改进的五氟苄基溴衍生化反应测定水中酚类化合物  

Improved pentafluorobenzyl bromide derivatization reaction for determination of phenolic compounds in water

作　　者：崔君 顾华[1,3] 张强[1,2,3] CUI Jun;GU Hua;ZHANG Qiang(Shanghai Resources Environment Supervision and Inspection Center,Ministry of Land and Resource,Shanghai 200072;Shanghai Institute of Geological Prospecting Technology,Shanghai 200072;Shanghai Institute of Geological Survey,Shanghai 200072)

机构地区：[1]国土资源部上海资源环境监督检测中心,上海200072 [2]上海市地质勘查技术研究院,上海200072 [3]上海市地质调查研究院,上海200072

出　　处：《分析试验室》2021年第1期54-58,共5页Chinese Journal of Analysis Laboratory

基　　金：国家地下水监测工程运行维护与地下水质监测(上海市部分)项目资助。

摘　　要：建立了气相色谱-质谱法测定水中6种酚类化合物(2,6-二氯酚、2,4-二氯酚、2,4,6-三氯酚、2,4,5-三氯酚、2,3,4,6-四氯酚和五氯酚)的方法。样品经二氯甲烷-乙酸乙酯混合溶剂萃取后,用旋转蒸发浓缩至1 mL,加入五氟苄基溴进行改进版衍生化反应,产物用DB-5 mS毛细管柱分离,采用选择离子监测模式测定。酚类化合物的检出限在0.05~0.13μg/L之间。目标物在0.05~1 mg/L范围内线性关系良好,相关系数R^(2)为0.9972~0.9983。以地下水水样为基体,加入3个浓度水平的标准溶液进行加标回收实验,加标回收率在60.4%~109.6%,相对标准偏差在0.1%~12%之间。A gas chromatography-mass spectrometry method for the determination of six phenolic compounds(2,6-dichlorophenol,2,4-dichlorophenol,2,4,6-trichlorophenol,2,4,5-trichlorophenol,2,3,4,6-tetrachlorophenol,pentachlorophenol)was developed.The sample was extracted via a mixed solvent of dichloromethane/ethyl acetate,and concentrated to 1 m L using a Rocket rotary evaporator.Subsequently,pentafluorobenzyl bromide was added to perform the optimized derivatization reaction.The product was separated by a DB-5 MS capillary column.The selective ion detection mode was used.The detection limits of the phenolic compounds were between 0.05 and 0.13μg/L.The targets had satisfied linear relationships in the range of0.05-1 mg/L,and the correlation coefficients(R^(2))were 0.9972-0.9983.Taking the groundwater sample as the matrix,adding the standard solutions with 3 concentration levels,the recovery results were 60.4%-109.6%,and the relative standard deviations were 0.1%-12%.

关 键 词：酚类化合物 气相色谱-质谱法 五氟苄基溴 

分 类 号：O657.71[理学—分析化学]