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液相色谱-串联质谱法测定马饲料中的抗凝血类药物

高照 张亦农

质谱学报2011,Vol.32Issue(6):360-366,7.
质谱学报2011,Vol.32Issue(6):360-366,7.

液相色谱-串联质谱法测定马饲料中的抗凝血类药物

Quantification of Anticougulants in Equine Feed Using Liquid Chromatography-Tandem Mass Spectrometry

高照 1张亦农1

作者信息

  • 1. 国家体育总局中国反兴奋剂中心,北京100029
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摘要

Abstract

A fast screening and simultaneous determination method of four Coumarin-type and one indandione anticoagulants in equine feed was established using LC-MS/MS coupled with solid phase extraction. The fragmentation pathways were studied according to the characteristic fragment ions under electrospray ionization. Due to the weak acidity of the drugs, samples were first infiltrated and deproteinized with methanol, then enriched by solid-phase extraction (SPE) using a MCX cartridge after extracted with 0. 02 mol/L NaOH. Detection was performed on a mass spectrometer by negative electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode in five different time segment except for cou-marin with positive mode to achieve simultaneously quantitative analysis of five anticoagulants. The limits of detection are 10 ng/g for dicoumarin and warfarin, 4 ng/g for acenocou-marin and coumarin, 15 ng/g for penidione. Limits of quantitation are as low as 10-40 ng/g and the intra-day and inter-day relative standard deviations (RSD) are less than8. 63%and 10.20%, respectively.

关键词

液相色谱-串联质谱法/抗凝血类药物/马饲料/定量分析

Key words

LC-ESI-MS/MS/ anticoagulants/ equine dopings/quantitative analysis

分类

化学化工

引用本文复制引用

高照,张亦农..液相色谱-串联质谱法测定马饲料中的抗凝血类药物[J].质谱学报,2011,32(6):360-366,7.

质谱学报

OA北大核心CSCDCSTPCD

1004-2997

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