气相色谱质谱法检测水中5种甲氧基丙烯酸酯

建立了QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)-气相色谱质谱联用法检测农耕水环境中的5种甲氧基丙烯酸酯类杀菌剂(嘧菌酯、醚菌酯、肟菌酯、吡唑醚菌酯、嘧菌胺)残留的方法。农耕水样品过滤后,用乙腈溶剂进行提取,加入QuEChERS萃取包(4 g MgSO4,1 g乙酸钠)萃取后,将提取液转移至QuEChERS纯化管(1.2 g MgSO4,400 mg N-丙基乙二胺(PSA),400 mg石墨化炭黑(GCB)和400 mg C18)中净化,浓缩后用正己烷定容至1 mL,进样气相色谱质谱系统以多反应监测模式(MRM)分析,外标法定量。5种甲氧基丙烯酸酯类杀菌剂在0.02~2.0μg/mL质量浓度内与其对应的峰面积呈良好的线性关系,相关系数均大于0.995。检出限为0.012~0.019μg/m L,定量限为0.036~0.057μg/mL;在0.1,0.5和1.0μg/mL加标水平下,5种农药的回收率均在82.6%~103.2%之间;精密度测试的相对标准偏差小于5%。该方法前处理操作简单,高效,灵敏度高、准确性好,适用于农耕水中甲氧基丙烯酸酯类杀菌剂残留的测定。

Detection of Five Methoxyacrylate Fungicides in Agricultural Water by Gas Chromatography-Mass Spectrometry

An analytical method for determination of 5 methoxy acrylate fungicides(azoxystrobin,kresoxim-methyl,trifloxystrobin,pyraclostrobin and mepanipyrim)in agricultural water,which was based on QuEChERS pre-treat with gas chromatography-mass spectrometry(GC/MS),was established.Agricultural water samples was filtered first,then extracted by acetonitrile.QuEChERS extracts package(4 g magnesium sulfate,1 g sodium acetate)was added for extraction,and extraction solution was then transferred to purification tube(1.2 g magnesium sulfate,400 mg PSA,400 mg GCB and 400 mg C18)for purification.The purified solution was condensed and fixed to 1 mL with hexane.Samples were detected by multi-reactions monitoring(MRM)on GC/MS,and external standard method was selected for quantitative.Five methoxy acrylate fungicides showed good linear relationships with the chromatographic peak area in the range 0.02-2.0μg/mL,and the correlation coefficients were all above 0.995.The detection limits were in the range 0.012-0.019μg/mL,and quantitation limits were 0.036-0.057μg/mL.The recoveries of 5 pesticides at the spiked levels of 0.1,0.5 and 1.0μg/mL ranged from 82.6%to 103.2%.The relative standard deviations(RSD)of precision were below 5%(n=6).This multi-residue analytical method allowed for a rapid,efficient,sensitive and reliable quantitative analysis of methoxy acrylate fungicides in agricultural water.