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作 者:姚家彪[1] 赵颖[1] 潘伟[1] 蒋施[1] 钟钰[1] 金雁[1]
机构地区:[1]沈阳出入境检验检疫局综合技术中心,沈阳110016
出 处:《应用化学》2010年第4期488-493,共6页Chinese Journal of Applied Chemistry
基 金:"十一.五"国家科技支撑计划(2006BAK02A08-005)资助项目
摘 要: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1×10-5g/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(UPLCMS/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.
关 键 词:GPC PSA 超高效液相色谱-串联质谱 氨基甲酸酯
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