通过生物材料中苄酯的气相色谱法同时测定C2 - C22非酯化脂肪酸和其他代谢相关羧酸。
Simultaneous determination of C2-C22 non-esterified fatty acids and other metabolically relevant carboxylic acids in biological material by gas chromatography of their benzyl esters.
作者信息
Schatowitz B, Gercken G
机构信息
Department of Biochemistry, University of Hamburg, F.R.G.
出版信息
J Chromatogr. 1988 Mar 18;425(2):257-68. doi: 10.1016/0378-4347(88)80030-6.
A method for the simultaneous determination of non-esterified short-, medium- and long-chain fatty acids and other types of metabolically relevant carboxylic acids such as hydroxy, keto, aromatic and dicarboxylic acids in biological material by capillary gas chromatography of benzyl ester derivatives is described. Sample preparation avoiding incomplete isolation of carboxylic acids consisted of deproteinization and extraction with ethanol, fixation of carboxylic acids as carboxylates, removal of interfering compounds such as neutral lipids by hexane extraction and amino acids, acyl carnitines and other cations by cation-exchange chromatography, derivatization of keto groups of ketocarboxylic acids into O-methyl oximes and benzyl ester formation by reaction of the potassium carboxylates with benzyl bromide via crown ether catalysis. The sample preparation conditions were investigated, showing the usefulness of this method for quantitative determinations. Chromatograms obtained from human serum, human urine and rat heart ventricle and concentrations of carboxylic acids in these specimens are presented.
描述了一种通过苄酯衍生物的毛细管气相色谱法同时测定生物材料中非酯化的短链、中链和长链脂肪酸以及其他类型与代谢相关的羧酸（如羟基酸、酮酸、芳香酸和二羧酸）的方法。避免羧酸不完全分离的样品制备包括用乙醇进行脱蛋白和萃取、将羧酸固定为羧酸盐、通过己烷萃取去除干扰化合物（如中性脂质）以及通过阳离子交换色谱法去除氨基酸、酰基肉碱和其他阳离子、将酮羧酸的酮基衍生化为O-甲基肟以及通过羧酸钾与苄基溴在冠醚催化下反应形成苄酯。研究了样品制备条件，表明该方法在定量测定方面的实用性。给出了从人血清、人尿液和大鼠心室获得的色谱图以及这些标本中羧酸的浓度。
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