Simultaneous determination of 45 herbicides and insecticides in aquatic feeds by enhanced matrix removal-lipid coupled with gas chromatography-triple quadrupole-tandem mass spectrometry
The aim of this experiment was to establish a method for simultaneous determination of 45 pesticide residues,which include herbicides and insecticides,in aquatic feed using gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)coupled with enhanced matrix removal-lipid.Optimized instrumental parameters,extraction reagents,purification method,volume of activated water for enhanced matrix removal-lipid(EMR-Lipid),addition of primary secondary amine(PSA),and matrix effect of sample.The optimal pretreatment process was finally determined as follows:The DB-5MS gas chromatographic column with low loss and the 453A1925-UI quartz liner with ultra-high inertia were selected.The sample was extracted with 1%acetate acetonitrile,cleaned-up by dispersive solid-phase extraction using EMR-lipid dispersant sorbent and PSA sorbent,the optimal volume of activated water was 5 mL,the amount of PSA adsorbent was 0.12 g,detected by gas chromatography-triple quadrupole mass spectrometry,multiple reaction monitoring(MRM)mode,the matrix matching calibration and external standard method were used for quantitation.The results showed that the 45 pesticide residues had good linear relationships in the range of 10 to 500 μg/L,with correlation coefficients between 0.9911 and 0.9999,The detection limit(LODs)of the method were 0.5～3.3 μg/kg,and the limit of quantitation(LOQs)were 1.7～10.1 μg/kg,the recovery was between 68.34%and 114.7%except methidathion with recovery between 58.01%and 59.27%,the relative standard deviations(RSDs,n=6)was 0.7%～11.0%.The purification effect and detection limit of method were superior to current standard for feed detection.30 samples of various feed matrices were analyzed sold on market,the result suggested that 3 target pesticides were positive in 3 samples,the positive pesticide were chlorpyrifos,atrazine and trifluralin with content of 8.3,10.1,20.1 μg/kg separately.The method was simple operation,high sensitivity,good repeatability and environment-friendly,and could be used for simultaneous rapid quantitative detection of 45 herbicides and insecticides residues in feed.
gas chromatography-triple quadrupole-tandem mass spectrometry(GC-MS/MS)enhanced matrix removal-lipid clean-upmulti-pesticide residuesaquatic feed
万方数据
维普
