气相色谱-质谱法测定土壤中多溴联苯  

Determination of Polybrominated Biphenyls in Soil Using Gas Chromatography-Mass Spectrometry

作　　者：吉义平 董静 宋洲 钟旭 罗火焰 周宇齐 Ji Yiping;Dong Jing;Song Zhou;Zhong Xu;Luo Huoyan;Zhou Yuqi(Hubei Province Geological Experimental Testing Center,Wuhan 430034;Hubei Huaxiang Geological Environmental Testing Technology Co.,Ltd.,Wuhan 430000;Hubei Key Laboratory of Resources and Eco-environment Geology(Hubei Geological Bureau),Wuhan 430034,China)

机构地区：[1]湖北省地质实验测试中心,湖北武汉430034 [2]湖北华祥地质环境检测科技有限公司,湖北武汉430000 [3]资源与生态环境地质湖北省重点实验室(湖北省地质局),湖北武汉430034

出　　处：《广东化工》2023年第10期191-194,共4页Guangdong Chemical Industry

基　　金：典型水生态环境监测关键技术研究与应用(KJ2021-18,KJ2022-36,KJ2023-39);土壤中溴代阻燃剂多溴联苯和多溴二苯醚的检测方法研究(CSZXKJ-202114)。

摘　　要：建立了气相色谱-质谱法同时测定土壤中一至十溴代多溴联苯(PBBs)的方法。对比研究了不同提取条件和净化条件对一至十溴代PBBs测定的影响。在优化的前处理条件下,PBBs在5~500μg/L(其中十溴联苯在50~5000μg/L)范围内线性关系良好,相关系数均大于0.999。当样品称样量为10 g时,一至九溴代PBBs的方法检出限为0.05~0.20μg/kg,十溴联苯为1.13μg/kg。在加标水平为1.0μg/kg、10.0μg/kg和40.0μg/kg时,PBBs的平均回收率在70.1%~111%之间,相对标准偏差(n=6)在0.91%~9.48%之间。采用该方法对实际土壤样品进行了检测,检出了6种PBBs,其浓度范围为0.068~1.765μg/kg。该方法准确、可靠、灵敏度高,能够满足实际土壤样品中一至十溴代PBBs的测试要求。A gas chromatography-mass spectrometry method for simultaneous determination of monobromo to decabromo polybrominated biphenyl(PBBs)in soil was developed.The effects of different extraction conditions and purification conditions were compared.Under appropriate pretreatment conditions,the linear relationship between monobromo to enobromide was good in the range of 5~500μg/L(decabromoide is 50~5000μg/L),and the correlation coefficients were greater than 0.999.When the sample weight was 10 g,the method detection limits were 0.05~0.20μg/kg for monobromo to enobromide PBBs and 1.13μg/kg for decabromoide.When the spiked levels were 1.0μg/kg,10.0μg/and 40.0μg/kg,the average recoveries ranged from 70.1%to 111%,and the relative standard deviations(n=6)ranged from 0.91%to 9.48%.The method was used to detect actual soil samples,and six target compounds were detected,with the concentration range of 0.068~1.765μg/kg.The method is accurate,reliable and sensitive,and can meet the test requirements of PBBs in actual soil samples.

关 键 词：气相色谱-质谱法 土壤 分析 多溴联苯 

分 类 号：O4[理学—物理]