Gas-liquid chromatography-mass spectrometry of mono- and dithiols as their tert.-butyldimethylsilyl derivatives.
Gas-liquid chromatography-mass spectrometry of mono- and dithiols as their tert.-butyldimethylsilyl derivatives.
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单硫醇和二硫醇及其叔丁基二甲基甲硅烷基衍生物的气相色谱-质谱法。
DOI：
10.1016/s0021-9673(01)93107-3
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发表时间：
1989
期刊：
影响因子：
--
通讯作者：
Mawhinney,TP
中科院分区：
文献类型：
--
作者：
Landrum,DC;Mawhinney,TP
使用气-液色谱和质谱仪与衍生剂一起使用，可以得到稳定的衍生物和一致的裂解模式，从而能够准确地识别各种化合物。在本研究中，N-甲基-N-叔丁基二甲基硅基三氟乙酰胺或N-叔丁基二甲基硅咪唑用于一系列单硫醇和二硫醇的衍生化反应：从乙硫醇到十六硫醇，从1，2-乙二硫醇到1，9-二十二硫醇。当用这种方法分析时，所得到的24个硫醇的叔丁基二甲基硅基衍生物很容易区分。用毛细管气-液色谱实现了每个衍生物的基线完全分离，每个衍生物都产生了一个显著的质量-57[M+自由基点−57]片段。叔丁基二甲基硅基硫醚无色，室温下稳定3个月以上。该方法为分析各种来源的硫醇化合物提供了一种方便的途径。
The use of gas—liquid chromatography and mass spectrometry with derivatizing agents that give stable derivatives and consistent fragmentation patterns allows for accurate identification of a variety of compounds. In this study either N-methyl- N-tert.-butyldimethylsilyltrifluoroacetamide or N-tert.-butyldimethylsilylimidazole were employed to derivatize a range of mono- and dithiols: from ethanethiol to 1-hexadecanethiol and 1,2-ethanedithiol to 1,9-nonanedithiol. When analyzed in this way, the resultingtert.-butyldimethylsilyl derivatives of the 24 thiols tested were readily distinguishable. Complete baseline separation of each derivative by capillary gas—liquid chromatography was achieved, and each produced a prominent mass minus 57[M+radical dot− 57] fragment. Thetert.-butyldimethylsilyl-thioethers were colorless and were stable at room temperature for over 3 months. This method may provide a convenient approach to the analysis of thiol compounds from a wide variety of sources.