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分散液液微萃取-柱前衍生-高效液相色谱法测定水样中双酚A
引用本文:李鱼,刘建林,翦英红.分散液液微萃取-柱前衍生-高效液相色谱法测定水样中双酚A[J].分析化学,2009,37(10).
作者姓名:李鱼  刘建林  翦英红
作者单位:1. 华北电力大学能源与环境研究中心,北京,102206;吉林大学环境与资源学院,长春,130012
2. 华北电力大学能源与环境研究中心,北京,102206
3. 吉林大学环境与资源学院,长春,130012
基金项目:国家"973"计划项目 
摘    要:建立了分散液液微萃取-柱前衍生-高效液相色谱法测定水样中双酚A的分析方法.通过交互正交试验和混合型优化实验设计对影响因素(萃取剂体积、分散剂类型及其体积、水样体积、pH值及离子强度)进行了优化.优化后的分散液液微萃取条件为:60 μL萃取剂,0.4 mL分散剂(甲醇),pH 4.0;优化后的柱前衍生化条件:0.1 mL 2.0 g/L衍生剂(对硝基苯甲酰氯)、衍生化时间30 min;方法的线性范围:0.002~0.2 mg/L(r=0.9997),检出限0.007 μg/L(S/N=3);不同浓度双酚A的萃取率为59.0%~63.0%,相对标准偏差(RSD)2.5%~9.2%(n=5);水样中双酚A的加标率为86.5%~107.1%,RSD为4.0%~11.9%(n=5),其它雌激素(雌酮、雌二醇、雌三醇和17α-乙炔基雌二醇)对双酚A的测定无干扰.本方法可以对水环境中的痕量BPA进行检测,具有操作简便、快速等优点.

关 键 词:分散液液微萃取  柱前衍生  高效液相色谱  双酚A

Combination of Dispersive Liquid-Liquid Microextraction and Pre-column Derivatization-High Performance Liquid Chromatography for Determination of Bisphenol A in Water Sample
LI Yu,LIU Jian-Lin,JIAN Ying-Hong.Combination of Dispersive Liquid-Liquid Microextraction and Pre-column Derivatization-High Performance Liquid Chromatography for Determination of Bisphenol A in Water Sample[J].Chinese Journal of Analytical Chemistry,2009,37(10).
Authors:LI Yu  LIU Jian-Lin  JIAN Ying-Hong
Institution:LI Yu1,2,LIU Jian-Lin1,JIAN Ying-Hong21(Energy and Environment Research Center,North China Electric Power University,Beijing 102206)2(College of Environment and Resources,Jilin University,Changchun 130012)
Abstract:An analytical method,dispersive liquid-liquid microextraction-pre-column derivatization-high performance liquid chromatography,was developed for the determination of bisphenol A(BPA) in water sample.Several factors,influencing the performance of dispersive liquid-liquid microextraction(DLLME) such as extractant volume,disperser type and volume,water volume,pH,and ionic strength,were studied and optimized using interactive orthogonal array and mixed level design experiments.The optimized dispersive liquid-li...
Keywords:Dispersive liquid-liquid microextraction  pre-column derivatization  high performance liquid chromatography  bisphenol A  
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