液相色谱串接质谱测定马饲料中的三种生物碱  

Determination of Alkaloid in Horse Feed using Liquid Chromatography-tandem Mass Spectrometry

作　　者：高照[1,2] 张亦农[1] 

机构地区：[1]国家体育总局反兴奋剂中心,北京1000292 [2]北京体育大学

出　　处：《中国运动医学杂志》2011年第11期1032-1036,1031,共6页Chinese Journal of Sports Medicine

摘　　要：本文建立了采用高效液相色谱串接质谱（LC-MS/MS）同时快速筛查和定量测定马复合饲料中三种天然痕量生物碱（吗啡、可待因、罂粟碱）的方法。样品经充分粉碎后用1 mmol/L HClO4溶液提取,并通过混合型固相萃取进行净化。采用ZORBAX Eclipse Plus-C18（150 mmL×2.1mm ID,3.5μm）色谱柱以含0.4%甲酸的水溶液和乙腈作为流动相进行梯度洗脱,正离子多反应监测（MRM）模式下进行检测。吗啡的检出限为0.50 ng/g,定量限为1.0 ng/g;可待因的检出限为0.75 ng/g,定量限为1.5 ng/g;罂粟碱的检出限为0.20 ng/g,定量限为0.50 ng/g。三种药物空白饲料高、中、低添加浓度水平下的回收率在77.4~97.8%之间,日内、日间精密度分别不高于6.2%和7.1%,实验结果表明本方法有较好的灵敏度和精密度,可以满足马饲料中该类药物的常规检测分析。The aim of this study was to establish a liquid chromatography–tandem mass spectrometry（LC–MS/MS） method for the fast detection and quantification of morphine,codeine,papaverine（papaveris residues） in horse feeds for the purpose of avoiding contamination of doping from external sources to the racing horses.Feed samples were firstly deproteinated and extracted with 10 ml 1mmol/L HClO4 and then purified by a mix-mode solid-phase extraction（SPE）.The separation was performed on a ZORBAX Eclipse Plus-C18（150 mm L×2.1 mm ID,3.5 μm） column with 0.4% formic acid solution and acetonitrile as mobile phases and the extracts were analysed by LC–MS/MS in positive electro-spray ionization（＋ESI） mode with multiple reaction monitoring（MRM）.The limits of detection and quantification of the drugs were in the range of 0.20-0.75 ng/g and 0.50-1.5 ng/g,respectively.The recoveries of all analytes spiked in blank samples at three levels were between 77.4%~97.8% and the intra-day and inter-day relative standard deviations（RSD） were less than 6.2% and 7.1%.The results validated that this method with good reproducibility and sensitivity could be applied in screening and confirmation of the drugs in routine analysis.

关 键 词：液相色谱串联质谱 马饲料 阿片生物碱 快速筛查与测定 

分 类 号：S821.5[农业科学—畜牧学]