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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 60-63 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Cold silanization ; Medium polarity columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Silane-coupling agents, commonly used for fiberglass reinforced plastics (FRP), were applied for deactivation of silanol sites in glass capillary columns prior to coating with mediumpolarity phases such as Carbowax and Superox. The columns, prepared in a two-stage process in the case of glass (acidic leaching and drying, dynamic cold silanization followed by static coating with the phase) or a one stage process in the case of fused silica, gave the best results when deactivation and hence wettability were induced by glycidoxypropyltrimethoxy silane.
    Additional Material: 3 Ill.
    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. 523-524 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Split injection ; Injection time influence ; PAH ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 558-562 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns, glass ; On-column injection ; Sugars ; Oligosaccharides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sugars were separated gas chromatographically on short apolar glass capillary columns by using cold, on-column injection (OCI) techniques. After silylation, oligomers up to the hexasaccharides could be efficiently separated in resonable retention times. Response factors of silylated sugars were determined as a function of varying sample amounts and concentrations. The optimum injection amount was found to be 1 μl in heptane as solvent.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 19-22 
    ISSN: 0935-6304
    Keywords: Thin layer chromatography, HPTLC ; Anticircular mode ; Cosmetic emulsions ; Jojoba wax ester quantitation ; Triglyceride quantitation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cosmetic creams were analyzed for their content of jojoba wax and shea fat using anticircular HPTLC, a fast, precise, and reliable method. After optimization of the solvent system (petrol ether/diethyl ether) for the separation of jojoba wax and shea fat, the spots were visualized with phosphomolybdic acid by the “dip-in” technique, subsequently heated, and finally recorded by scanning with a densitometer at 546 nm. Results showed that one particular concentration range gives an optimum correlation between calibration curves and sample evaluations.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 838-842 
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography, HPTLC ; Elution characteristics ; Temperature effect ; Solvent polarity effect ; Polar lipids ; Boric acid ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 440-443 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; GC/MS ; Capillary column, fused silica ; EI-MS/CI-MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In order to facilitate the gas chromatographic determination of butyric as well as other short chain fatty acids, triglycerides containing these fatty acids were transbutylated and transpentylated to give FABES (fatty acid butyl esters) and FAPES (fatty acid pentyl esters), respectively. This method allows the molecular weight of the compounds to be increased while their polarity is decreased. Short chain esters elute sufficiently separated from the solvent; due to the decreased polarity, elution of long chain fatty acids is only slightly retarded compared to the corresponding methyl esters. Quantitative evaluation over a large series of injections proved the linearity of correction factors in both cases, FABES and FAPES, with a slight deviation for 16:0 and 18:0, respectively. Structural characterization was performed by GC/MS. It was shown that there are characterstic fragmentations for FABES as well as for FAPES. The El-mass spectra give structural information about the alcohol and acid moieties, the ester molecule and the Cl-spectra indicate the molecular weight. The absence of abundant highly characteristic peaks in the spectra of these esters makes the detection of FABES or FAPES in complex mixtures more difficult than the detection of FAMES with their very characteristic ions at m/z 74 and 87.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography, HPTLC ; Anti-circular development ; On-plate derivatization ; Visible scanning ; Quantitation ; Tryptamides/serotonin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 124-128 
    ISSN: 0935-6304
    Keywords: Chromatography, gas, capillary ; Fatty acids, volatile ; Biological samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method was developed to analyze and quantitate volatile fatty acids such as acetic, propionic, butyric, iso-butyric, valeric, and iso-valeric acid from samples of biological origin. A capillary column system including an automatic on-column injection device as well as a precolumn of larger internal diameter than the analytical column was elaborated for this purpose.In order to obtain well resolved and correctly quantifiable chromatographic peaks it turned out to be essential to work under acidic/aqueous conditions. To achieve a better sample transfer into the chromatographic system an organic solvent had to be used together with the aqueous milieu, thus improving wetting properties of the liquid sample plug introduced into the column. Cold on-column injection was applied in order to avoid discrimination of the various acids due to sample splitting and the automatic technique was chosen in view of the large number of samples from biological extractions which had to be analyzed.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 218-223 
    ISSN: 0935-6304
    Keywords: High performance planar chromatography, HPPLC ; Preparative anticircular chromatography (PACH) ; Sample collection ; Quantification ; Silica Gel (20 × 20 and 10 × 10 cm) plates ; RP-18 (20 × 20 and 10 × 10 cm) plates ; Unsaponifiables from plant lipids ; Fatty acid methyl esters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A preparative anticircular chromatography (PACH) device was constructed to elucidate different applications of separation problems as well as to compare different sample collection techniques in this particular PLC mode. An anticircular PC apparatus had to be established which allowed the utilization of 20 X 20 cm thin-layer plates as well as sampling positioning at any given radius. Typical solvent migration times were 8-12 minutes and ca. 8-10 ml of solvent was needed for an entire 20 cm plate. It was shown that peak broadening effects due to diffusion during long migration could be avoided in the same way as for analytical anticircular PLC on 10 X 10 plates. On the other hand, longer migration distances allow increased resolution, in turn allowing higher sample loads, particularly in the case of trace compound enrichment. A full description of the apparatus is given, including the sampling device.Different sample collection techniques were tried and evaluated, including the through-flow technique by on-line center collection for plate washing as well as classical scraping-off of interesting zones. Further evaluation of the method included quantification and evaluation of consistency by UV/VIS scanning after spot-visualization. Several application examples are given to illustrate the efficiency of the preparative anticircular PLC-system.
    Additional Material: 12 Ill.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 12 (1989), S. 308-315 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Mass spectrometry ; Ion trap detector ; FID detection ; Lipid analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fatty acids, as their methyl esters (FAMES), are routinely analyzed from a wide variety of plant and animal tissues and fluids. Samples have mainly been analyzed to date using capillary GC with FID detection. However, FID detection is non-specific, and open to misinterpretation. This is particularly important in the analysis of minor lipid components from, e.g. organ tissues, plasma and other body fluids, where non-FAMES impurities or contaminants can be present in relatively high amounts. This suggests that even for routine work, a mass spectral detector is necessary for the unambiguous identification-or rather, recognition-of FAMES. The FAMES analyzer we propose consists of three components: an automatic injector; a medium polarity, high-temperature stable capillary column; a mass spectrometric detector, in our case the Finnigan-MAT ion trap detector (ITD 800). Here, on-column injection allowed controlled sample transfer even for low absolute concentrations of lipids, and a column effluent splitter gave simultaneous qualititative and quantitative analysis. For automatic routine analysis, a mass spectral library routine using a tailor-made library of FAMES spectra of the most common naturally occurring fatty acids, plays an essential role. Library comparison parameters used in the standard ITD software usually give “first hit” recognition over a wide sample dynamic range (ca. 2 pg to 〉 200 ng in the best cases). This gives an absolute recognition even of minor lipid components, especially when combined information from mass spectra and GC retention data is used. By analogy with the now well known concept of the Amino Acid Analyzer, we propose the system described as a FAMES Analyzer. Mass spectrometers like the Finnigan MAT ITD 800 are inexpensive, reliable, sensitive, and easy to operate. Unlike the Amino Acid Analyzer, the FAMES Analyzer needs the specific detection offered by mass spectrometry because the number of acids to be analyzed, including isomers, is much greater.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
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