气相色谱-串联三重四级杆质谱法测定蔬菜水果中7种农药残留

Determination of 7 Kinds of Residual Pesticide in Vegetables and Fruits by Gas Chromatography-Triple Guadrupole Tandem Mass Sectrometry

建立了气相色谱串联质谱(GC-MS/MS)定量和定性检测蔬菜水果中甲拌磷、甲拌磷砜、甲拌磷亚砜、氟虫腈、氟甲腈、氟虫腈砜、氟虫腈亚砜等7种农药多残留量的方法。样品中的待测农药组分经乙腈提取,采用QuEChERS法为净化方法,以外标法进行定量,以气相色谱-三重四级杆串联质谱多反应检测模式(MRM)检测。结果表明,不同样品的加标回收率为73.2%～107.1%,相对标准偏差为0.07%～3.19%,检出限为0.002～0.010 mg/kg。该方法准确性高、重复性好、操作简便,符合农药残留分析的要求。

A method was developed for the quantitative and qualitative determination of 7 kinds of pesticide residues, including phorate, phorate sulfone, phorat-sulfoxide, fipronil, fipronil-desulfiny, fipronil-sulfone, fipronil-sulfide in vegetables and fruits by triple quadrupole gas chromatography- mass spectrometry.Samples were extracted with acetonitrile and then purified by QuEChERS.Samples were determined by GC-MS/MS with multiple reaction monitoring mode(MRM),and quantitated by extrnal standardmethod.The results showed that the additive recovery rates ofdifferent samples were 73.2%-107.1%, the relative standard deviations(RSD)were between 0.07%-3.19%, detection limit of this method was 0.002-0.010 mg/kg.This method had high precision, good reproducibility, simple operation, could meet requirements of pesticide residue analysis.