QUANTITATION OF 2-KETOACIDS IN BIOLOGICAL-FLUIDS BY GAS-CHROMATOGRAPHY CHEMICAL IONIZATION MASS-SPECTROMETRY OF 0-TRIMETHYLSILYL-QUINOXALINOL DERIVATIVES
QUANTITATION OF 2-KETOACIDS IN BIOLOGICAL-FLUIDS BY GAS-CHROMATOGRAPHY CHEMICAL IONIZATION MASS-SPECTROMETRY OF 0-TRIMETHYLSILYL-QUINOXALINOL DERIVATIVES
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DOI：
10.1002/bms.1200080406
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发表时间：
1981-01-01
期刊：
影响因子：
--
通讯作者：
CARTIER, P
中科院分区：
文献类型：
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作者：
ROCCHICCIOLI, F;LEROUX, JP;CARTIER, P
建立了一种灵敏度高、专属性强的三甲基硅基喹恶啉类化合物气相色谱-化学电离-质谱法测定各种生物体液中2-酮酸的方法。2-酮酸和2-酮戊酸在酸性介质中经邻苯二胺衍生化和萃取后，在毛细管柱上硅烷化，以氨气为反应气体，通过监测相应质子化分子离子的/Z值自动测定其浓度。每种2-酮酸的检出限均小于50 ng/−。尿样和血浆中2-酮酸的回收率在97%~104%之间。对干扰物质遇到的问题进行了测试和讨论。这种方法已经成功地应用于以脂肪2-酮酸积聚为特征的各种代谢紊乱。讨论了支链2-酮酸与其他化合物，特别是丙酮酸的代谢关系。
A very sensitive and specific method of 2‐ketoacid determination in various biological fluids using gas chromatography chemical ionization mass spectrometry ofO‐trimethylsilyl‐quinoxalinol derivatives is described. After derivatization witho‐phenylenediamine in acidic medium and extraction, the 2‐ketoacids, and the 2‐ketovaleric acid used as internal standard, are silylated and resolved on a capillary column and their concentrations automatically determined by monitoring them/zvalues corresponding to their respective protonated molecular ions, using ammonia as reactant gas. The detection limit is below 50 ng ml−1of each 2‐ketoacid. The recoveries of 2‐ketoacids from urine and plasma were between 97 and 104%. Problems encountered with interfering substances were tested for and discussed. This method has been applied successfully to various metabolic disorders characterized by an accumulation of aliphatic 2‐ketoacids. The metabolic interrelationship of branched chain 2‐ketoacids and other compounds, especially pyruvate, is discussed.