引用本文:
王金成, 樊芸, 卢宪波, 张海军, 陈吉平. 固相萃取-高效液相色谱法同时测定自来水中氯代多环芳烃和多环芳烃[J]. 环境化学, 2018, 37(9): 1987-1993
WANG Jincheng, FAN Yun, LU Xianbo, ZHANG Haijun, CHEN Jiping. Solid-phase extraction combined with HPLC for the determination of chlorinated polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in tap water samples[J]. Environmental Chemistry, 2018, 37(9): 1987-1993

固相萃取-高效液相色谱法同时测定自来水中氯代多环芳烃和多环芳烃
王金成, 樊芸, 卢宪波, 张海军, 陈吉平
中国科学院大连化学物理研究所, 大连, 116023
摘要:
建立了自来水中6种氯代多环芳烃和15种多环芳烃的固相萃取-高效液相色谱荧光检测分析方法.500 mL水样过C18固相萃取柱富集,经6 mL的50%甲醇水溶液淋洗,10 mL二氯甲烷-正己烷(1:1)洗脱.目标化合物经色谱柱(SUPELCOSILTMLC-PAH柱,150 mm×4.6 mm, 5 μm)分离后,荧光检测,外标法定量.结果表明,21种目标化合物在线性范围内线性关系良好,相关系数均大于0.999;目标化合物的加标回收率为70%-98%,相对标准偏差(RSD)0.6%-8.8%;方法的检出限(LOD, S/N=3)为0.3-5.0 ng·L-1,定量限(LOQ,S/N=10)为1.1-16.7 ng·L-1.方法简便快速,可用于自来水中氯代多环芳烃和多环芳烃的检测.
关键词:    氯代多环芳烃    多环芳烃    固相萃取    高效液相色谱    自来水   
Solid-phase extraction combined with HPLC for the determination of chlorinated polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in tap water samples
WANG Jincheng, FAN Yun, LU Xianbo, ZHANG Haijun, CHEN Jiping
Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian, 116023, China
Abstract:
A novel method was developed for the determination of six chlorinated polycyclic aromatic hydrocarbons and fifteen polycyclic aromatic hydrocarbons in tap water samples, using solid-phase extraction coupled with high performance liquid chromatography with fluorescence detection. Extraction and cleanup of tap water samples were performed on a C18 solid-phase extraction cartridge. The optimal extraction parameters of solid-phase extraction were as follows:sampling volume 500 mL;washing solvent:6 mL 50% methanol; eluting solvent 10 mL n-hexane and dichloromethane (1:1, V/V).The separation of the target compounds was achieved on a SUPELCOSILTMLC-PAH column (150 mm×4.6 mm, 5 μm) with acetonitrile-water as mobile phase using gradient elution. Quantitative determination was achieved by external standard method. The correlation coefficients(r) were greater than 0.999 in the linear ranges of 21 target compounds. The average recoveries of target compounds were 70%-98% and the corresponding relative standard deviations (RSD, n=3) were 0.6%-8.8%. The limits of detection(LOD,S/N=3) and limits of quantification(LOQ,S/N=10)were in the range of 0.3-5.0 ng·L-1 and 1.1-16.7 ng·L-1. The proposed method is simple and fast. It can be applied for the rapid determination of chlorinated polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in tap water samples.
Key words:    polycyclic aromatic hydrocarbons    chlorinated polycyclic aromatic hydrocarbons    solid-phase extraction    high performance liquid chromatography    tap water   
收稿日期: 2017-11-07
基金项目: 农业部公益性行业科研专项(201503108)和国家自然科学基金青年基金(21507132)资助.
王金成,Tel:0411-84379972,E-mail:wangjincheng@dicp.ac.cn;陈吉平,Tel:0411-84379562,E-mail:chenjp@dicp.ac.cn
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