液相色谱-串联质谱法测定宠物食品中赭曲霉毒素A和B  

Determination of Ochratoxin A and Ochratoxin B in Pet Food by Liquid Chromatograpy-Tandem Mass Spectrometry

作　　者：陈祥准 李舟 黄芙珍 朱振瓯 刘滨 韩超 

机构地区：[1]温州出入境检验检疫局,浙江温州325027

出　　处：《分析科学学报》2017年第2期267-270,共4页Journal of Analytical Science

基　　金：温州市科技局科技项目(No.2013G0007)

摘　　要：建立了同时测定宠物食品中赭曲霉毒素A和B的液相色谱-串联质谱分析方法。样品经乙腈/水(1∶1,V/V)提取,HLB固相萃取柱净化。采用Agilent ZOBRAX C_(18)柱(150×2.1mm,5μm)分离,以0.1%甲酸水溶液-乙腈作为流动相,梯度洗脱。目标化合物在多反应监测模式(MRM)下进行检测,外标法定量。在优化的条件下,赭曲霉毒素A和B在0.1~10.0ng·mL^(-1)范围内呈良好的线性关系,相关系数均不低于0.9993,方法定量限分别为0.1μg·kg^(-1)和0.05μg·kg^(-1)。方法平均回收率为78.3%~107.5%,相对标准偏差不大于9.5%。该方法前处理简单、选择性好、灵敏度高,可用于宠物食品中赭曲霉毒素A和B的测定。A method of liquid chromatography-tandem mass spectrometry（LC-MS/MS）was used for the simultaneous determination of Ochratoxin A and Ochratoxin B in pet food sample.Samples were extracted with acetonitrile/water（1∶1,V/V）and cleaned up with HLB solid phase extraction.A gradient elution program was applied with the mobile phase of 0.1% formic acid solution and acetonitrile.The analyte was determined in multiple reaction monitoring transitions（MRMs）mode and the quantification was performed by the external standard method.The results indicated that the calibration curves for Ochratoxin A and Ochratoxin B was linear in the range of 0.1-10.0 ng·mL-1,with correlation coefficients more than 0.9993,and the limits of quantification（LOQs）were 0.1μg·kg-1 and 0.05μg·kg-1.The average recoveries ranged from 78.3% to 107.5% with the RSDs less than 9.5%.This method is simple,good selectivity and sensitive,and is suitable for the determination of Ochratoxin A and Ochratoxin B in pet food.

关 键 词：宠物食品 赭曲霉毒素A 赭曲霉毒素B 液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]