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.
出处
《分析科学学报》
CSCD
北大核心
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)
