatography ; solid trapping ; solvent trapping ; polymeric phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---One way of collecting extracted analytes after a supercritical fluid extraction (SFE) is to pass the depressurized fluid through a trap composed of a solid adsorbent. The influence of the adsorbent nature on the trap efficiency has been studied. First, the retention factors of each compound of a polarity test mix (tetracosane, naphthalene, fluoranthene, acetophenone, N,N-dimethylaniline, 2-naphthol, decanoic acid) have been determined on five high specific area (greater than 800 m2/g) polymeric phases by supercritical fluid chromatography (SFC). The comparison of this values with those obtained on octadecyl silica (ODS) showed that polymeric phases have the greatest retention power. After that, the efficiency of a solid trap filled with the greatest retention power polymeric adsorbent was evaluated by using pure carbon dioxide and 2.5%, 5%, 10%, and 20% methanol-modified carbon dioxide. As expected, this trap permitted a quantitative collection of all the former compounds even when a content as high as 10% of methanol was implemented. A solid trap filled with ODS adsorbent allowed quantitative collection of all the compounds only at a methanol content lower than 2.5%.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 194
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 185-188 
    ISSN: 0935-6304
    Schlagwort(e): Dill ether ; stereoselective synthesis ; dill ether stereoisomers ; enantioselective GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 195
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 197-199 
    ISSN: 0935-6304
    Schlagwort(e): Chiral recognition of 2-pentanol enantiomers ; enantioselective interactions ; capillary gas chromatography ; permethylated-β-cyclodextrin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 196
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 287-290 
    ISSN: 0935-6304
    Schlagwort(e): DNA ; capillary electrophoresis ; sample injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Silver-coated capillaries were used for direct sample injection in multiplexed capillary electrophoresis. The absence of an additional electrode simplifies mechanical alignment, reduces contamination, and decreases the amount of sample needed. Capillaries were coated by a silver paint which is a suspension of silver particles in an organic solvent. To provide electrical contact, the upper part of the capillary and a platinum wire were wound together by a copper wire. Electrical resistance from the platinum wire to the tip of the capillary was small enough (7 ω to 50 ω) to inject large amounts of DNA samples. Electrokinetic injection from eight separate sample vials to eight capillaries was demonstrated for DNA sequencing by multiplexed capillary electrophoresis. Signal-to-noise ratio and resolution were good enough to call up to 350 base pairs.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 197
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 481-490 
    ISSN: 0935-6304
    Schlagwort(e): solid-phase extraction ; estrogens ; urine ; solvation parameter model ; system maps ; gas chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A general model is presented for the prediction of experimental conditions for the isolation of organic compounds from aqueous solution by solid-phase extraction. The solvation parameter model is used to predict the variation of retention as a function of solvent composition from characteristic solute descriptors and combined with a frontal analysis model to adjust the predicted breakthrough volumes to account for the influence of the small number of theoretical plates characteristic of sorbent cartridges. System maps are used to determine breakthrough volumes for sample processing, the composition and volume of wash solvents for matrix simplification, and the composition and volume of eluting solvents. System maps are provided for an octadecylsiloxane-bonded silica sorbent with methanol and acetonitrile as cosolvents with water. These maps are used to calculate the experimental conditions for the isolation of estrogens from urine and the model validated by experimental verification of the model predictions. The proposed approach provides a simple theoretical framework for computer-aided method development in solid-phase extraction.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 198
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 427-434 
    ISSN: 0935-6304
    Schlagwort(e): Linear solvation energy relationship ; retention ; mobile phase ; stationary phase ; additives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Linear solvation energy relationships (LSERs) were used to delineate which specific intermolecular interactions are responsible for changes in retention for a variety of well characterized analytes when acidic and basic additives were used in reversed phase HPLC. The effects of trifluoroacetic acid, triethylamine and a combination of trifluoroacetic acid and triethylamine on the LSERs were compared to those observed in the absence of additives. These effects were examined using four different mobile phase modifiers and five different stationary phases. Trifluoroacetic acid alone and in combination with triethylamine produced LSER regression coefficients nearly identical to those obtained with no additive present in the mobile phase. Triethylamine alone produced different LSER regression coefficients from the other systems unless the mobile phase contained trifluoroethanol as the mobile phase modifier, or the stationary phase consisted of a polymeric support.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 199
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 498-504 
    ISSN: 0935-6304
    Schlagwort(e): Nonaqueous solvents ; capillary electrophoresis ; charge transfer complexation ; argentation ; silver ion ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---This study represents the first application of Ag(I) charge transfer complexation in nonaqueous capillary electrophoresis. This method applies the principles of argentation chromatography to nonaqueous electrophoretic separations and is termed “nonaqueous argentation electrophoresis”. Since the separations are performed in 100% nonaqueous media, the advantages of nonaqueous solvents, such as enhanced solubility and flexibility in selectivity enhancement, compared to an aqueous or mixed hydroorganic solvent, are realized. A variety of compounds were separated. Qualitatively, the separation of eleven sulfonamides in 100% acetonitrile is shown to improve greatly upon the addition of Ag(I). These results also show that nonaqueous argentation electrophoresis provides fast, well-resolved separations of compounds, such as N-containing heterocyclics, that can selectively complex with Ag(I). Migration data and separation selectivities of these compounds by nonaqueous argentation electrophoresis were compared to previous aqueous argentation electrophoresis results. Selectivities were found to be significantly different for the two separation media. Ag(I) complexation provides an effective means of manipulating selectivity in nonaqueous capillary electrophoresis.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 200
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 519-522 
    ISSN: 0935-6304
    Schlagwort(e): Supercritical Fluid Extraction (SFE) ; Micellar Eletrokinetic Capillary Chromatography (MEKC) ; Diuron ; sugar cane ; orange ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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