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采用液相色谱-串联质谱法对肌肉中的类固醇进行确证分析。

Confirmatory analysis of steroids in muscle using liquid chromatography-tandem mass spectrometry.

机构信息

National Food Institute (DTU-FOOD), DK-2860 Søborg, Denmark.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2011 Apr;28(4):428-37. doi: 10.1080/19440049.2010.549153. Epub 2011 Feb 15.

Abstract

A method is described for screening and confirmation of synthetic and endogenous steroids in muscle tissue. The method is sensitive, selective, and rapid and the consumption of organic solvents is low, compared to previously published methods. The procedure involves hydrolysis, defattening with heptane and final clean up with SPE using C(18) cartridge. After filtration, the analytes are analysed by LC/MS/MS and quantification is performed using deuterated internal standards. Decision limits (CCα) varied from 0.02 to 0.33 µg kg(-1) and the detection capabilities (CCβ) were <0.50 µg kg(-1). The mean within-laboratory reproducibility ranged 5-22% (%RSD(IR)). Endogenous steroids (e.g. testosterone, epitestosterone and androstenedione) have been included in the method, to provide an insight into their levels, as the presence of these steroids was detected several times during analysis of imported meat.

摘要

一种用于筛选和确认肌肉组织中合成和内源性甾体的方法。与之前发表的方法相比,该方法具有灵敏度高、选择性好、速度快且有机溶剂消耗低的特点。该方法包括水解、正己烷脱脂,最后用 C(18)小柱固相萃取净化。过滤后,采用 LC/MS/MS 分析分析物,并使用氘代内标进行定量。决策限(CCα)为 0.02 至 0.33 µg kg(-1),检测能力(CCβ)<0.50 µg kg(-1)。实验室内部重现性平均值为 5-22%(%RSD(IR))。内源性甾体(如睾酮、表睾酮和雄烯二酮)已包含在该方法中,以了解其水平,因为在分析进口肉时多次检测到这些甾体的存在。

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