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目的建立气相色谱定量测定螃蟹中19种有机氯(OCPs)类混合农药残留的方法。方法样品用乙腈提取,环己烷-乙酸乙酯(1∶1,V/V)定容,凝胶渗透色谱(GPC)和氨基固相萃取柱(Carb/NH2)联合净化,经气相色谱(GC)检测分析。结果 19种化合物在0.02~2 mg/L内线性关系良好(r>0.993),各有机氯的检出限为0.04~0.31μg/kg(S/N=3)。在加标水平为20、40、80μg/kg时,方法的回收率为81.3%~116.2%,相对标准偏差为0.6%~7.5%。结论该方法选择性好、灵敏度高,样品净化效果好,适用于螃蟹中有机氯类农药的多残留痕迹测定。
Objective To establish a method for the quantitative determination of 19 organochlorine (OCPs) mixed pesticides in crabs by gas chromatography. Methods The samples were extracted with acetonitrile, fixed with cyclohexane-ethyl acetate (1: 1, V / V), and purified by gel permeation chromatography (GPC) and amino-solid phase extraction cartridges (Carb / NH2) GC) test analysis. Results The linear range of 19 compounds was 0.02-2 mg / L (r> 0.993). The detection limit of each organic chlorine was 0.04-0.31 μg / kg (S / N = 3). The method recoveries ranged from 81.3% to 116.2% with relative standard deviations of 0.6% -7.5% at the spiked levels of 20, 40 and 80 μg / kg. Conclusion The method has good selectivity, high sensitivity and good purification effect. It is suitable for the determination of trace residues of organochlorine pesticides in crabs.