优化QuEChERS法联合UPLC-MS/MS测定马兰草中35种农药的残留  

Optimized QuEChERS method combined with UPLC-MS/MS in determining 35 pesticide residues in Kalimeris indica(L.)Sch.-Bip.

作　　者：刘勋 张迅 LIU Xun;ZHANG Xun(Guizhou Provincial Food and Drug Inspection Institute,Guiyang 550000,Guizhou,China;Guizhou Provincial Drug Evaluation Center,Guiyang 550081,Guizhou,China)

机构地区：[1]贵州省食品药品检验所,贵州贵阳550000 [2]贵州省药品评价中心,贵州贵阳550081

出　　处：《贵州医科大学学报》2024年第8期1154-1159,1169,共7页Journal of Guizhou Medical University

基　　金：贵州省科技计划项目(黔科合支撑〔2021〕一般418)。

摘　　要：目的建立优化的QuEChERS提取方法结合超高效液相色谱-串联质谱(UPLC-MS/MS)测定马兰草中35种农药残留的方法。方法13批次马兰草样品净化前处理后,采用QuEChERS提取方法,以乙腈作为提取溶剂、经亲水亲油平衡材料(HLB SPE)固相萃取柱净化,选择waters Xbridge C18色谱柱(10 cm×2.1 mm,2.6μm)、0.1%甲酸溶液(含5 mmol/L甲酸铵)-乙腈为流动相,柱温40℃、流速0.3 mL/min,应用超高效液相色谱-串联质谱法(UPLC-MS/MS)在多反应监测模式(MRM)下扫描,采用基质标准曲线法对马兰草中35种目标农药进行定量分析。结果所检35种农药在0.77~155.38μg/L浓度范围内线性关系良好,相关系数均大于0.9938;方法加标回收率为71.3%~108.7%,相对标准偏差(RSD)为1.7%~6.7%,检测限范围为0.77~7.77μg/L,1批样品中检出甲拌磷。结论本研究建立的方法具有操作简便、灵敏度高及可靠性强等特点,适用于马兰草中多种农药残留的检测。Objective To establish an optimized QuEChERS method combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)for the simultaneous determining 35 pesticide residues in Kalimeris indica(L.)Sch.-Bip.Methods After purification pretreatment of 13 batches of Kalimeris indica(L.)Sch.-Bip.samples,the QuEChERS method was used.Acetonitrile was selected as the extraction solvent,and the pesticides were purified by hydrophilic and lipophilic balance material(HLB SPE)solid-phase extraction column.UPLC-MS/MS settings:waters Xbridge C18 chromatographic column(10 cm×2.1 mm,2.6μm),0.1% formic acid solution(containing 5 mmol/L ammonium formate)-acetonitrile as a mobile phase,column temperature of 40℃,flow rate of 0.3 mL/min.Under multiple reaction monitoring mode(MRM),UPLC-MS/MS were applied to scan and quantitatively analyze 35 target pesticides in Kalimeris indica(L.)Sch.-Bip using a matrix standard curve.The tested 35 pesticides showed good linear relationships within the concentration range of 0.77-155.38μg/L and correlation coefficients greater than 0.9938.The recovery rate of the spike-in method was 71.3% to 108.7%,and the relative standard deviation(RSD)was 1.7% to 6.7%.The detection limit range was from 0.77 to 7.77μg/L.Methyl phosphorus was detected in one batch of the samples.Conclusion The method established in this study is easy to operate,with high sensitivity and strong reliability.It is suitable to detect various pesticide residues in Kalimeris indica(L.)Sch.-Bip.

关 键 词：QUECHERS 马兰草 超高效液相色谱-串联质谱 农药残留 

分 类 号：R284.1[医药卫生—中药学]