气质联用法测定纺织品中的含氯农药残留  

Determination of chlorinated pesticide residues in textiles by GC-MS method

作　　者：洪华[1] 申晓萍[1] 王海英[2] 李培才[1] 任凤云[1] 高丽[1] 张瑞萍[3] 

机构地区：[1]南通出入境检验检疫局,江苏南通226004 [2]南京工业大学,江苏南京211800 [3]南通大学,江苏南通226007

出　　处：《印染》2013年第21期40-44,共5页China Dyeing and Finishing

基　　金：国家质检总局科技计划项目;计划编号:2011IK096

摘　　要：对纺织品中三种含氯有机农药（十氯酮、乙滴涕、碳氯灵）残留量的萃取和检测方法进行了研究,讨论了萃取时间、温度、溶剂、萃取方式对回收率和精密度的影响.试验结果表明,水浴振荡萃取回收率要优于超声萃取和索氏萃取,在萃取条件为时间45 min、温度35℃、萃取溶剂为乙酸乙酯时,有最高回收率.气相色谱～质谱联用技术可同时对这三种农药残留量进行定性与定量测定.十氯酮、乙滴涕、碳氯灵的最低检出限分别为0.1,0.02,0.06 mg/L.方法的准确度评定试验表明,在0.5 ～2.0 mg/kg的添加水平下,总体回收率为51.0％ ～ 98.0％,相对标准偏差为1.79％ ～ 7.47％.The extraction and detection methods for the residues of three chlorinated organic pesticides（telodrin,perthane and chlordecone） in textiles are studied.The effects of extraction time,temperature,solvent and extraction methods on the recoveries are discussed.The results show that the recovery of bath oscillation extraction method is better than those of ultrasonic extraction method and soxhlet extraction method.The highest recovery rate can be obtained when extracting at 35 ℃ for 45 min with ethyl acetate as a solvent.Qualitative and quantitative determination of three pesticide residues can be carried out at the same time with the gas chromatography-mass spectrometry technique.The detection limits of telodrin,perthane and chlordecone are 0.1,0.02,0.06 mg/L respectively.The accuracy assessment experiments show that the overall recovery rate is 51.0％ ～ 98.0％ and the relative standard deviation is 1.79 ％ ～ 7.47％ under the addition level of 0.5 ～ 2.0 mg/kg.

关 键 词：测试 十氯酮 乙滴涕 碳氯灵 残留量 萃取 纺织品 

分 类 号：O657.63[理学—分析化学] TS107[理学—化学]