UPLC-MS/MS测定桂皮中的氨基甲酸酯类农药残留

Simultaneoue Determination of Carbamate Pesticide in Cinnamomum cassia by UPLC-MS/MS

建立桂皮中8种氨基甲酸酯类农药的Qu ECh ER-超高效液相色谱-串联质谱检测方法。样品经乙腈提取并由混合净化剂(PSA、MWCNTs和无水硫酸镁)净化,色谱柱分离,在多反应监测模式下进行测定。在0.001~0.5μg/m L范围内,8种氨基甲酸酯类农药在桂皮中的峰面积与其质量浓度呈良好线性关系(R^(2)>0.99)。在0.02,0.04和0.20 mg/kg添加水平下重复6次试验,8种氨基甲酸酯类农药回收率为71.0%~110.7%,相对标准偏差(S_(RSD))为1.7%~10.3%,定量限(S_(LOQ))为0.02 mg/kg。试验方法简捷、灵敏、稳定,可满足实际检测需求。

An analytical method for the determination of 8 carbamate pesticides in Cinnamomum cassia using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)matching a Qu ECh ERS procedure was developed.The samples were extracted with acetonitrile and cleaned-up by primary secondary amine(PSA),multi-walled carbon nanotubes(MWCNTs)and MgSO_(4) as sorbent in Cinnamomum cassia.The analytes were separated by a column of C_(18)connected to an electrospray ionization source in positive mode(ESI+)and monitoring(MRM)mode.Eight pesticides showed good linearity in the range 0.001-0.5μg/m L with correlation coefficients higher than 0.99.The average recoveries ranged from71.0% to 110.7% in Cinnamomum cassia at three levels(0.02,0.04 and 0.20 mg/kg)and the relative standard deviation(S_(RSD))was 1.7%-10.3%(n=6).The S_(LOQ)was 0.02 mg/kg.The method was simple,sensitive and stable,meeting the requirements of practical detection.