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

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。

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

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.