固相萃取-气相色谱法测定水果中氯吡脲

Determination of chlorpyrifos in fruits by solid phase extraction-gas chromatography

中文关键词:  水果  氯吡脲  固相萃取  气相色谱

英文关键词:forchlorfenuron  gas chromatography  fruit  solid-phase extraction

中文摘要:

      目的 建立固相萃取-气相色谱法(solid-phase extraction and gas chromatography, SPE-GC)检测水果中氯吡脲的方法, 并对猕猴桃、无籽黑提、夏橙和黄心西瓜4种常见水果中氯吡脲的残留进行检测。方法 比较了正己烷、乙酸乙酯、丙酮、甲醇等有机溶剂的萃取效果, 并比较了不同固相萃取小柱的净化效果。结果 萃取溶剂最佳为易分离水层的乙腈, 溶解进样溶剂为丙酮, 溶解度高毒性小且价格经济, 固相萃取小柱选用Florisil柱较好。在此实验条件下, 氯吡脲在0.01~100 mg/L浓度范围内线性良好(r2=0.999893), 检出限为 0.01 mg/kg, 实验回收率在72.8%~90%之间, 相对标准偏差(relative standard deviation, RSD)≤7.9%, 基质效应可以忽略(91.4%~103.0%)。结论 该方法简单准确, 线性范围大, 适用于水果中氯吡脲的残留检测。利用此方法对普洱市某大型超市内猕猴桃等4种水果进行检测, 均未检出氯吡脲, 可见超市水果膨大剂污染很微小。

英文摘要:

      Objective To establish a method for detecting chlorpyrifos in fruits by solid-phase extraction and gas chromatography (SPE-GC), and detected the residues of chlorpyrifos in 4 common fruits of kiwi, seedless black, summer orange and yellow heart watermelon. Methods The extraction effects of organic solvents such as n-hexane, ethyl acetate, acetone and methanol were compared, and the purification effects of different solid phase extraction cartridges were compared. Results The extraction solvent was preferably acetonitrile which is easy to separate the water layer, and the dissolution injection solvent was acetone, whose solubility is high and the toxicity is small and the price is economical. The solid phase extraction column was preferably a Florisil column. Under the experimental conditions, chlorpyrifos had a good linearity in the concentration range of 0.01?100 mg/L (r2=0.999893), the detection limit was 0.01 mg/kg, and the experimental recovery rate was between 72.8% and 90%. The relative standard deviation (RSD) was ≤7.9%, and the matrix effect was negligible (91.4%?103.0%). Conclusion This method is simple, efficient and low instrument requirements, which could be used for the determination of chlorpyrifos residues in fruits. With the method, no forchlorfenuron was detected in kiwifruit and other four fruits in a supermarket in Pu’ er city, which indicated that the supermarket fruit swelling agent pollution is very small.