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分散液相微萃取-高效液相色谱法测定水和土壤中多环芳烃
引用本文:叶朝霞,李莉,胡文凌,庞明,李蕾.分散液相微萃取-高效液相色谱法测定水和土壤中多环芳烃[J].理化检验(化学分册),2012(4):467-470.
作者姓名:叶朝霞  李莉  胡文凌  庞明  李蕾
作者单位:嘉兴市环境保护监测站;嘉兴学院生物与化学工程学院
摘    要:以二硫化碳为萃取剂,丙酮为分散剂对水样和土壤样中残留的多环芳烃进行分散液相微萃取。提取液供高效液相色谱仪的二极管阵列检测器和荧光检测器测定。选用LiChrospherPAH色谱柱作为固定相,用乙腈和水以不同比例混合的溶液作为流动相进行梯度淋洗。在优化的试验条件下,对合成水样中多环芳烃的富集倍数达220~560倍,16种多环芳烃可有效分离并测定。16种多环芳烃的检出限(3S/N)在0.002~0.05μg.L-1之间。用标准加入法测得回收率在64%~108%之间,测定值的相对标准偏差(n=7)在2.0%~7.8%之间。

关 键 词:高效液相色谱法  分散液相微萃取  多环芳烃  水样  土壤样

HPLC Determination of Polycyclic Aromatic Hydrocarbons in Water and Soil Samples with Dispersive Liquid Phase Micro-extraction
YE Zhao-xia,LI Li,HU Wen-ling,PANG Ming,LI Lei.HPLC Determination of Polycyclic Aromatic Hydrocarbons in Water and Soil Samples with Dispersive Liquid Phase Micro-extraction[J].Physical Testing and Chemical Analysis Part B:Chemical Analgsis,2012(4):467-470.
Authors:YE Zhao-xia  LI Li  HU Wen-ling  PANG Ming  LI Lei
Institution:1.Jiaxing Municipal Environmental Monitoring Station,Jiaxing 314000,China; 2.Dept.of Biology and Chemical Engineering,Jiaxing College,Jiaxing 314001,China)
Abstract:Residual amounts of polycyclic aromatic hydrocarbons(PAH′s) in samples of water and soil were extracted by dispersive liquid phase micro-extraction(DLPME) with CS2 as extraction solvent and acetone as dispersant.The eluate was used for HPLC analysis,and the detectors of DAD and FLD were adopted in the determination.LiChrospher PAH column was used as stationary phase and mixed solutions of acetonitrile and water with different mixing ratio were used as mobile phase in the gradient elution.Under the optimized conditions,the enrichment factors between 220-560 were achieved,and 16 PAH′s in water samples were clearly separated.Values of detection limit(3S/N) found were in the range of 0.002-0.05 μg·L-1.Values of recovery found by standard addition method were in the range of 64%-108% with RSD′s(n=7) in the range of 2.0%-7.8%.
Keywords:HPLC  Dispersive liquid phase micro-extraction  PHA′s  Water sample  Soil sample
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