建立了丙酮和乙腈(体积比85: 15)提取,凝胶渗透色谱(GPC)法和PSA(N-丙基乙二胺)固相萃取柱2种方法净化,超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测菠菜、黄瓜、大葱、蘑菇、香菇、木耳、牛肝菌和胡萝卜中19种氨基甲酸酯类农药(NMCs),同位素稀释法定量.实验结果表明,GPC法净化,回收率为70.1%～95.7%;PSA固相萃取柱净化,回收率为70.2%～94.9%.方法的检出限均为1×10~(-5) g/kg.各种NMCs在确定的添加范围内线性关系良好,线性相关系数r均＞0.99,所建立的检测方法实用、准确、灵敏度高.
A method was developed for the simultaneous determination of 19 carbamate pesticides residues in spinach, cucumber, scallion, fungus, mushroom, agaric and carrot by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) combined with isotope internal standard method. The vegetable and mushroom samples were extracted with V(acetone): V(acetonitrile)=85: 15 then purified by gel permeation chromatography(GPC) or solid phase extraction(SPE). The recoveries ranged from 70.1% to 95.7% with the cleaning method of GPC and from 70.2% to 94.9% with the cleaning method of primary-secondary amine(PSA) SPE.The limits of detection(LOD) were 1×10~(-5) g/kg. The method showed a good linear relationship with the correlation coefficients over 0.99.This method is practical, accurate and highly sensitive.
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