微波辅助萃取-气相色谱-质谱法测定环境固体废物中多溴联苯和多溴联苯醚  

Determination of polybrominated biphenyls and polybrominated diphenyl ethers in environmental solid wastes by microwave assisted extraction gas chromatography-mass spectrometry

作　　者：孔维巍 KONG Weiwei(Institute of Geological Sciences of Jilin Province,Changchun 130012,Jilin)

机构地区：[1]吉林省地质科学研究所,吉林长春130022

出　　处：《吉林地质》2022年第1期72-78,共7页Jilin Geology

摘　　要：环境固体废物种类繁多,成分复杂。目前没有针对复杂环境固体废物出台相关检测标准。本文采用微波加速萃取体系提取,在国标GB/T37639—2019基础上,对样品的提取进行了筛选和优化;扩大了检测目标物的范围,从单一的塑料制品检测,扩大到树脂、橡胶等高分子固体废物。以丙酮-甲苯(体积比1∶1)为提取溶剂,微波萃取温度150℃,萃取时间30 min,提取效果最佳;采用气相色谱-质谱法,对多溴联苯及多溴联苯醚进行同时测定,建立了环境固体废物中多溴联苯及多溴联苯醚的分析测试方法。结果表明,方法的线性范围在0.5~100μg/mL之间,线性相关系数在0.999以上,检出限在0.02~2.41μg/g之间,回收率在81.2%~109.7%之间,相对标准偏差RSD在1.1%~5.8%之间。本方法前处理提取效率高,萃取时间短、溶剂用量少、灵敏度高,定性、定量分析准确可靠,分析时间短,可用于大批量环境固体废物样品的分析测定。There are many kinds of environmental solid wastes with complex components. At present, there is no relevant testing standard for solid waste in complex environment. In this paper, microwave accelerated extraction system is used for extraction. Based on the national standard GB/T37639—2019, the extraction of samples is screened and optimized to expand the scope of detection targets, from single detection of plastic products to polymer solid wastes such as resin and rubber. Using acetone toluene(volume ratio 1∶1) as extraction solvent, microwave extraction temperature 150℃, extraction time 30 min, the extraction effect was the best;18 kinds of polybrominated biphenyls and polybrominated diphenyl ethers were determined simultaneously by gas chromatography-mass spectrometry. An analytical method for polybrominated biphenyls and polybrominated diphenyl ethers in environmental solid waste was established. The results show that the linear range of the method is 0.5~100 μg/mL, the linear correlation coefficient is more than 0.999, and the detection limit is 0.02~2.41 μg/g, the recovery was 81.2%~109.7%, and the relative standard deviation RSD was 1.1%~5.8%. The method has the advantages of high pretreatment extraction efficiency, short extraction time, less solvent consumption, high sensitivity, accurate and reliable qualitative and quantitative analysis and short analysis time. It can be used for the analysis and determination of a large number of environmental solid waste samples.

关 键 词：固体废物 多溴联苯 多溴联苯醚 微波萃取 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学]