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气相色谱-质谱联用同时测定肉类中的合成代谢和分解代谢类固醇激素

Simultaneous determination of anabolic and catabolic steroid hormones in meat by gas chromatography-mass spectrometry.

作者信息

Hartmann S, Steinhart H

机构信息

University of Hamburg, Institute of Biochemistry and Food Chemistry, Germany.

出版信息

J Chromatogr B Biomed Sci Appl. 1997 Dec 19;704(1-2):105-17. doi: 10.1016/s0378-4347(97)00460-x.

Abstract

A rapid and economical method for the determination in meat of androgens, estrogens, progestogens and corticoids, including some precursors and metabolites, has been developed. The extracted steroids are separated in a polar, a neutral, and a phenolic fraction by C8-SPE followed by a liquid-liquid extraction of the phenolates. Each fraction is separately purified by normal-phase SPE. The different steroid fractions can be analysed either together to obtain a comprehensive hormone pattern in one step or separately to enhance detection selectivity and sensitivity. Using a universally applicable silylation of the hydroxyl and keto groups, detection limits of 0.02-0.1 microg/kg are reached by GC-MS (EI) in the selected ion monitoring mode.

摘要

已开发出一种快速且经济的方法,用于测定肉类中的雄激素、雌激素、孕激素和皮质类固醇,包括一些前体和代谢物。通过C8固相萃取(SPE)将提取的类固醇分离为极性、中性和酚类组分,随后对酚盐进行液液萃取。每个组分通过正相SPE分别纯化。不同的类固醇组分可以一起分析以一步获得全面的激素图谱,也可以单独分析以提高检测的选择性和灵敏度。通过对羟基和酮基进行普遍适用的硅烷化处理,在选择离子监测模式下,气相色谱-质谱联用仪(EI)的检测限达到0.02-0.1微克/千克。

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