分散固相萃取/气相色谱法测定大米中21种有机氯农药

Determination of Seven Organophosphorus Pesticides in Rice by Disperse Solid Phase Extraction Gas Chromatography

建立一种通过固相分散萃取-气相色谱法快速检测大米中21种有机氯农药残留的方法。试样用乙腈提取,提取液经分散固相萃取净化,使用带电子捕获检测器的气相色谱仪检测,根据色谱峰的保留时间定性,外标法定量。本方法在35min内完成《食品安全国家标准食品中农药最大残留限量》(GB2763-2016)规定限值的大米中21种有机氯农药残留的测定,21种有机氯农药的线性范围为0.005~1.000μg/m L,在0.05、0.1和0.5μg/m L添加水平的回收率为93.5%~106.7%,响应值相对标准偏差范围为1.22%~3.55%(n=6),方法检测限为0.001~0.008mg/kg。该方与国标方法相比快速、准确、灵敏,适合于大米中有机氯类药物残留的监控和筛查工作。

A method for rapid determination of 21 organochlorine pesticide residues in Rice by solid phase dispersion extraction and gas chromatography was established.. The sample was extracted with acetonitrile, the extract was purified by dispersed solid phase extraction, and detected by gas chromatography with electron capture detector. The quality of the sample was determined according to the retention time of the chromatographic peak and quantified by external standard method.The method has been applied to the determination of 21 organochlorine pesticides residues in rice within 35 minutes. The linear range of 21 organochlorine pesticides is 0.005 ~1.000 ug/mL in 0.05, 0.1 and 0.5 ug/mL. The recovery of the 21 organochlorine pesticides is 93.5%~106.7%, and the relative standard deviation of response value is 1.22%~3.55%(n=6). The limit is 0.001 ~0.008 mg/kg. Compared with the national standard method, this prescription is fast, accurate and sensitive, and is suitable for monitoring and screening of organochlorine residues in rice.