固相萃取-气相色谱法测定大米中有机氯有机磷农药残留

Determination of Organochlorine and Organic Phosphorus Pesticides Residues in Rice by Gas Chromatography Couple with Solid-Phase Extraction

采用固相萃取方法,结合气相色谱建立了同时检测大米中15种有机氯、有机磷农药残留的分析方法。样品用乙腈提取,氨基固相萃取柱净化,经DB-5石英毛细管柱分离后,直接用气相色谱(GC)检测,外标法定量。结果表明15种农药在0.01~0.2μg/mL浓度范围内呈现良好的线性关系,相关系数r均大于0.9951,样品在2个添加水平时的回收率为85.9%~103%,相对标准偏差(RSD)为1.3%~7.3%,检出限为0.002~0.004 mg/kg。该方法样品前处理简单、高效,测定的准确性好,灵敏度高,适用于大米中多种类农药残留的分析。

An analytical method for the simultaneous determination of 15 organochlorine and organic phosphorus pesticides residues in rice was established based on solid-phase extraction couples with gas chromatography(GC).The sample was extracted by acetonitrile and cleaned up by NH2-SPE.After separated on DB-5 capillary column,the analytes were detected by the gas chromatography.The quantitation for all the compounds was carried out using external standard method.The results shows good linearity for 15 pesticide at the range of 0.01~0.2μg/mL with correlation coefficient larger than 0.9951.The recoveries of the pesticides spiked to sample at two levels varied from 85.9%to 103%,with the repeatability RSD from 1.3%to 7.3%.The detection limits for 15 pesticides are 0.002~0.004 mg/kg.The established method is simple,effective,accurate and has high sensitivity,and it can be used for the detection of multiple pesticide residue in the rice.