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乙腈-硫酸铵-水双水相萃取-高效液相色谱法测定地下水中苯并(a)芘和苯并(e)芘
引用本文:王磊,安彩秀,朱裕穗,肖凡,刘金巍.乙腈-硫酸铵-水双水相萃取-高效液相色谱法测定地下水中苯并(a)芘和苯并(e)芘[J].岩矿测试,2013,32(2):325-329.
作者姓名:王磊  安彩秀  朱裕穗  肖凡  刘金巍
作者单位:1. 河北省地矿中心实验室,河北保定,071051
2. 中国地质调查局水文地质环境地质调查中心,河北保定,071051
基金项目:河北省地矿中心实验室技术创新项目(20110302)
摘    要:传统的液液萃取技术主要采用与水不相溶的有机溶剂作萃取剂,这种异相萃取的传质速率一般较低,需反复振荡或多次萃取.本文建立了以乙腈-硫酸铵-水的双水相萃取体系高效液相色谱法测定地下水中苯并(a)芘和苯并(e)芘的方法,以密度比水小的乙腈为萃取剂,将其与水样混合(互溶)获得乙腈-水体系,然后加入硫酸铵,溶液澄清、分相后取上层有机相(乙腈)进样分析.考察了萃取剂的选择、双水相的形成条件、离子强度以及pH等对测定结果的影响.两种化合物线性范围为2.00~ 400.00 ng/mL,相关系数大于0.999.方法检出限为0.012~0.020 ng/mL,平均回收率为94.6%~97.3%,相对标准偏差为1.3% ~2.5%.与传统萃取方法相比,该方法具有操作流程简单、快速的特点,可实现对野外环境水样进行原地样品前处理.

关 键 词:地下水  苯并(a)芘  苯并(e)芘  双水相体系  高效液相色谱法
收稿时间:2012/9/20 0:00:00
修稿时间:2012/12/6 0:00:00

Extraction and Detection of Benzo(a)pyrene and Benzo(e)pyrene in Groundwater Using Acetonitrile-(NH4)2SO4-Water System Coupled with Liquid Chromatography
WANG Lei,AN Cai-xiu,ZHU Yu-sui,XIAO Fan and LIU Jin-wei.Extraction and Detection of Benzo(a)pyrene and Benzo(e)pyrene in Groundwater Using Acetonitrile-(NH4)2SO4-Water System Coupled with Liquid Chromatography[J].Rock and Mineral Analysis,2013,32(2):325-329.
Authors:WANG Lei  AN Cai-xiu  ZHU Yu-sui  XIAO Fan and LIU Jin-wei
Institution:Hebei Province Geological and Mineral Center Laboratory, Baoding 071051, China;Hebei Province Geological and Mineral Center Laboratory, Baoding 071051, China;Hebei Province Geological and Mineral Center Laboratory, Baoding 071051, China;Hebei Province Geological and Mineral Center Laboratory, Baoding 071051, China;Centre for Hydrogeology and Environmental Geology Survey, Chinese Academy of Geological Sciences, Baoding 071051, China
Abstract:Conventional liquid-liquid extraction (LLE) methods usually use water immiscible organic solvents as the extraction solvents and achieve phase separation through repeated shock or multiple extractions. In this paper, a new method for the determination of benzo(a)pyrene and benzo(e)pyrene in groundwater by High Performance Liquid Chromatography (HPLC) with acetonitrile-(NH4)2SO4-water extraction system is described. In the proposed extraction procedure, a low-density extraction solvent (acetonitrile) was injected into a water sample to form the acetonitrile-water system. A salt (ammonium sulfate) was then injected into the acetonitrile-water solution to separate the system into two phases. The upper organic phase (acetonitrile) was collected and analyzed by HPLC. All the parameters, such as the selection of extraction agent, aqueous two phase formation conditions, ionic strength and pH, are discussed and optimized. The two kinds of compound are linear and in the range of 2.00-400.00 ng/mL, and the correlation coefficient (R2) is greater than 0.999. The detection limits of the method for the compounds ranged from 0.012-0.020 ng/mL and the average recoveries ranged from 94.6%-97.3% with precision of 1.3%-2.5%. Compared with conventional extraction methods, the method has the characteristics of simple operation and rapidity. Pretreatment of environmental water samples can be operated in the field, which is good for the routine analysis of benzo(a)pyrene and benzo(e)pyrene in groundwater.
Keywords:groundwater  benzo(a)pyrene  benzo(e)pyrene  aqueous two-phase system  High Performance Liquid Chromatography
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