HPLC-MS/MS法测定大米中5种农药残留

Determination of 5 Pesticide Residues in Rice by HPLC-MS/MS

建立高效液相色谱-串联质谱法(HPLC-MS/MS)测定大米中禾草敌、稻瘟灵、敌瘟磷、丙草胺、生物苄呋菊酯5种农药残留的方法。样品经乙腈提取,分别用C_(18)、Cleant TPH固相萃取柱净化,以C_(18)色谱柱分离待测物,在电喷雾正离子化模式下,采用多反应监测(MRM)检测。结果表明,5种农药在1～200μg/L的质量浓度范围内线性关系良好,相关系数均大于0.998,方法检出限为0.2～1.0μg/kg。经3个水平的回收率试验,平均回收率为72.1%～102.0%,相对标准偏差(n=6)为5.08%～10.87%,该方法适用于大米中5种农药残留的同时检测。

A method for the simultaneous determination of molinate,Isoprothiolane,Edifenphos,pretilachlor,and bioresmethrin in rice by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was established.The samples were extracted with acetonitrile,cleaned up by C18 and Cleant TPH solid phase extraction column.The resulting samples were separated on a C18 column and detected under positive multiple reactions monitoring(MRM)mode.The results showed that the linear calibration curves were obtained in the entire range(1-200μg/L)for 5 pesticides,with the correlation coefficients higher than 0.998.For all the samples,the average spiked recoveries ranged for 72.1%-102.0%by three levels,and the relative standard deviations were in the range of 5.08%-10.87%(n=6).The method could use for the determination of the 5 pesticide residues in rice.