固相萃取-气相色谱质谱联用技术测定水中7种多溴联苯醚  

Determination of Seven Polybrominated Diphenyl Ethers in Water Using Solid-phase Extraction-gas Chromatography-mass Spectrometry Technology

作　　者：李敬超 张厚勇 葛璇 张恒 张翰林 刘雷[1] Li Jingchao;Zhang Houyong;Ge Xuan;Zhang Heng;Zhang Hanlin;Liu Lei(School of Municipal and Environmental Engineering,Shandong Jianzhu University,Shandong,250000;Shandong Ji'nan Ecological Environment Monitoring Center,Shandong,250000)

机构地区：[1]山东建筑大学市政与环境工程学院,山东250000 [2]山东省济南生态环境监测中心,山东250000

出　　处：《当代化工研究》2024年第9期44-47,共4页Modern Chemical Research

摘　　要：鉴于多溴联苯醚的广泛使用和生物毒性,建立了水中7种多溴联苯醚的固相萃取-气相色谱质谱检测方法。水样经过手动固相萃取仪富集,以C18柱为萃取柱,调节水样pH为3.0~4.0,用30 mL正己烷/二氯甲烷(3:1)混合溶液为洗脱剂,分三次洗脱,用气质联用仪检测。7种多溴联苯醚在0.0~1.25μg/L范围内线性良好,标准曲线的相关系数均大于0.99。该方法检出限为0.16~0.52 ng/L,在低、中、高3个加标浓度水平下,不同水体中7种多溴联苯醚的加标回收率为88.2%~116.3%,相对标准偏差为1.3%~9.8%,满足分析要求。In view of the widespread use and biological toxicity of polybrominated diphenyl ethers,a solid-phase extraction-gas chromatography mass spectrometry detection method for seven polybrominated diphenyl ethers in water was established.The water sample was enriched by a manual solid-phase extraction instrument.A C18 column was used as the extraction column.The pH of the water sample was adjusted to 3.0~4.0.30 mL n-hexane/dichloromethane(3:1)mixed solution was used as the eluent and washed three times.Take off and detect by GC-MS.The seven polybrominated diphenyl ethers have good linearity in the range of 0.0~1.25μg/L,and the correlation coefficients of the standard curves are all greater than 0.99.The detection limit of this method is 0.16~0.52 ng/L.At the three spike concentration levels of low,medium and high,the spike recovery rate of 7 kinds of polybrominated diphenyl ethers in different water bodies is 88.2%~116.3%,and the relative standard deviation is 1.3%~9.8%,meet-ing the analysis requirements.

关 键 词：多溴联苯醚 气相色谱质谱法 固相萃取 环境水 

分 类 号：X830-2[环境科学与工程—环境工程]