液相色谱-串联质谱法同时测定中草药保健食品中15种有机磷和氨基甲酸酯类农药残留

Simultaneous determination of 15 kinds of organophosphorus and carbamate pesticides in herbal health foods by liquid chromatography-tandem mass spectrometry

目的建立高效液相色谱-串联质谱法同时测定中草药保健食品中15种有机磷和氨基甲酸酯类农药残留。方法样品经乙腈提取后,高速离心,经分散型固相萃取小柱净化。采用Atlantis C_(18)(2.1 mm×100 mm,3μm)柱,以0.1%甲酸-乙腈为流动相,梯度洗脱分离。质谱采用正离子模式(electrospray ionization,ESI+),多反应监测模式(multiple reaction monitoring,MRM)进行检测,基质曲线外标法定量。结果该方法对15种农药残留的线性范围为0.001~0.1μg/mL,线性相关系数r≥0.993,加标回收率为82.7%~113.3%,相对标准偏差为2.7%~10.6%,检出限为0.8~24.6μg/kg。结论本方法操作简单、快捷,适用于中草药保健食品中15种有机磷和氨基甲酸酯类农药残留的同时检测,为保健食品质量控制提供依据。

Objective To establish a method for simultaneous determination of 15 kinds of organophosphorus and carbamate pesticides in herbal health foods by liquid chromatography-tandem mass spectrometry（LC-MS/MS）. Methods The samples were extracted by acetonitrile, and purified by dispersive solid-phase extraction column after centrifugation with high speed. The analysis was performed on an Atlantis C_（18） column（2.1 mm×100 mm, 3 μm） using 0.1% formic acid-acetonitrile as mobile phase with gradient elution. Mass spectrometry was performed by positive electrospray ionization（ESI＋） mode and multiple reaction monitoring（MRM） model, and the matrix curve was quantified by external standard method. Results The linear ranges of 15 kinds of pesticide standards were 0.001~0.1 μg/mL, with linear correlation coefficients？ greater than or equal to 0.993, the recoveries at different concentrations were between 82.7%~113.3%, and relative standard deviations（RSDs） were 2.7%~10.6%. The limit of detections（LODs） were 0.8~24.6 μg/kg. Conclusion The method is simple and fast, and suitable for simultaneous determination of 15 organophosphorus and carbamate pesticide residues in Chinese herbal health foods, which provides a basis for the quality control of health foods.