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  • 1
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; Solid-phase microextraction ; Local anaesthetic lidocaine ; Optimisation of extraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Solid-phase microextraction (SPME) has been combined with gas chromatography (GC) and liquid chromatography (LC) for the determination of lidocaine in human urine. A polydimethylsiloxane (PDMS) coated fibre was directly immersed into buffered urine. Extraction conditions such as time, pH, ionic strength, temperature, and agitation were optimised. The extracted lidocaine was thermally desorbed in a split/splitless injector for analysis with a GC-FID system or desorbed with liquid in a specially designed SPME-LC interface for analysis with an LC-UV system. After optimisation the method developed was evaluated and validated. Extraction yields of 22% were obtained in about 45 min. The reproducibility of the method is 〈5% (relative standard deviation). For five-times diluted urine, linear ranges were found from 5–1000 and 25–1000 ng·mL−1 for SPME-GC and SPME-LC, with detection limits of 5 ng·mL−1 for SPME-GC and 25 ng·mL−1 for SPME-LC. SPME can be used as a simple sample pretreatment method for the determination of lidocaine in urine by GC and LC.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 4 (1981), S. 444-447 
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; Reversed-phase ion-pair system ; Biogenic amines and metabolites ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The liquid chromatographic separation of some biogenic amines and their metabolites with a reversed-phase ion-pair system has been optimized. The effects of the nature of the stationary phase, the column temperature, the pH, and the ion-pair reagent concentration of the mobile phase have been investigated. The most striking result is the influence of the column temperature on selectivity.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Retention gap ; LC trace enrichment ; Aqueous samples ; Organic pollutants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trace enrichment for the GC analysis of a series of chlorinated pesticides and polychlorinated biphenyls (PCBs) in aqueous samples has been achieved through a simple on-line technique involving sorption on an LC micro-precolumn followed by direct elution into a gas chromatograph with hexane. A 5-m retention gap coupled to the capillary GC column served as the recipient of a relatively large sample volume (ca. 100 μl) introduced into the GC. Partially concurrent solvent evaporation during sample introduction allowed a large sample capacity. Recoveries of more than 95% were observed for the majority of the compounds studied. Using 1.0 ml aqueous samples, detection limits of less than 1 ppt were found. The applicability of the developed method was demonstrated for a river water sample.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 0935-6304
    Keywords: Coupling LC/GC ; Retention gap ; Polychlorinated biphenyls ; Sediment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Narrow-bore column liquid chromatography coupled on-line with capillary gas chromatography (LC/GC) is used for the determination of polychlorinated biphenyls (PCBs) in sediment via a heart-cutting technique. This method is compared with a method in which two off-line column clean-up steps are used with subsequent analysis by capillary gas chromatography. For the LC/GC analysis the recovery of PCBs was 90-100%. For two sediment samples from the river Meuse the LC/GC and the other, more laborious method showed good agreement.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 12 (1989), S. 793-796 
    ISSN: 0935-6304
    Keywords: Microcolumn liquid chromatography ; Flame photometric detection ; Organophosphorus compounds ; On-line preconcentration ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The potential of an interface for the on-line coupling of microcolumn liquid chromatography (LC)and a flame photometric detector (FPD) has been further investigated. With the micro-LC/FPD system, relatively high-molecular-weight polar compounds such as cyclic adenosine monophosphate, guanosine monophos- phate, glucose monophosphate, fructose monophosphate, and phytic acid were separated and selectively detected. In order to increase the sensitivity, on-line preconcentration with a microprecolumn inserted in the rotorof a Valcovalve has been applied. Preliminary results have shown that an injection volume of at least 500 1-11 water containing organophosphorus acids at a 5-50 ng/rnl concentration level is possible.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 0935-6304
    Keywords: Polar solvents ; Coupled LC-GC ; Partially concurrent solvent evaporation ; Trace enrichment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Coupling column liquid chromatography and gas chromatography on-line is becoming more important in analytical chemistry. Especially when large amounts of polar solvents can be introduced into the gas chromatograph without any problem, the technique will offer new possibilities. With a DPTMDS retention gap, evaporation rates and flooded zones of some solvents have been determined. Two modes of operation using partially concurrent solvent evaporation conditions are discussed: (1) injecting a sample via a loop of an LC valve followed by introduction into the gas chromatograph with an LC pump; (2) trace enrichment on a precolumn followed by on-line desorption with n-propanol into the gas chromatograph. Preliminary results for a splitter system, inserted between the retention gap and the analytical column which allows a considerable increase of the evaporation rate are also presented.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A benzenesulphonic acid-type cation exchanger (pKa 〈 1) is used as trapping-column material in a phase-system switching for the on-line coupling of column liquid chromatography and thermospray mass spectrometry. Phase-system switching is used to remove non-volatile constituents from the mobile phase, so that eluents containing non-volatile buffers and ion-pairing agents can be used without contaminating the mass spectrometer. The total analytical system is optimized using four benzalkonium test compounds (quaternary ammonium compounds). The reversed-phase separation of the test compounds as well as the parameters involved in the sorption on and desorption from the trapping column are studied. Important parameters during sorption are the concentration of the phosphate buffer and the percentage of acetonitrile in the mobile phase. During desorption of the test compounds from the ion-exchanger the percentage of acetonitrile in the desorption eluent and the pH are the most important factors. As an example, the analysis of domiphen in nasal drops is shown.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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  • 8
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Liquid chromatography/thermospray mass spectrometry (LC/TSP MS) has been used for the determination of vitamin D3 and some of its metabolites, i.e. 1α(OH) vitamin D3, 25(OH) vitamin D3, 1α,25(OH)2 vitamin D3 and 24,25(OH)2 vitamin D3, using positive and negative ion detection. Using these two modes positional isomers can be identified. Detection in the negative ion mode was preferred because of the slightly higher sensitivity. The limits of detection, using multiple ion detection, are 50-100 nM (6-12 pmol injected). On-line post-column derivatization based on [4 + 2] cyclo-addition (Diels-Alder reaction) proceeds within 1 min at room temperature. If this step is included in LC/TSP MS, the detection limits of the analytes can be improved 7-70-fold depending on the analyte tested. The best results (detection limits down to 1 nM, i.e. 0.12 pmol injected) are obtained with discharge ionization in the negative ion mode.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 17 (1973), S. 2835-2846 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Experimental data are presented describing the formation of porosity in styrene-divinylbenzene copolymers as a function of the organic components present during the suspension polymerization. The reaction system contains a mixture of diluents such as toluene and hexane, which results in matrices that differ significantly in pore structure from the porous resins so far known. From these data a model of the physical structure is proposed.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 47 (1998), S. 313-345 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Sample pretreatment ; Coupling on-line to capillary GC ; Robotization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Sample pretreatment is often the bottleneck of a tracelevel analytical procedure. In order to increase performance, increasing attention is therefore being devoted to combining sample pretreatment on-line with the separation technique that has to be used. In the present review, a variety of procedures in use today for sample treatment coupled on-line to capillary gas chromatography (GC) is briefly discussed. Special attention is devoted to coupled-column techniques such as SPE-GC and LC-GC (SPE, solid-phase extraction; LC, column liquid chromatography) which are topics of much current interest, also because of their frequent use in so-called hyphenated systems.
    Type of Medium: Electronic Resource
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