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目的:建立固相萃取-气相色谱法测定蔬菜、水果中15种有机磷农药残留量的分析方法。方法:蔬菜、水果捣碎经乙腈提取,浓缩,CARB/NH2柱净化,丙酮溶解定容,用CP-SIL 24CB毛细管柱和TSD检测器测定。结果:相关系数为0.9966~0.9999,15种有机磷农药回收率加标0.080 mg/kg时,为80.0%~111.2%之间,加标0.20 mg/kg时,为85.0%~108.5%之间,加标4.00 mg/kg时,为97.2%~103.5%之间,变异系数RSD,加标4.00 mg/kg时,为2.21%~6.39%之间。结论:实验结果表明,在选定的色谱条件下,采用固相萃取-气相色谱法对蔬菜、水果中15种有机磷农药残留量进行测定。本法线性范围宽,线性良好,重现性好,回收率很高,能满足有机磷农药残留量测定,完全能够达到国家标准方法的要求。
Objective: To establish a method for the determination of 15 organophosphorus pesticide residues in vegetables and fruits by solid-phase extraction and gas chromatography. Methods: Vegetables and fruits were mashed and extracted with acetonitrile, concentrated, purified by CARB / NH2 column, and dissolved in acetone. The volume was determined by CP-SIL 24CB capillary column and TSD detector. Results: The correlation coefficients ranged from 0.9966 to 0.9999. The recoveries of 15 kinds of organophosphorus pesticides ranged from 80.0% to 111.2% with the standard addition of 0.080 mg / kg, and were between 85.0% and 108.5% at the standard addition of 0.20 mg / kg. When the standard addition of 4.00 mg / kg was between 97.2% and 103.5%, the coefficient of variation RSD was between 2.21% and 6.39% when the standard addition was 4.00 mg / kg. Conclusion: The experimental results show that 15 kinds of organophosphorus pesticide residues in vegetables and fruits are determined by solid-phase extraction and gas chromatography under the selected chromatographic conditions. The linear range of the law, good linearity, good reproducibility, high recovery, to meet the determination of organophosphorus pesticide residues, fully able to meet the requirements of the national standard methods.