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目的利用固相萃取-气相色谱法(SPE-GC)为检测方法,建立复杂基质蔬菜膳食中19种有机磷农药残留的同时分析方法。方法样品初步粉碎后加入乙腈,在高速分散均质机中匀浆提取,用氯化钠分层,有机相经氮吹浓缩后用石墨化碳黑/氨基(Carb-NH2)固相萃取柱净化,丙酮-二氯甲烷(1:1,V/V)作为淋洗液,浓缩后的淋洗液经DB-1701柱分离进入火焰光度检测器(FPD)进行测定分析。结果 19种农药分离效果良好,在0.025μg/ml~0.6μg/ml时相关系数r均>0.999 1,方法检出限在0.000 7 mg/kg~0.003 4 mg/kg,0.025 mg/kg、0.05 mg/kg和0.2 mg/kg 3个添加水平时的平均回收率为73.9%~118.9%,相对标准偏差(RSD)为1.19%~9.62%。结论该方法简便、快速,结果准确,适用于蔬菜膳食样品中有机磷农药残留的分析以及相关膳食人体健康的风险监测研究。
OBJECTIVE To establish a simultaneous method for the determination of 19 organophosphorus pesticide residues in vegetables with complex matrix by SPE-GC method. Methods After initial crushing, acetonitrile was added into the sample and homogenized in high speed homogenizer. The organic phase was separated by sodium chloride. The organic phase was concentrated by nitrogen and cleaned up with carbon black / amino acid (Carb-NH2) SPE cartridge , Acetone-methylene chloride (1: 1, V / V) as eluent, and the concentrated eluent was separated by DB-1701 column into flame photometric detector (FPD) for analysis. The results showed that 19 kinds of pesticides were separated well and the correlation coefficients r were all 0.999 1 at 0.025μg / ml ~ 0.6μg / ml. The limits of detection were 0.0007 mg / kg ~ 0.003 4 mg / kg, 0.025 mg / kg, The average recovery was 73.9% ~ 118.9% with relative standard deviations (RSDs) of 1.19% ~ 9.62% at the three levels of mg / kg and 0.2 mg / kg. Conclusion The method is simple, rapid and accurate. It is suitable for the analysis of organophosphorus pesticide residues in vegetable meal samples and the risk monitoring of dietary health.