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使用极性硅氧烷液相通过气相色谱-质谱联用技术鉴定单酰甘油和单烷基甘油。

Identification of monoacyl- and monoalkylglycerols by gas--liquid chromatography--mass spectrometry using polar siloxane liquid phases.

作者信息

Myher J J, Marai L, Kuksis A

出版信息

J Lipid Res. 1974 Nov;15(6):586-92.

PMID:4430882
Abstract

A comparative study was made of the spectra obtained after gas-liquid chromatography-mass spectrometry of the trimethylsilyl ethers of 1- and 2-monoacyl- and monoalkyl-glycerols. The glycerol derivatives were resolved on the basis of positional substitution and the degree of unsaturation on Silar-5CP (a cyanopropylphenylsiloxane) liquid phase, and the peaks were examined in a Varian MAT CH-5 single-focusing mass spectrometer. The 1-monoacyl- and 1-monoalkylglycerols possessed m/e M - 103 and m/e 205, respectively, as unique peaks, while the 2-monoacyl- and 2-monoalkylglycerols contained m/e 218 as the highly favored fragment. These differences were large and consistent enough to serve as a basis for identification and quantitation of the isomers in a mixture. The saturated and unsaturated monoacyl- and monoalkylglycerols differed markedly in the kind and intensity of the base peaks and other major fragments. In view of the effective gas-liquid chromatographic resolution of these compounds, the marked differences in the spectra of the trimethylsilyl ethers of the saturated and unsaturated species provided a distinct advantage for their identification by the gas-liquid chromatography-mass spectrometry system.

摘要

对1-和2-单酰基甘油及单烷基甘油的三甲基硅醚进行气-液色谱-质谱分析后所得的光谱进行了比较研究。甘油衍生物基于在Silar-5CP(氰丙基苯基硅氧烷)液相上的位置取代和不饱和度得以分离,并且在瓦里安MAT CH-5单聚焦质谱仪中对峰进行了检测。1-单酰基甘油和1-单烷基甘油分别具有m/e M - 103和m/e 205作为独特峰,而2-单酰基甘油和2-单烷基甘油含有m/e 218作为高度有利的碎片。这些差异足够大且一致,足以作为鉴定和定量混合物中异构体的基础。饱和与不饱和的单酰基甘油和单烷基甘油在基峰及其他主要碎片的种类和强度上有显著差异。鉴于这些化合物在气-液色谱上的有效分离,饱和和不饱和物种的三甲基硅醚光谱中的显著差异为通过气-液色谱-质谱系统对其进行鉴定提供了明显优势。

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