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

作　　者：高照[1] 张亦农[1] 

机构地区：[1]国家体育总局中国反兴奋剂中心,北京100029

出　　处：《质谱学报》2011年第6期360-366,共7页Journal of Chinese Mass Spectrometry Society

摘　　要：建立了马复合饲料中双香豆素、香豆素、醋硝香豆素、苄丙酮香豆素、苯茚二酮5种抗凝血类药物的高效液相色谱-串联质谱(HPLC-MS/MS)同时快速筛查和定量测定方法,并对该类化合物在电喷雾电离条件下的主要碎裂途径进行了探讨。方法以甲醇和0.02mol/L NaOH溶液作为提取溶剂,饲料样品经提取后利用混合型阳离子交换固相萃取进行净化,采用正负切换多反应监测(MRM)模式对试样中5种香豆素类及茚二酮类抗凝血剂进行定性与定量分析。苯茚二酮的检出限为15ng/g,香豆素和醋硝香豆素的检出限为4ng/g,华法林和双香豆素的检出限为10ng/g。5种药物的定量限在10～40ng/g之间,日内日间精密度分别不高于8.63%和10.20%。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 coomarin with positive mode to achieve simultaneously quantitative analysis of five ant,coago lants. The limits of detection are 10 ng/g for dicoumarin and warfarin, 4 ng/g for acenoco marin and coumarin, 15 ng/g for penidione. Limits of quantitation are as low as 10 -10ng/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 

分 类 号：O657.63[理学—分析化学]