快速溶剂萃取-气相色谱-质谱联用法测定土壤中菊酯类和八氯二丙醚  

Determination of pyrethroids and octachlorodipropyl ether in soil by gas chromatography-mass spectrometry with rapid solvent extraction

作　　者：乔淞汾 杨利娟 冉卓 秦冲 陈阳 刘爱琴 QIAO Songfen;YANG Lijuan;RAN Zhuo;QIN Chong;CHEN Yang;LIU Aiqin(Hebei Research Center for Geoanalysis,Hebei Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Baoding 071052,China)

机构地区：[1]河北省地质实验测试中心,河北省矿产资源与生态环境重点实验室,河北保定071052

出　　处：《化学分析计量》2024年第11期91-96,共6页Chemical Analysis And Meterage

摘　　要：建立了快速溶剂萃取-气相色谱质谱联用法测定土壤中6种菊酯类农药和八氯二丙醚的方法。以正己烷和丙酮(体积比为1∶1)混合溶剂作为萃取溶剂,在80℃,100MPa下循环萃取2次,萃取液经AN60C045型石墨化炭黑固相萃取小柱净化。采用气相色谱质谱联用法检测,载气为高纯氦气,进样口温度为240℃,柱流量为1.0mL/min,进样体积为1.0μL,离子源温度为230℃,以内标法定量。6种菊酯类和八氯二丙醚的质量浓度均在200~8000μg/L范围内与其色谱峰面积线性关系良好,相关系数均大于0.995,检出限为0.02~0.11mg/kg。样品平均回收率为78.08%~128.08%,测定结果的相对标准偏差为1.37%~9.08%(n=6)。该方法简单快捷、检出限低、准确度高,可用于土壤中菊酯类农药测定,为土壤管控提供参考。A rapid solvent extraction and gas chromatography-mass spectrometry method was established for the determination of 6 pyrethroids and octachlorodipropyl ether in soil.A mixture of n-hexane and acetone(volume ratio of 1∶1)was used as extraction solvent,and the samples were extracted twice at 80℃and 100 MPa.The extraction liquid was purified by AN60C045 graphitized carbon black solid phase extraction column.The carrier gas was high purity helium,the inlet temperature was 240℃,the column flow rate was 1.0 mL/min,the sample volume was 1.0μL,the ion source temperature was 230℃,and the quantity was determined by internal standard method.The concentrations of six pyrethroids and octachlorodipropyl ether ranged from 200-8000μg/L and showed good linear relationships with their chromatographic peak areas,and the correlation coefficients were all greater than 0.995.The limits of detection were 0.02-0.11 mg/kg.The average recoveries were 78.08%-128.08%,and the relative standard deviation was 1.37%-9.08%(n=6).The method is simple,rapid,low detection limit and high accuracy,and can be used for the determination of pyrethroids in soil,providing a reference for soil control.

关 键 词：快速溶剂萃取 气相色谱质谱联用法 土壤 菊酯类农药 八氯二丙醚 

分 类 号：O657.7[理学—分析化学]