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通过气相色谱/质谱联用技术(GC/MS)增强类固醇的化学衍生化

Enhancement of chemical derivatization of steroids by gas chromatography/mass spectrometry (GC/MS).

作者信息

Bowden John A, Colosi Dominic M, Mora-Montero Diana C, Garrett Timothy J, Yost Richard A

机构信息

Department of Chemistry, University of Florida, PO Box 117200, Gainesville, FL 32611, United States.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Oct 1;877(27):3237-42. doi: 10.1016/j.jchromb.2009.08.005. Epub 2009 Aug 7.

DOI:10.1016/j.jchromb.2009.08.005
PMID:19692297
Abstract

Steroid derivatization was investigated by varying the experimental parameters (reagent, reaction time, and reaction temperature) to determine the optimal conditions for individual steroids, and for larger subsets. Three methods of derivatization enhancement were also investigated: the use of sonication, the use of a microwave heating, and the addition of solvents to the reaction mixture. On a comprehensive level, derivatization using N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA) was most efficient, while the application of solvent addition and microwave heating, in several cases, provided a clear enhancement. In addition, generalized rules for steroid derivatization are described.

摘要

通过改变实验参数(试剂、反应时间和反应温度)来研究类固醇衍生化,以确定单个类固醇以及更大子集的最佳条件。还研究了三种增强衍生化的方法:使用超声处理、使用微波加热以及向反应混合物中添加溶剂。从综合层面来看,使用N-甲基-N-三甲基硅烷基-三氟乙酰胺(MSTFA)进行衍生化最为有效,而在几种情况下,添加溶剂和微波加热的应用能显著增强衍生化效果。此外,还描述了类固醇衍生化的通用规则。

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