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采用液相色谱-电化学检测法测定食用动物组织中玉米赤霉醇/玉米赤霉烯酮及其代谢物,并通过气相色谱/质谱法进行确证。

Determination of zeranol/zearalenone and their metabolites in edible animal tissue by liquid chromatography with electrochemical detection and confirmation by gas chromatography/mass spectrometry.

作者信息

Roybal J E, Munns R K, Morris W J, Hurlbut J A, Shimoda W

机构信息

Food and Drug Administration, Animal Drug Research Center, Denver Federal Center, CO 80225-0087.

出版信息

J Assoc Off Anal Chem. 1988 Mar-Apr;71(2):263-71.

PMID:2968338
Abstract

A sensitive method is described for the determination and confirmation of zeranol and zearalenone, as well as their isomers and metabolites, in edible animal tissue. The analytes are extracted from tissue with methanol, hydrolyzed enzymatically, cleaned up by acid-base partitioning, determined by liquid chromatography (LC) with electrochemical (EC) detection, and confirmed by gas chromatography/mass spectrometry (GC/MS). LC analysis is performed by isocratic elution with a buffered mobile phase using a Nova-Pak reverse-phase C18 column with amperometric EC detection at +0.90 V. Capillary GC/MS analysis of the trimethylsilyl derivatives provides mass spectral confirmations.

摘要

本文描述了一种灵敏的方法,用于测定和确证食用动物组织中的玉米赤霉醇、玉米赤霉烯酮及其异构体和代谢物。分析物用甲醇从组织中提取,经酶水解,通过酸碱分配进行净化,采用液相色谱(LC)-电化学(EC)检测法进行测定,并通过气相色谱/质谱(GC/MS)进行确证。LC分析采用等度洗脱,使用缓冲流动相,Nova-Pak反相C18柱,在+0.90 V下进行安培EC检测。三甲基硅烷基衍生物的毛细管GC/MS分析提供质谱确证。

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