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目的:结合固相萃取技术,克服了中草药样品中复杂的基质干扰问题,建立超高效液相色谱-串联质谱(UPLC-MS/MS)法检测中药材中15种氨基甲酸酯类杀虫剂的残留量。方法:样品中残留的农药经乙腈提取,PSA固相萃取柱净化后,采用UPLC-MS/MS法进行测定。结果:15种农药在其各自的浓度范围内,线性关系良好,相关系数在0.995～0.999之间。在定量限(LOQ)、5倍定量限和10倍定量限3个添加浓度水平,平均加标回收率在61.8%～98.1%之间;RSD在1.8%～14.8%之间。结论:该方法操作简便,净化效果好,灵敏度高,可为中药材中氨基甲酸酯类杀虫剂污染状况调查提供检测方法支持。
OBJECTIVE: To overcome the problem of complex matrix interference in Chinese herbal medicine by solid-phase extraction, and to establish a method for the determination of 15 carbamate insecticides in Chinese herbal medicines by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) Residues. Methods: Residual pesticides in the sample were extracted with acetonitrile and cleaned up by PSA solid-phase extraction column, and determined by UPLC-MS / MS. Results: The 15 pesticides showed good linearity within the range of their respective concentrations with the correlation coefficients between 0.995 and 0.999. The average spike recoveries ranged from 61.8% to 98.1% at 3 levels of LOQ, 5-fold and 10-fold limit of quantification. RSD ranged from 1.8% to 14.8%. Conclusion: The method is simple and easy to operate, with good purification effect and high sensitivity. It can provide the detection method support for the investigation of the pollution status of carbamate insecticides in Chinese herbal medicines.