UPLC-MS/MS法同时测定裸花紫珠药材中9种农药残留

Simultaneous determination of 9 pesticide residues in medicinal Callicarpa nudiflora by UPLC-MS/MS

目的采用固相萃取(SPE)前处理技术净化样品,建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定裸花紫珠药材中9种农药残留的方法。方法裸花紫珠样品用乙腈提取,通过Cleanet-TPH固相萃取柱净化,采用安捷伦1290~6460超高效液相色谱质谱联用仪测定,流动相为乙腈-水(含0.1%甲酸),扫描方式为多反应离子监测(MRM)模式。结果多菌灵、敌百虫、敌敌畏、灭线磷、倍硫磷、甲拌磷、丙溴磷、辛硫磷、丁硫克百威等9种被测物质的线性关系良好,相关系数为0.997 8~0.999 7,各农药的定量限为0.003~3.1μg/kg,测试精密度和重复性良好,RSD值均<3.0%;高、中、低3个浓度的样品加标回收率范围为92.7%~103.9%。3批裸花紫珠样品检出了多菌灵、敌百虫、辛硫磷等3种农药残留。结论所建立的方法简便、准确度及灵敏度高、分析速度快、专属性好,可用于裸花紫珠药材中9种农药残留的测定。

Objective To develop a method for the determination of 9 pesticide residues in medicinal Callicarpa nudiflora by ultra-performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） after purification of samples by solid phase extraction（SPE） pretreatment. Methods The samples of Callicarpa nudiflora were extracted with acetonitrile, purified by Cleanet-TPH solid phase extraction column, and analyzed by UPLC-MS/MS（Agilent1290-6460）; the mobile phase was acetonitrile-water（containing 0.1% formic acid） and the scanning mode was multiple reaction monitoring（MRM）. Results The linear relationships of 9 kinds of tested substances was good, including carbendazim, dipterex, dichlorvos, chlorpyrifos, fenthion, phorate, profenofos, phoxim and carbosulfan; the correlation coefficient（r） was between 0.997 8 and 0.999 7; the limit of quantification（LOQ） of each pesticide was in the range of0.003~3.1 μ g/kg, the test precision and repeatability were good, and the RSD values were all3.0%. The recovery of high, medium and low concentrations of the samples ranged from 92.7% to 103.9%. Three kinds of pesticide residues such as carbendazim, dipterex and phoxim were detected in 3 batches of Callicarpa nudiflora sample. Conclusion The method established in this study is simple, accurate and sensitive, fast in analysis and good in specificity. It can be used for the determination of 9 pesticide residues in medicinal Callicarpa nudiflora.