QuEChERS/气相色谱-三重四极杆串联质谱法同步测定砂仁中28种有机磷农药残留  

Simultaneous Determination of 28 Organophosphorus Pesticide Residues in Amomum villosum by QuEChERS/Gas Chromatography-Triple Quadrupole Mass Spectrometry

作　　者：吴学进[1] 王明月[1] 李春丽[1] 张振山[1] 李萍萍[1] 庞朝海 WU Xue-jin;WANG Ming-yue;LI Chun-li;ZHANG Zhen-shan;LI Ping-ping;PANG Chao-hai(Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables,Analysis and Testing Center,Chinese Academy of Tropical Agricultural Sciences,Haikou 571101,China)

机构地区：[1]中国热带农业科学院分析测试中心海南省热带果蔬产品质量安全重点实验室,海南海口571101

出　　处：《分析测试学报》2020年第2期212-218,共7页Journal of Instrumental Analysis

基　　金：现代农业产业技术体系建设专项资金(CARS-31-13);豇豆中典型农药残留风险评估(GJFP2019006)。

摘　　要：建立了同步测定砂仁中28种有机磷类农药残留的QuEChERS结合气相色谱-三重四极杆串联质谱分析方法。砂仁样品先用1%(体积分数)乙酸乙腈提取,再经900 mg MgSO 4、150 mg PSA、100 mg C18和25 mg GCB组合吸附剂净化后,将提取液浓缩过滤,采用气相色谱-三重四极杆串联质谱在多反应监测(MRM)模式下检测,基质匹配标准曲线外标法定量。结果表明,28种有机磷农药在0.05~1.00 mg/L范围内线性良好,相关系数(r^2)均大于0.99;在0.2、0.4、1.0 mg/kg3个加标水平下的平均回收率为82.1%~104%,相对标准偏差(RSD)不大于15%。28种有机磷农药残留的检出限(LODs)为0.005~0.010 mg/kg,定量下限(LQDs)为0.010~0.033 mg/kg。该方法简便、快速、灵敏,具有良好的灵敏度、准确度和精密度,为提高砂仁的质量和安全性提供了一种快速、高效、可靠的分析方法。An QuEChERS/gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)was developed for the simultaneous determination of 28 organophosphorus pesticide residues in Amomum villosum.The sample was firstly extracted with acetonitrile containing 1% acetic acid(by volume),and then purified with a mixed sorbent of 900 mg MgSO 4,150 mg PSA,100 mg C 18 and 25 mg GCB.After being concentrated and filtered,the extract was analyzed by GC-MS/MS in multiple reactions monitoring(MRM)mode and quantified by the matrix-matched standard calibration curve method.Results showed that the calibration curves for 28 organophosphorus pesticides detected were linear in the range of 0.05-1.00 mg/L with correlation coefficients(r^2)more than 0.99.The average recoveries at spiked levels of 0.2,0.4,1.0 mg/kg for all target compounds in the samples were in the range of 82.1%-104%,with relative standard deviations(RSD)no more than 15%.The limits of detection(LODs)ranged from 0.005 mg/kg to 0.010 mg/kg,and the limits of quantitation(LQDs)were between 0.010 mg/kg and 0.033 mg/kg.With simplicity,rapidness,good sensitivity,accuracy and precision,the method could provide a fast,efficient and reliable analytical approach for improving the quality and safety of Amomum villosum.

关 键 词：砂仁 农药残留 气相色谱-三重四极杆串联质谱(GC-MS/MS) QUECHERS 

分 类 号：O657.71[理学—分析化学]