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建立了板栗中44种有机磷农药多残留的分析方法。样品以V(乙腈)∶V((水)=4∶1为提取剂,经高速匀浆方法提取,提取液以ENVI-18固相萃取柱净化,除去样品中大部分的脂肪和甾醇等干扰基质,再经在线凝胶渗透色谱-气相色谱/质谱(GPC-GC/MS)分析,进一步除去样液中色素和脂肪等大分子干扰物质,有效地降低了样品中的复杂基质所带来的背景干扰。加标水平为0.05 mg/kg时,大部分农药的回收率为65%～120%,相对标准偏差小于15%;44种农药的检出限为0.002～0.05 mg/kg。采用外标法定量,气相色谱-质谱法(GC-MS)定性定量分析,线性关系和回收率结果均满意。实验证明,本方法是一种快速、准确、灵敏度高的同时检测板栗中有机磷农药多残留的检测方法。
To establish a chestnut in 44 kinds of organophosphorus pesticide multi-residue analysis. The sample was extracted by high speed homogenization method with V (acetonitrile): V (water) = 4: 1 as extractant, and the extract was purified by ENVI-18 solid phase extraction column to remove most of the interference of fat and sterol in the sample Matrix and further analyzed by GPC-GC / MS to further remove the macromolecular interferences such as pigment and fat from the sample solution, effectively reducing the amount of complex matrix brought by the sample Background interference.The recoveries of most pesticides ranged from 65% to 120% at spiking levels of 0.05 mg / kg with relative standard deviations less than 15%, and the detection limits of 44 pesticides ranged from 0.002 to 0.05 mg / kg. The results showed that the method was a rapid, accurate and sensitive method for the simultaneous determination of organophosphorus pesticides in Chinese chestnut by quantitative analysis by GC-MS and qualitative and quantitative analysis by gas chromatography-mass spectrometry (GC-MS) Residue detection method.