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

中文关键词:  液相色谱-串联质谱法  中草药保健食品  有机磷  氨基甲酸酯

英文关键词:cordycepin  ultra performance liquid chromatography-mass spectrometry  high performance liquid chromatography  rapid screening  quantitative determination

中文摘要:

      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 C18(2.1 mm×100 mm, 3 μm)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0.001~0.1 μg/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0.8~24.6 μg/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。

英文摘要:

      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 C18 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.