分散固相萃取GC-MS法快速测定葡萄酒和葡萄中22种农药残留  

Fast Determination of 22 Kinds of Pesticide Residuals in Grape Wine and in Grape by d-SPE Plus GC-MS

作　　者：陈楠楠[1] 高红波[2] 钟其顶[2] 熊正河[2] 谷学新[1] 叶能胜[1] 

机构地区：[1]首都师范大学化学系,北京100048 [2]中国食品发酵工业研究院,北京100027

出　　处：《酿酒科技》2012年第7期119-123,共5页Liquor-Making Science & Technology

基　　金：科技部院所专项<食品加工过程快速监控技术研究及标准化(项目编号:2010EG111008)>;"十二五"科技支撑计划项目<我国传统发酵食品制造安全预警技术研究与应用(项目编号:2012BAK17B11)>

摘　　要：建立了以磷酸三苯酯(TPP)为内标快速测定葡萄和葡萄酒中22种农药残留的方法。采用乙腈萃取,PSA/GCB/ODS作为吸附剂的分散固相萃取法(d-SPE)进行前处理,与传统前处理方法相比,d-SPE在耗时和成本上具有很明显的优势。对比了基质匹配标准溶液和分析保护剂2种方法对基质效应的消除效果,前者效果更为突出;经GC-MS定性和定量分析,22种农药在0.05～0.3 mg/L范围内线性良好,大多数农药3个水平的回收率在70%～130%之间,精密度和重复性(n=5)均小于10%,定量限(LOQ)为0.02～0.1 mg/L。结果表明,该方法适合于葡萄和葡萄酒中农药残留的检测。A method had been developed for fast determination of 22 kinds of pesticide residuals in grape and in grape wine.Such method adopted the extraction with acetonitrile and a cleanup step using dispersive solid-phase extraction（d-SPE） with primary-secondary amine（PSA）,graphitized carbon black（GCB） and octadecylsilane（ODS） used as sorbents.Compared with previous cleanup methods,d-SPE had the advantages in time and cost.Compared with analytic protective agents,the use of matrix-matched standard solution had better performance in decreasing the matrix effects.Through quantitative and qualitative analysis by GC-MS,the acceptable linearity of 22 kinds of pesticide residuals was achieved in the range of 0.05～0.30 mg/L,their recoveries were between 70 % and 130 %,the precision and the repeatability were less than 10 % and 16 % respectively（n=5）,and LOQ was between 0.02～0.1 mg/L.Such method was suitable for the determination of pesticide residuals in grape wine and in grape.

关 键 词：分散固相萃取 葡萄 葡萄酒 农药残留 快速检测 

分 类 号：TS261.7[轻工技术与工程—发酵工程] O657.63[轻工技术与工程—食品科学与工程] TS255.7[理学—分析化学]