气相色谱法测定氨基酸的氮选择检测法

W Büser, H F Erbersdobler
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引用次数: 0

摘要

用热离子氮磷检测器测定了氨基酸的七氟丁基异丁基酯衍生物。检测器的线性度(超过50年),允许测定高于0.3 pMol和110 nMol,无需进一步稀释。由于检测器的特异性,在水解前不需要对样品进行分馏或其他预处理。当比较填充柱和毛细管柱上的分离时,氨基酸衍生物的分离范围从一般到优异。然而,在毛细管分析仪上,只能进行几次运行,因为它在足够长的时间内不可用。单碱性氨基酸的测定重现性较高,变异系数< 3,精氨酸、组氨酸、胱氨酸和少量组分的测定重现性稍差。组氨酸需要通过水解产物与乙酸酐的共注射进行柱上酰化。色氨酸、半胱氨酸和蛋氨酸砜等氨基酸至今尚未被研究。与其他分析方法相比,该程序的缺点是相当复杂的衍生化,到目前为止,还不容易自动化。最后,通过对13个热处理(罐装)食品样品进行8次检测,验证了该方法的实用性。
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[Gas chromatographic determination of amino acids with nitrogen-selective detection].

Heptafluorobutyryl isobutyl ester derivatives of amino acids were determined, using the thermionic nitrogen-phosphorus detector. The linearity of the detector (more than 5 decades), allows determinations above 0.3 pMol and 110 nMol, without the need for further dilution. Due to the specificity of the detector, no fractionation or other pretreatment of the samples prior to hydrolysis were necessary. The separation of the amino acid derivatives ranges from fair to excellent when comparing separations on packed columns with those on capillary columns. On the capillary analyser, however, only a few runs could be performed, since it was not available for a long enough period of time. The reproducibility of the determination was high in the monobasic amino acids, with a coefficient of variation (c.v.) of less than 3, but somewhat worse in arginine, histidine, cystine and minor components. Histidine needs an on-column acylation by the co-injection of the hydrolysate with acetic anhydride. The amino acids tryptophan, cysteic acid and methionine sulphone have not been investigated until now. A disadvantage of the procedure compared with other analytical methods is the rather complicated derivatisation, which until now, has not been easily automated. Finally, the practicability of the method is demonstrated by the results of eightfold determinations in 13 heat-treated (canned) food samples.

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[Food irradiation]. [International Journal of Food Research and Technology]. [Food research and technology]. [International Journal of Food Research and Technology]. [International Journal of Food Research and Technology].
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