气相色谱质谱法同时测定地表水中5种杀菌剂的残留量

Simultaneous determination of five fungicides residues in surface water by gas chromatography-mass spectrometry

采用QuEChERS净化联合气相色谱三重四级杆质谱建立地表水中检测地表水中嘧霉胺、腐霉利、霜霉威、乙霉威和抑霉唑残留的分析方法。地表水样品采用乙腈溶剂提取、无水硫酸镁盐析,提取液以十八烷基键合硅胶(C18)、N-丙基乙二胺(PSA)为净化剂进行分散固相萃取净化。采用Rtx-5MS色谱柱(30 m×250μm,0.25μm)分离,进样气相色谱质谱,采用多反应监测模式(MRM)扫描分析。5种农药的检出限如下:嘧霉胺为0.008 mg/kg,腐霉利为0.005 mg/kg,霜霉威为0.012 mg/kg,乙霉威为0.007 mg/kg和抑霉唑为0.008 mg/kg。样品平均回收率均在82.9%~99.6%之间;精密度检测的相对标准偏差均小于5%(n=6)。该方法前处理简便快捷、成本低、效率高、准确性好,可满足地表水中多种农药残留的同时分析。

The combination of QuEChERS and gas chromatography-triple quadrupole mass spectrometry(GCMS/MS)was employed to establish an analytical method for determination 5 pesticide residues in surface water,including pyrimethanil,procymidone,propamocarb,diethofencarb and imidazole.Water samples were extracted by acetonitrile solution,anhydrous magnesium sulfate was used for salting out.The exracted solution were purified by dispersive solid phase extraction C18 and N-propyl ethylenediamine(PSA).Rtx-5MS(30 m×250μm,0.25μm)column was selected for seperation,samples were detected on GC-MS/MS by multiple reaction monitoring(MRM).The detection limits of 5 pesticides were as follows:pyrimethanil:0.008 mg/kg;procymidone:0.005 mg/kg;propamocarb:0.012 mg/kg;diethofencarb:0.007 mg/kg;imidazole:0.008 mg/kg.The recoveries were ranged from 82.9%to 99.6%.The relative standard deviation(RSD)of precision was with 5%(n=6).This method was proved to be simple,fast,low cost,high efficiency and accurate,and can be used for simultaneous analysis of pesticide residues in surface water.