摘要
目的建立气相色谱质谱法测定蔬菜中的21种有机磷类、氨基甲酸酯类和拟除虫菊酯类农药残留量的方法。方法样品经组织捣碎、乙腈提取、QuEChERS净化、正己烷定容,同时以环氧七氯为内标,配制成1.0μg/ml的混合标准工作液,采用GC-MS检测21种有机磷类、氨基甲酸酯类和拟除虫菊酯类农药。结果有机磷类农药的LOD为0.001 mg/kg^0.007 mg/kg,LOQ为0.003 mg/kg^0.021 mg/kg;氨基甲酸酯类农药的LOD为0.001 mg/kg^0.004 mg/kg,LOQ为0.003 mg/kg^0.012 mg/kg;拟除虫菊酯类农药的LOD为0.001 mg/kg^0.008 mg/kg,LOQ为0.003 mg/kg^0.024 mg/kg。平均加标回收率为61.9%~99.9%,相对标准偏差(RSD)为3.5%~15.0%。50份蔬菜样品中,毒死蜱检出2份,水胺硫磷检出1份,克百威检出3份,联苯菊酯检出2份,甲氰菊酯检出1份,氯氟氰菊酯检出12份,氟氯氰菊酯检出1份,氯氰菊酯检出7份,其余农药残留指标均未检出。结论该方法灵敏度高,回收率高,检出限低,符合分析要求,适合蔬菜中21种有机磷类、氨基甲酸酯类和拟除虫菊酯类农药残留检测的要求。
Objective To establish the QuEChERS-gas chromatography-mass spectrometry（ GC-MS） method for the residues determination of 21 organophosphorus,carbamate and pyrethroid pesticides in vegetables. Methods The samples were mashed and extracted with acetonitrile,purified by Qu ECh ERS,constanted volume with hexane. At the same time,the epoxy seven chlorine was used as internal standard to prepare the mixed standard working fluid formulated as 1. 0 μg/ml. 21 organophosphorus,carbamate and pyrethroid pesticides in the samples were detected by GC-MS. Results The LOD and LOQ of organophosphorus pesticides were within 0. 001 mg/kg-0. 007 mg/kg and 0. 003 mg/kg-0. 021 mg/kg,respectively. The LOD and LOQ of carbamate pesticides were within 0. 001 mg/kg-0. 004 mg/kg and 0. 003 mg/kg-0. 012 mg/kg,respectively.The LOD and LOQ of pyrethroid pesticides were within 0. 001 mg/kg-0. 008 mg/kg and 0. 003 mg/kg-0. 024 mg/kg,respectively. The average spiked recoveries were within 61. 9%-99. 9%,and the relative standard deviation（ RSD） was within3. 5%-15. 0%. Chlorpyrifos in 2 samples,optunal in 1 sample,carbamate in 3 samples,bifenthrin in 2 samples,fenpropathrin in 1 sample,cyhalothrin in 12 samples,cyfluthrin in 1 sample,cypermethrin in 7 samples were detected,and the remaining pesticide residues in the rest samples were not detected. Conclusion The method has high sensitivity,high recovery rate,low detection limit,and could met the requirement of the detection of 21 organophosphorus,carbamate and pyrethroid pesticides in vegetables.
出处
《中国卫生检验杂志》
CAS
2017年第15期2135-2139,共5页
Chinese Journal of Health Laboratory Technology
基金
江西省卫生计生委科技计划(20156070)
