张振山 乐渊 黎舒怀 刘春华 李萍萍

摘要 [目的]建立QuEChERS-超高效液相色谱-串联质谱检测砂仁中10种氨基甲酸酯类农药残留量的方法。[方法]砂仁样品先用含1%甲酸的乙腈溶液提取，再经盐析剂盐析后加入MgSO4、PSA和C18进行萃取、净化，采用UPLC-MS/MS检测，基质匹配标准曲线外标法进行定量。[结果]目标化合物在2.5～100.0 μg/L有良好的线性关系，R2≥0.999;在0.02、0.08和0.40 mg/kg 3个添加水平下，10种农药成分加标回收率为70.7% ～ 113.3%，RSD为0.2%～4.9%（n=3）;定量限（LQD）在0.19～4.01 μg/kg。[结论]该方法操作简单、净化效果好、灵敏度高、准确度高，适用于砂仁药材中10种氨基甲酸酯类农药的残留检测。

关键词 砂仁;氨基甲酸酯类农药;QuEChERS-超高效液相色谱-串联质谱

中图分类号 S481+.8 文献标识码 A 文章编号 0517-6611（2021）01-0199-04

doi：10.3969/j.issn.0517-6611.2021.01.053

Abstract [Objective]To establish a method for the simultaneous determination of 10 carbamate pesticide residues in Amomum villosum Lour. by QuEChERS-ultraperformance liquid chromatography-tandem mass spectrometry. [Method]The samples were extracted with acetonitrile （containing 0.1% formic acid）and followed by salting-out process， the extract was further purified by C18， PSA and anhydrous magnesium sulfate. The prepared samples were then analyzed by UPLC-MS/MS and quantified by the matrix-matched standard calibration curve method. [Result]The target compound had a good linear relationship between 2.5-100.0 μg/L， R2≥0.999;at spiked levels of 0.02，0.08 and 0.40 mg/kg， the average recoveries of all the pesticides were 70.7% - 113.3%， and the RSD was 0.2% -4.9%（n =3） . The limits of detection（LOD） was 0.19 - 4.01 μg/kg. [Conclusion]The method has simple operation， good purification effect， high sensitivity and high accuracy， and is suitable for the detection of 10 carbamate pesticide residues in Amomum vilosum Lour..

Key words Amomum villosum Lour.;Carbamate pesticide;QuEChERS-UPLC-MS/MS

砂仁是姜科植物阳春砂（Amomum villosum Lour.）、绿壳砂（Amomum villosum Lour.var.xanthioides T.L.Wu et Senjen）或海南砂（Amomum longiligularg T.L.wu）的干燥成熟果实，为四大南药之一，具有化湿开胃、温脾止泻、理气安胎的功效，主要用于湿浊中阻、脘痞不饥、脾胃虚寒、呕吐泄泻、妊娠恶阻、胎动不安等病症[1]，在治疗消化系统等方面的疾病具有很独特的功效[2]。随着砂仁药材的需要量逐年增加，砂仁的人工种植面积也在逐渐扩大，药材的农药滥用误用现象也时有发生[3]。

氨基甲酸酯类农药是在有机磷类农药之后发展起来的一种合成农药，作为杀虫剂、除草剂和杀菌剂广泛应用于农业生产中，具有高效、低残留的特点[4]。然而，在中药材的害虫防治过程中也易产生农药残留，不仅会污染水体、土壤，破坏生态结构，也会影响临床用药健康，对人类的健康产生危害[5]。笔者拟采用 QuEChERS 净化工艺，优化提取与净化方法，旨在建立砂仁中10种氨基甲酸酯类农药残留的检测方法，满足砂仁中氨基甲酸酯类农药的日常检测要求。……