ASE–GC–MS法同时测定农用地土壤中的多环芳烃、多氯联苯和有机氯农药  

Simultaneous determination of polycyclic aromatic hydrocarbons,polychlorinated biphenyls and organochlorine pesticides in soil by GC–MS coupled with accelerated solvent extraction

作　　者：吴亮 岳中慧 张皓 范鹏飞 朱姝 张鑫 WU Liang;YUE Zhonghui;ZHANG Hao;FAN Pengfei;ZHU Shu;ZHANG Xin(Research Institute No.230,CNNC,Changsha 410007,China)

机构地区：[1]核工业230研究所

出　　处：《化学分析计量》2019年第4期7-12,17,共7页Chemical Analysis And Meterage

基　　金：中国核工业地质局铀矿地质项目(201918)

摘　　要：建立同时检测农用地土壤中15种多环芳烃、7种多氯联苯和8种有机氯农药的方法,对样品前处理流程及仪器工作参数进行优化。样品经正己烷–二氯甲烷(1∶1)加速溶剂萃取,以硅酸镁小柱净化,二氯甲烷–正己烷(1∶4)洗脱,用气相色谱–质谱法同时测定。各目标化合物在质量浓度在5.0~500μg/L范围内相对响应因子的相对标准偏差均小于9.3%;平均加标回收率为60.3%~105.6%,相对标准偏差为1.7%~12.8%(n=6),方法检出限为0.12~0.40μg/kg。该方法快速、稳健,净化效果好,能满足农用地土壤中30种持久性有机污染物的检测要求。The method for simultaneous determination of 15 polycyclic aromatic hydrocarbons,7 polychlorinated biphenyls and 8 organochlorine pesticides in agricultural soil was established. Sample pretreatment process and working parameters were optimized. The sample was extracted with n-hexane–dichloromethane(1∶1) by accelerated solvent extraction,purified by magnesium silicate column and eluted by dichloromethane–n-hexane(1∶4),then simultaneously determined by gas chromatography–mass spectrometry. Experimental results showed that the relative deviations of relative response factors was less than 9.3% in the range of 5.0–500 μg/L while average recoveries of 30 compounds were 60.3%–105.6% with the relative standard deviations of 1.7%–12.8%(n=6). The detection limits ranged from 0.12μg/kg to 0.40 μg/kg. The method is proved to be efficient,robust and has good purification effect,it can be used for determination of 30 items of persistent organic pollutants in agricultural soil.

关 键 词：气相色谱-质谱法 农用土壤 多环芳烃 多氯联苯 有机氯农药 同时测定 加速溶剂萃取 

分 类 号：O657.7[理学—分析化学]