固相膜萃取/气相色谱-质谱法检测水体中痕量酚类化合物  

Determination of Trace Amounts of Phenol Compounds in Source Water by Solid Phase Membrane Extraction/Gas Chromatography-Mass Spectrometry

作　　者：金铎 麦锦欢 彭旭辉 罗丽春 关淑霞 赵志伟[1,2] 孙天一 李俊民[2] 

机构地区：[1]瀚蓝环境股份有限公司广东省城市水循环与水质安全保障技术企业重点实验室(产学研培育基地),广东佛山528200 [2]哈尔滨工业大学市政环境工程学院城市水资源与水环境国家重点实验室,黑龙江哈尔滨150090

出　　处：《分析测试学报》2015年第1期80-85,共6页Journal of Instrumental Analysis

基　　金：瀚蓝环境股份有限公司科技项目基金资助(JSB2013-08(06))

摘　　要：建立了固相膜萃取/气相色谱-质谱法同时测定水体中多种痕量酚类化合物的分析方法。采用固相膜萃取技术提取水中的痕量酚类化合物,对洗脱液种类、洗脱液体积、水样初始p H值和洗脱速率等萃取条件进行优化,并用DB-5MS色谱柱分离,气相色谱-质谱法（GC-MS/SIM）进行定量测定。实验结果表明,在pH2.0的初始条件下,选择10 m L乙酸乙酯-二氯甲烷混合溶液（体积比1∶1）作为洗脱剂,控制洗脱速率为1 m L/min时,酚类化合物的平均回收率高达82.3%-97.1%。在1-800μg/L质量浓度范围内,酚类化合物的峰面积与对应质量浓度呈良好线性关系,相关系数（r^2）均在0.996以上,检出限均不大于0.017μg/L,相对标准偏差（RSD,n=8）为1.6%-4.3%。将方法应用于我国北江流域水样检测,结果可靠。该方法萃取时间短、灵敏度和准确度高、简单易行,满足实际水体中对痕量酚类化合物的检测要求,可显著提高水中痕量酚类化合物的分析效率。A solid phase membrane extraction with gas chromatography-mass spectrometric（GC-MS） method was established for the simultaneous determination of various trace amounts of phenol compounds.The solid phase membrane extraction technology was developed to extract trace amounts of phenol compounds in raw water.Some factors influencing the extraction efficiency of solid phase membrane,including type of eluent,elution volume,initial pH and elution rate were optimized.The separation was performed on a DB-5MS column.Gas chromatography-mass spectrometry（GC-MS） was used to quantitatively analyze the target compounds.The experimental results indicated that with the initial pH value of 2.0 and the elution rate of 1 mL/min,selecting 10 mL dichloromethane-ethyl acetate（1∶1） as extraction eluent,the average recoveries could reach to 82.3%-97.1%.In the optimal conditions,the calibration curves were linear between peak areas and mass concentrations of phenol compounds in the range of 1- 800 μg/L,with correlation coefficients（r^2） more than 0.996.The limits of detection（MLD） of phenol compounds were not more than 0.017 μg/L.The precision of the method is high,with relative standard deviations（RSD,n=8） of 1.6%-4.3%.The method was successfully applied in the analysis of trace phenol compounds in water samples collected from the Beijiang River,China.With the advantages of short extraction time,sensitivity,accurancy and simplicity,the method could meet the requirements for the detection of trace phenol compounds in raw water and could significantly improve the efficiency in the analysis of phenol compounds.

关 键 词：固相膜萃取 气相色谱-质谱法(GC-MS) 酚类化合物 痕量 

分 类 号：O657.72[理学—分析化学] TQ572.48[理学—化学]