气相色谱/三重四级杆质谱法同时测定蔬菜水果中13种农药残留

Simultaneous Determination of 13 Kinds of Pesticide Residues in Vegetables and Fruits by Gas Chromatography/Triple Quadrupole Tandem Mass Spectrometry

建立了固相萃取(SPE)前处理方法联合气相色谱/三重四极杆质谱(GC-MS/MS)检测蔬菜水果中西玛津、莠去津、嘧霉胺、异丙甲草胺、二甲戊灵、氟虫腈、稻瘟灵、虫螨腈、乙酯杀螨醇、哒螨灵、咪鲜胺、苯醚甲环唑、嘧菌酯共13种农药多残留的检测分析方法。结果表明:13种农药在30 min内实现了良好的分离,在0.01~2.00 mg/L的质量浓度范围内线性关系良好,相关系数>0.998,方法检出限为0.001~0.010 mg/kg。13种农药在0.01、0.10、1.00 mg/L 3个浓度添加水平下,平均回收率在82.9%~111.2%之间,测定值的相对标准偏差(n=6)在1.1%~5.6%之间,能够满足农药多残留的分析要求。

SPE-GC-MS/MS was proposed for the determination of 13 kinds of pesticide residues,including simazine, atrazme,pynmethand, metolachlor, pendimethalin, fipronil, isoprothiolane, ehlorfenapyr, ehlorobenzilate, pyridaben, prochloraz, difenoeonazole, azoxystrobin in vegetables and fruits.Results showed that 13 pesticides could be well separated within 30 minutes, and the linear ranges of 13 pesticides were all 0.01-2.00 mg/L with the linear relative coefficients more than 0.998 and detection limits in the range of 0.001 ~0.010 mg/kg.Recovery rates at the three concentrat- ions of 0.01,0.10,1.00 mg/L ranged from 82.9% to 111.2%, and RSDs （n=6） were in the range of 1.1%- 5.6%, which fitted for the requirements of residue analysis.