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目的建立蔬菜中残留有机氯及有机磷农药的大口径毛细管气相色谱测定法。方法采用大口径毛细管气相色谱分析技术代替传统的填充柱气相色谱技术,采用程序升温分离蔬菜中残留的多种有机氯及有机磷农药。结果本实验中敌百虫、敌敌畏、甲拌磷、乐果、甲基对硫磷、杀螟硫磷、马拉硫磷、倍硫磷、乙基1605最低检出浓度为0.004~0.008mg/kg,线性范围为0.5~5.0μg/ml,相关系数为0.9965~0.9990,平均回收率范围为88.47%~96.51%,RSD为2.98%~5.16%。α-666、β-666、γ-666、δ-666、p,p’-DDE、o,p’-DDT、p,p’-DDD、p,p’-DDT的线性范围为0.002~0.2μg/ml,相关系数为0.9994~0.9997,最低检出浓度为0.0007~0.001mg/kg,平均回收率范围86.51%~98.45%,RSD为2.47%~5.32%。结论该法可以很好地分离蔬菜中残留的多种有机氯和有机磷农药,灵敏度高,结果准确可靠。
Objective To establish a method for the determination of residual organochlorine and organophosphorus pesticide residues in vegetables by capillary gas chromatography. Methods Large-bore capillary gas chromatography was used to replace traditional column packed gas chromatography (GC-MS). A variety of organochlorine and organophosphorus pesticide residues in vegetables were separated by temperature program. Results The minimum detectable concentrations of trichlorfon, dichlorvos, phorate, dimethoate, methyl parathion, fenitrothion, malathion, fenthion and ethyl 1605 in this experiment ranged from 0.004 to 0.008 mg / kg, the linear range of 0.5 ~ 5.0μg / ml, the correlation coefficient of 0.9965 ~ 0.9990, the average recovery range of 88.47% ~ 96.51%, RSD of 2.98% ~ 5.16%. The linear range of α-666, β-666, γ-666, δ-666, p, p’-DDE, o, p’-DDT, p, p’-DDD, p, p’-DDT was 0.002-0.2 μg / ml, the correlation coefficient was 0.9994 ~ 0.9997, the lowest detected concentration was 0.0007 ~ 0.001mg / kg, the average recoveries ranged from 86.51% to 98.45%, RSD was 2.47% ~ 5.32%. Conclusion The method can be well separated from vegetables in a variety of organic chlorine and organophosphorus pesticides, high sensitivity, the results are accurate and reliable.