蔬菜中多种有机磷农药残留的固相萃取-气相色谱测定方法研究

Simultaneous determination of organophosphorus pesticide residues in vegetables by solid phase extraction coupled with gas chromatography (SPE-GC)

目的建立同时测定蔬菜中多种常见有机磷农药残留的固相萃取-气相色谱法。方法样品经乙腈提取、固相小柱净化,气相色谱法进行测定。结果在优化的条件下,多达19种的有机磷农药均能较好的分离,峰面积与浓度之间呈现良好线性,相关系数r≥0.9994,定量检出限为2.5~16.9μg/kg。蔬菜加标回收率为62.4%~111.5%,相对标准偏差(RSD)为0.74%~5.26%。结论该法操作简便,灵敏,准确,重现性好,适用于蔬菜中多种常见有机磷农药残留的测定和分析。

Objective To establish a method for the simultaneous determination of common organic phosphorus pesticide residues in vegetables by solid phase extraction coupled with gas chromatography （ SPE- GC）. Methods Samples were extracted by acetonitrile, cleaned up on a solid phase column purification and determined by SPE-GC. Results Under the selected con- ditions, up to 19 kinds of organic phosphorus pesticide could be completely separated and showed good linearity. The correlation coefficient （r） was ≥ 0.9994, with the detection limit of 2.5-16.9 μg/kg. The recovery rate of standard addition was 62.4%- 111.5%, and the relative standard deviation （ RSD ） was 0.74%-5.26%. Conclusions The experimental results show that the method is simple, highly sensitive and accurate, with a good reproducibility. It is suitable for the determination and analysis of the common organophosphorus pesticide residues in vegetables.