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,5μm)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.
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 volume500 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） were0.6%—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.
作者
王金成
樊芸
卢宪波
张海军
陈吉平
WANG Jincheng;FAN Yun;LU Xianbo;ZHANG Haijun;CHEN Jiping(Dalian Institute of Chemical Physics,the Chinese Academy of Sciences,Dalian,116023,China)
出处
《环境化学》
CAS
CSCD
北大核心
2018年第9期1987-1993,共7页
Environmental Chemistry
基金
农业部公益性行业科研专项(201503108)
国家自然科学基金青年基金(21507132)资助~~
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
polycyclic aromatic hydrocarbons
chlorinated polycyclic aromatic hydrocarbons
solid-phase extraction
high performance liquid chromatography
tap water
