简易凝胶柱净化-气相色谱法检测动物源性 样品中残留的敌敌畏

Determination of dichlorvos in animal origin samples by gel purification column-gas chromatography

中文关键词:  敌敌畏  气相色谱法  凝胶净化柱  动物源样品

英文关键词:dichlorvos  gas chromatography  gel purification column  animal origin samples

中文摘要:

      目的 建立动物源样品中敌敌畏的简易凝胶色谱净化-气相色谱检测方法。方法 采用凝胶净化粉湿法装填于玻璃层析柱, 制成长约15 cm、直径1 cm的简易凝胶净化柱, 对样品的净化洗脱液进行分段收集, 分析其中敌敌畏回收率的规律。结果 最终确定4.6~25 mL体积段的洗脱液为敌敌畏的最佳洗脱体积段, 乙酸乙酯-环己烷(6:4, V:V)为最优配比的洗脱溶液, 凝胶柱装填3.00 g凝胶粉时净化效果最佳。选取猪肉、牛肉、鸡肉、鱼肉样品, 进行确证试验, 回收率和变异系数均满足精确度要求, 方法检出限为0.003 μg/mL, 加标回收率为88.2 %~100.7 %, 相对标准偏差为 0.4 %~1.2 %。结论 该方法快速、灵敏、准确, 适合动物源性食品中敌敌畏的测定。

英文摘要:

      Objective To develop a gel purification column-gas chromatography method to detect dichlorvos in animal origin samples. Method The simple gel purification column used for purifying the samples was made of glass column unit, filled with organic solvent and gel purification powder, and about 15 cm in length and 1 cm in diameter. The recoveries rule of dichlorvos in eluent was investigated by step-collection method. Results The optimum condition for the purification was 10~25 mL eluent volume segment, ethyl acetate and cyclohexane (6:4, V:V) as elution solution and 3.00 g gel purification powder as filler. The recoveries ranged 88.2%~100.7% in pork, beef, chicken and fish, with values of RSD (n=6) ranged 0.4 %~1.2 %, and the limit of detection was 0.003 μg/mL. Conclusion This method is quick, sensitive and accurate, which is suitable for determination of dichlorvos in animal origin samples.