免疫亲和色谱净化后，采用液相色谱/串联质谱法测定鸡蛋中的常山酮。

Determination of halofuginone in eggs by liquid chromatography/tandem mass spectrometry after cleanup with immunoaffinity chromatography.

作者信息

Mortier L, Daeseleire E, Huet A-C, Delahaut P, Van Peteghem C

机构信息

Ministry of the Flemish Community, Agricultural Research Centre Ghent (CLO), Department of Animal Product Quality and Transformation Technology (DVK), Brusselsesteenweg 370, 9090 Melle, Belgium.

出版信息

Rapid Commun Mass Spectrom. 2004;18(16):1817-20. doi: 10.1002/rcm.1562.

DOI:10.1002/rcm.1562

PMID:15329875

Abstract

A sensitive and very selective high-performance liquid chromatography/tandem mass spectrometric (LC/MS/MS) method for the detection of halofuginone in whole egg has been developed. After deproteinisation with acetonitrile and evaporation of the organic solvent, halofuginone was further isolated by applying immunoaffinity chromatography. The concentrated eluent was injected into the LC/MS/MS system on a C18 column. The precursor ion ([M+H]+) produced by positive electrospray ionisation was selected for fragmentation with argon. Validation parameters such as recovery, linearity and repeatability, decision limit (CCalpha) and detection capability (CCbeta) were determined.

摘要

已开发出一种灵敏且极具选择性的高效液相色谱/串联质谱（LC/MS/MS）方法，用于检测全蛋中的常山酮。用乙腈进行脱蛋白处理并蒸发有机溶剂后，通过免疫亲和色谱法进一步分离常山酮。将浓缩后的洗脱液注入C18柱的LC/MS/MS系统。选择正电喷雾电离产生的前体离子（[M + H]+）用氩气进行裂解。测定了回收率、线性和重复性、决策限（CCα）和检测能力（CCβ）等验证参数。