固相萃取结合气相色谱法测定蔬菜中33种有机磷农药的残留量

Determination of 33 organophosphorous pesticide residues in vegetables by GC-SPE

目的建立蔬菜中33种有机磷农药残留量的分析方法。方法蔬菜捣碎后经乙腈提取,盐析,浓缩,SPE柱净化,丙酮定容,采用DB-5MS毛细管柱和FPD检测器测定。可检测33种有机磷农药。结果 33种有机磷农药在40～800μg/L质量浓度范围内呈线性,相关系数(r)为0.998 8～0.999 9。加标回收率为73.1%～108.6%。相对标准偏差(RSD)为1.69%～8.39%。定量检出限3.5μg/kg。结论实验结果表明,在设定色谱条件下用全自动固相萃取仪净化后测定有机磷农药具有简便,快速,灵敏,准确的特点,能满足蔬菜中有机磷农药残留量的检测要求。

Objective To establish a method of determining 33 organophosphorous pesticide residues in vegetables.Methods Samples were detected by a FPD detector after extracted,salted-out,concentrated and purified with DB-5MS capillary column.Results There was a good linearity between the peak area and the concentration of residues within the mass concentration rang of 40-800 μg/L,the correlation coefficients were 0.998 8-0.999 9.The recoveries of standard addition were in the range of 73.1%-108.6% and the RSDs were in the range of 1.69%-8.39%.The detection limits were 3.5 μg/L.Conclusion The established method of determining 33 organophosphorous pesticide residues in vegetables was simple,fast,sensitive,high accuracy and precision.The method could meet the requirements for the determination of organophosphorous pesticide residues in vegetables.