液相色谱-串联质谱法同时测定动物血浆中21种霉菌毒素或其代谢物残留  

Simultaneous Detection of 21 Kinds of Mycotoxins and Their Metabolites in Animal Plasma with Impurity Adsorption Purification Followed by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王瑞国[1] 苏晓鸥[1] 王培龙[1] 张维[1] 薛岩[2] 李玉[2] 

机构地区：[1]中国农业科学院农业质量标准与检测技术研究所,农业部农产品质量安全研究重点实验室,北京100081 [2]奥特奇生物制品(中国)有限公司,北京100600

出　　处：《分析化学》2017年第2期231-237,共7页Chinese Journal of Analytical Chemistry

基　　金："十二五"农村领域国家科技计划(No.2011BAD26B0405);公益性行业(农业)科研专项经费(No.201203088-01)资助~~

摘　　要：建立了同时检测动物血浆中黄曲霉毒素B1等21种霉菌毒素或其代谢物残留的液相色谱-串联质谱方法。动物血浆样品中加入0.1%甲酸-乙腈溶液、NaCl和无水MgSO_4进行萃取,无水MgSO_4和C_(18),PSA,A-AL对提取液进行脱水净化,经浓缩、复溶和离心后,再进行测定。采用反相C_(18)色谱柱分离,以0.1%甲酸-0.5 mmol/L乙酸铵溶液和0.1%甲酸-甲醇溶液作为流动相进行梯度洗脱,采用电喷雾离子源(ESI)多反应监测离子模式(MRM)进行检测,基质标准曲线外标法进行定量分析,线性范围在0.05~100 ng/mL之间,方法的定量限为0.05~0.5 ng/mL。在高、中、低3个添加浓度水平下,21种霉菌毒素的平均回收率为62.0%~116.4%,相对标准偏差小于19%。A novel method for simultaneous detection of mycotoxins（e.g.,aflatoxin B1） or their metabolic residues in animal plasma with impurity adsorption purification followed ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） was developed.Extraction of mycotoxins and their metabolites from animal plasma sample was performed with 0.1% formic acid-acetonitrile solution after addition of sodium chloride and hydrous magnesium sulfate.The extract was then dehydrated and purified with hydrous magnesium sulfate,C18,primary secondary amine,and alumina-A.3 mL of the supernatant was evaporated and re-dissolved with 0.5 mL of 0.1% formic acid aqueous solution/acetonitrile（70∶30,V/V） for UPLC-MS/MS detection.The analytes were separated by a C（18） column utilizing gradient elution with 0.1%formic acid aqueous solution containing 0.5 mmol of ammonium acetate and 0.1% formic acid-methanol solution,and finally detected by tandem mass spectrometry in positive/negative ESI mode.Identification and quantification were achieved by LC-MS/MS with multi-reaction monitoring（MRM）.Good linearity in response was obtained in the analytes concentration range of 0.05-100 ng/mL with correlation coefficients larger than 0.99.The limits of quantification（S/N=10） were around 0.05-0.5 ng/mL.The recoveries of mycotoxins and their metabolites spiked in blank plasma samples were in the range of 62.0%-116.4%,with relative standard deviations（RSDs） less than 19.0%.

关 键 词：液相色谱-串联质谱 动物血浆 霉菌毒素 残留 

分 类 号：S859.8[农业科学—临床兽医学] O657.63[农业科学—兽医学]