分散固相萃取净化-气相色谱法测定大米中4种农药残留

Simultaneous determination of 4 pesticide residues in rice by gas chromatography with dispersive solid-phase extraction cleanup

中文关键词:  分散固相萃取  气相色谱  丁草胺  噻嗪酮  稻瘟灵  溴氰菊酯  大米

英文关键词:dispersive solid-phase extraction  gas chromatography  butachlor  buprofezin  isoprothiolane  deltamethrin  rice

中文摘要:

      目的 建立一种同时测定大米中丁草胺、噻嗪酮、稻瘟灵、溴氰菊酯4种农药残留的分散固相萃取-气相色谱法。方法 样品经乙腈提取, 盐析后, 提取液经N-丙基-乙二胺硅烷(N-propyl-ethylenediamine silane, PSA)和十八烷基硅胶(C18)分散固相萃取材料净化后上机测定。优化的色谱条件为: DB-17(30 m×0.25 mm, 0.25 μm)石英毛细管柱, 采用程序升温分离, 流速为1.0 mL/min, 进样量1.00 μL, 电子捕获检测器检测。结果 4种农药在0.001~8 μg/mL范围内线性良好, 相关系数(r)均大于0.999, 定量限为0.001~0.08 mg/kg, 4种农药平均回收率为89.6%~102.9%, 相对标准偏差(RSD)在2.11%~7.81%(n=6)之间。结论 该方法操作简便、快速、准确, 适用于大米中4种农药残留痕量分析。

英文摘要:

      Objective To establish a method for determination of butachlor, buprofezin, isoprothiolane and deltamethrin in rice by gas chromatography with dispersive solid-phase extraction. Methods The sample was extracted by acetonitrile, and after salt analysis, the extracting solution was purified by PSA and C18. The optimized chromatographic conditions were as follows: DB-17 (30 m×0.25 mm, 0.25 μm) quartz capillary column and heating process was used, the flow rate was 1.0 mL/min, and the sample amount was 1.00 μL, monitoring with an electron-capture detector. Results Four kinds of pesticide residues had good linear relationships in the range of 0.001~8 μg/mL, and the correlation coefficients were more than 0.999. The limits of quantification of the method were 0.001~0.08 mg/kg. The recoveries were 89.6%~102.9%, with the relative standard deviations of 2.11%~7.81%(n=6). Conclusions The method is simple, rapid and accurate, which can be used in the analysis of 4 pesticide residues in rice.