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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 509-512 
    ISSN: 0935-6304
    Keywords: Cholesterol oxidation ; gas chromatography ; oxysterols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The performance of a fused silica column coated with 50% phenyl-/50% dimethyl-polysiloxane, characterized by a high thermal stability, was evaluated for the gas chromatographic determination of cholesterol oxidation products. A silylated mixture of eighteen oxysterol standards (0.1 mg/ml of each compound) was injected into the gas chromatographic system. The temperature was programmed from 230 to 260°C at 2.5°/min and then to 290°C at 1°/min; the injector and detector temperatures were set at 325°C, and the gas linear velocity was 22.8 cm/s. The column gave a fast (15 min) and satisfactory resolution of the main cholesterol oxides. Good separation of the hydroxy from the epoxy derivatives was achieved.The suitability of the method for the determination of oxysterols in food matrices was successfully tested on a saponified lipid extract from egg yolk powder, previously enriched and purified by NH2 solid phase extraction.
    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 22 (1999), S. 149-152 
    ISSN: 0935-6304
    Keywords: Large volume on-column injection ; flooded zone ; capacity of 0.53 mm i. d. precolumns ; solvent trapping ; solvent vapor exit ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---0.53 mm i. d. uncoated precolumns of about 10 m in length followed by a solvent vapor exit have become a standard set-up for large volume on-column injection. It went unnoticed, however, that the introduction of a vapor exit requires two modification of previous working guidelines. First, the capacity of the precolumn to retain sample liquid is increased by a factor of 2.3-3 as a result of the around 100 times higher carrier gas flow rate. Secondly, it must be considered that this gain in retention of liquid is lost again upon closure of the exit: as the gas flow rate is reduced to a few mL/min, the layer of the residual sample liquid expands about 2.3-3 times. Hence, closure should occur late, and a section of the precolumn must be assigned for this secondary spreading.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0935-6304
    Keywords: Large volume on-column injection ; partially concurrent solvent evaporation ; solvent trapping ; retaining precolumn ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 0935-6304
    Keywords: Honey ; Free amino acids ; Capillary gas chromatography ; Heptafluorobutyryl isobutyl esters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The chemical analysis of honey tends to concentrate on factors related to its state of preservation, e.g. HMF, diastase activity, and water content. Although there is no characteristic of honey officially regarded as suitable for certification of its botanical origin, literature is available in which several of the “minor” components of honey, such as flavors, di- and trisaccharides, and free amino acids, have been used to certify the botanical origin of the product.In this paper, six kinds of honey from different botanical sources (acacia, citrus fruit, chestnut-tree, rhododendron, rosemary, and lime-tree) were analyzed by capillary gas chromatography, and the data obtained evaluated statistically to determine whether the amino acid profile could be used to verify the botanical source of the material.The results have shown that the presence of amino acids such as arginine, tryptophan, and cystine is characteristic of a particular kind of honey, and that others, such as proline, asparagine, lysine, and methionine, can be used for discrimination if quantitative data is available about the levels of the compounds present.Evaluation of optimum split ratio for amino acid determination, and problems concerning the derivatization process, are also discussed.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 303-307 
    ISSN: 0935-6304
    Keywords: High resolution gas chromatography ; Unsaponifiable coffee fraction ; Coffee diterpenic alcohols ; Robusta coffee determination ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The unsaponifiable lipid fractions extracted from Arabica and Robusta coffee samples were analyzed by high resolution gas chromatography (HRGC) in a polar column with a thermally stable stationary phase (TAP, Chrompack). Certain characteristic ratios among diterpenic alcohols were found to permit measurement of the amount of Robusta blended with Arabica coffee, given a minimum content of 5-10%. Determination does not appear to be influenced by geographic origin of produce or even by decaffeination.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 827-830 
    ISSN: 0935-6304
    Keywords: HPLC ; Fluorimetric detection ; UV detection ; Proteins of animal origin ; Lysinoalanine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This work suggests an HPLC method for qualitative and quantitative determination of Nε(2-amino-2-carboxyethyl)-L-lysine (LAL). LAL was released from total hydrolysates of various proteins of animal origin and derivatized with dansyl chloride. The performance of two different columns, Spherisorb 3S TG and μ-Bondapack C18, was compared; better resolution and quantitative response were obtained with the former. The mobile phase was a mixture of 0.01 M phosphate buffer (pH 7) and acetonitrile. Linear response and quantitative repeatability were tested for both detectors used (UV-Vis set at 254 nm; fluorimetric set at λex(max) = 360 nm and λem(max) = 525 nm).For LAL standard the minimum detectable amount was 0.05 ng, whereas for LAL in actual samples the amount was 0.5 ng (40 μg/g of analyzed proteins). Good analytical repeatability was obtained, resulting in CV % of 4.7 and 3.8 for UV and fluorimetric detectors, respectively. LAL recovery was determined using both detectors; the values obtained were 94 % (fluorimetric) and 92 % (UV). Greater noise levels were observed with the fluorimetric detector and its higher sensitivity could not, therefore, be fully utilized. The highest amounts of LAL were found in the casein (2816 μg/g) and cooked albumin (615 μg/g) samples.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 378-382 
    ISSN: 0935-6304
    Keywords: Large volume injection ; on-column injection ; flooded zone ; solvent trapping ; temperature measurement on precolumn wall ; water analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Solvent trapping reconcentrates volatile components after injection or on-line transfer of large volumes. When an early vapor exit is used, typically after a 5-10 m × 0.53 mm i.d. uncoated precolumn, the solvent trapping process differs from that described previously. The visual experiments and the conclusions drawn therefrom, as described in a previous paper, are supplemented with chromatographic results. They show that even hexane can be quantitatively analyzed in 250 μl of a pentane solution. Injection of a volume of 250 μl by vaporizer/precolumn solvent splitting was used in the analysis of gasoline in drinking water. Conditions for the transfer of a 1000 μl volume can easily be adjusted through detection of the front end of the flooded zone by a thermocouple mounted on the outer wall of the precolumn.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 355-362 
    ISSN: 0935-6304
    Keywords: Large volume injection ; solvent evaporation ; flooded zone ; solvent trapping ; on-column injection ; water analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Using a specially treated glass capillary, evaporation of the solvent during large volume injection into a precolumn was visually investigated in order to better understand the solvent trapping process. Using an early vapor exit, the process differs from the classical description of solvent trapping. First, there is a substantial pressure drop over the solvent-coated (“flooded”) precolumn, causing evaporation to take place not only at the rear edge, but also within the flooded zone or at its front end (which may result in almost complete loss of volatile solutes). Secondly, the evaporation rate increases as the liquid enters deeper into the precolumn, eventually turning partially concurrent evaporation into a fully concurrent evaporation with massive loss of volatiles. Thirdly, the capacity of the precolumn to retain liquid is substantially higher than observed in systems without early vapor exit
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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