液相色谱-串联质谱法测定柏子仁中黄曲霉毒素残留量

目的建立检测柏子仁中黄曲霉毒素B1,B2,G1,G2残留量的液相色谱-串联三重四极杆质谱法。方法将样品提取液经免疫亲和柱净化,甲醇洗脱,以甲醇/乙腈-0.1 mmol乙酸铵为流动相,经反相色谱柱Agilent Zorbax Extend-C18柱(250 mm×4.6 mm,5μm),用电喷雾正离子二级离子监测扫描模式(MRM)检测。结果黄曲霉毒素G2和B2质量浓度在0.03～3.2 ng/mL范围内、黄曲霉毒素B1和G1在0.1～10 ng/mL范围内与峰面积积分值线性关系良好。检测限(LOD)为0.1 ng/mL,定量限(LOQ)为0.2 ng/mL。3个质量浓度(0.25,1.0,5.0 ng/mL)的加标平均回收率为84.1%～96.8%,RSD为7.7%～13.4%。结论所用方法专属性强、灵敏度高、简便快速、结果准确,可定性定量测定柏子仁中残留的黄曲霉毒素。

Detemination of Aflatoxin Residual Quantity in Platycladi Seed by LC-MS/MS

Objective To establish a LC-MS/MS method for determining the residual quantity of aflatoxin B1,B2,G1 and G2 in platycladi seed.Methods The sample extraction solution was purified by immune affinity column and eluted by methanol.The mobile phase was mehanol/acetonitrile-0.1 mmol ammonium acetate.The detection was performed on the reversed phase chromatographic column Aglent Zorbax Extend-C18（250 mm×4.6 mm,5 μm） by ESI-MS positive ion MRM mode.Results Aflatoxin G2 and B2 in the range of 0.03-3.2 ng/mL and aflatoxin B1 and G1 in the range of 0.1-10 ng/mL showed the good linear relationship.The limit of detection（LOD） was 0.1 ng/mL and the limit of quantitation（LOQ） was 0.2 ng/mL.The average recovery rates in three concentrations（0.25,1.0,5.0 ng/mL） were 84.1%-96.8%,RSD 7.7%-13.4%.Conclusion This method is simple and rapid with strong specificity,high sensitivity and accurate results,which can be used to qualitative and quantitative determination of aflatoxin in platycladi seed.