固相萃取-GC-MS联用法测定何首乌中有机氯农药残留量

Determination of Residues of Organochlorinated Pesticides in Polygonum multiflorum by GC-MS with Solid-phase Extraction

目的:测定何首乌中9种有机氯农药残留量。方法:样品用乙酸乙酯超声提取并经Florisil固相萃取柱净化后,采用毛细管气-质联用仪测定有机氯农药残留量:色谱柱为DB-5MS弹性石英毛细管柱(30m×0.25mm,0.25μm),进样口温度为230℃,程序升温(初始温度100℃,以8℃·min-1升温至220℃,再以5℃·min-1升温至250℃,保持10min),载气流速为1mL·min-1,进样量为1μL。结果:9种有机氯农药能在30min内完全分离;平均回收率为80.4%～97.2%,RSD为3.5%～7.4%(n=6)。结论:本方法灵敏、准确,符合多种有机氯农药残留的检测要求。

OBJECTIVE：To determine the residues of 9 kinds of organochlorinated pesticides in Polygonum multiflorum.ME-THODS：Samples were extracted with ethyl acetate by ultrasonic wave assistant extraction and purified on Florisil solid-phase extraction column.The residues of organochlorinated pesticides were determined with capillary gas chromatography with GC-MS.The separation was performed on DB-5MS（30 m×0.25 mm,0.25 μm） fused-silica capillary column with injector temperature of 230 ℃.The initial column temperature was 100 ℃,then raised to 220 ℃ at the rate of 8 ℃·min^-1.The column temperature was ra-ised at 250 ℃ at the rate of 5 ℃·min^-1 for 10 min.The column flow was 1 mL·min^-1 and injection volume was 1 μL.RESULTS：9 kinds of organochlorinated pesticides were completely separated within 30 minutes.The average recoveries ranged from 80.4% to 97.2%（RSD ranged from 3.5% to 7.4%,n=6）.CONCLUSION：The method is sensitive and accurate for the content determination of the residues organochlorinated pesticides.