气相色谱法测定水果中毒杀芬残留量的方法优化研究  

Study on Optimization of Gas Chromatography Method for Determination of Toxaphene Residue in Fruit

作　　者：潘利 段保屹 温家豪 易忠明 吕杨萍 张思琦 PAN Li;DUAN Baoyi;WEN Jiahao;YI Zhongming;LYU Yangping;ZHANG Siqi(Wuzhou Customs Integrated Technical Service Center,Wuzhou 543000,China;Pingxiang Customs Integrated Technical Service Center,Pingxiang 532600,China)

机构地区：[1]梧州海关综合技术服务中心,广西梧州543000 [2]凭祥海关综合技术服务中心,广西凭祥532600

出　　处：《食品安全导刊》2025年第5期95-98,102,共5页China Food Safety Magazine

摘　　要：目的:优化气相色谱法检测水果中毒杀芬残留量的方法。方法:优化样品前处理方法,摒弃索氏提取器净化提取方式,采用振荡提取法,提取液经无水硫酸钠干燥后过佛罗里硅层析柱进行净化。采用HP-5毛细管色谱柱进行分离,电子捕获检测器检测,外标法定量。结果:毒杀芬在0.1~2.0μg·m L^(-1)线性关系良好,相关系数R≥0.996,方法定量限为0.02 mg·kg^(-1)。3个加标水平的平均回收率在64.2%~115.0%,相对标准偏差≤6.8%。结论:该方法灵敏、准确,可以满足水果中毒杀芬残留量检测的要求。Objective:To optimize the method for the determination of toxaphene residue in fruit by gas chromatography.Method:The sample pretreatment method was optimized and the extraction method was abandoned by Soxhlet extractor.The extraction solution was purified by oscillating extraction method and dried by anhydrous sodium sulfate and then purified by Flori silicon chromatography column.Separation was performed by HP-5 capillary chromatography column,detected by electron capture detector,and quantified by external standard method.Result:Toxaphene showed a good linear relationship between 0.1μg·mL^(-1)and 2.0μg·mL^(-1),with a correlation coefficient R≥0.996.The detection limit of the method was 0.02 mg·kg^(-1).The average recovery rate of the three spiked levels is between 64.2%and 115.0%,with a relative standard deviation of≤6.8%.Conclusion:The method is sensitive and accurate,and can meet the requirements of the detection of toxaphene residue in fruit.

关 键 词：气相色谱 毒杀芬 水果 

分 类 号：O657.71[理学—分析化学] TS255.7[理学—化学]