高效液相色谱-串联质谱法测定粮谷中的克瘟散

Study on the determination of edifenphos in grain by HPLC-MS/MS

应用高效液相色谱-三重四极杆质谱联用仪(HPLC-MS/MS)建立了粮谷中克瘟散的分析方法。实验确立以90%乙腈水溶液为提取溶剂,应用ProElut AFT-3固相萃取柱进行净化,乙腈-0.1%甲酸溶液(6+4,V/V)为定容液的预处理方法。实验结果表明,在最优条件下,目标物在1.0~100.0μg/L范围内线性良好,5种基质匹配(面粉、小米、糙米、玉米、大米)曲线的相关系数(r)均大于0.9997,加标实验回收率在78.5%~112.3%之间,相对标准偏差(RSD)为3.4%~13%,方法检出限(LOD,S/N≥3)为0.3μg/kg,定量限(LOQ,S/N≥10)为1.0μg/kg。经方法学验证,方法适用于粮谷中克瘟散的检测与定量测定。

This method was established for the study of Edifenphos in grain by HPLC-MS/MS. The analyst was extracted from the sample by acetonitrile-water solution （ V： V = 9 ： 1 ）, and then purified by ProElut AFT-3 solid phase extraction （SPE） cartridge. The eluent was concentrated to dry and redissolved in acetonitrile -0. 1% acid solution. As a result, all the calibration curves obtained in five matrix （flour, millet, brown rice, maize, and rice） were linear with correlation coefficients larger than 0. 9997 （r 〉0. 9997） in the range of 1.0 to 100, 0 μg/L, The recoveries were 78. 5% - 112. 3%, and the relative standard deviations （RSDs） were 3.4% - 13.0% at spiked levels of 1.0 - 10. 0μg/L, the limits of detection （LOD） was 0. 3 μg/kg, and the limit of quantitation （LOQ） was 1.0 μg/kg. The method is suitable to be used for the investigation of the Edifenphos in grain.