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目的建立蔬菜中三大类农药的固相萃取-双柱双检测器-同一升温程序下气相色谱同时测定法。方法样品经乙腈溶剂匀浆提取,Carb-NH2柱净化,样品间隔60 s进样2次,先经CP-Sil 5CB柱分离后进入NPD检测器进行有机磷和氨基甲酸酯类农药测定,然后经CP-Sil 24CB柱分离后进入ECD检测器进行有机氯和拟除虫菊酯测定,阳性样品双柱检测器端互换双柱验证。结果三大类农药在0.01μg/ml~2.0μg/ml范围内质量浓度与峰面积有良好的线性关系,方法检测限在0.0001 mg/kg~0.010 mg/kg,加标回收率在76%~124%之间,相对标准偏差(RSD)在0.95%~4.7%。结论该方法简便、快速,结果准确,能满足蔬菜中多种类农药残留同时分析的要求。
OBJECTIVE To establish a solid phase extraction and double column dual detector for three kinds of pesticides in vegetables - gas chromatography simultaneous determination method under the same temperature program. The samples were separated by acetonitrile solvent homogenization and purified on a Carb-NH2 column. The samples were injected twice at intervals of 60 s. The samples were separated by CP-Sil 5CB column and then entered the NPD detector for determination of organophosphorus and carbamate pesticides. CP-Sil 24CB column after separation into the ECD detector for organochlorine and pyrethroid determination of positive samples double-column detector exchange double-column verification. Results There was a good linear relationship between the mass concentration and the peak area of the three kinds of pesticides in the range of 0.01μg / ml ~ 2.0μg / ml. The detection limits were 0.0001 mg / kg ~ 0.010 mg / kg, the recoveries were in the range of 76% 124%, relative standard deviation (RSD) between 0.95% and 4.7%. Conclusion The method is simple, rapid and accurate. It can meet the requirement of simultaneous analysis of various pesticide residues in vegetables.