磁固相萃取-高效液相色谱法测定环境水样中双酚A
HPLC Determination of Bisphenol A in Environmental Water Samples with Magnetic Solid Phase Extraction
摘 要
采用磁固相萃取-高效液相色谱法测定环境水样中双酚A的含量.优化的试验条件如下:① 50 mL水样中加入20 mg磁性微球进行萃取;② 水样的pH为3.0;③ 萃取时间为15 min;④ 解析溶剂为甲醇(80+20)溶液;⑤ 解析时间为10 min.采用C18色谱柱为分离柱,以甲醇-水(85+15)混合液为流动相,在检测波长224 nm处进行测定.双酚A的质量浓度在5.0~500 μg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)为1.0 μg·L-1.方法应用于环境水样的分析,加标回收率在81.4%~109%之间,测定值的相对标准偏差(n=6)在5.7%~8.6%之间.
磁固相萃取
双酚A
环境水样
HPLC
Magnetic solid phase extraction
Bisphenol A
Environmental water samples
Abstract
HPLC was applied to the determination of bisphenol A in environmental water samples with magnetic solid phase extraction. The optimized conditions found were as follows:① 50 mL water sample was extracted with 20 mg magnetic microsphere;② pH of water sample:3.0;③ time of extraction:15 min;④ desorption solution:methanol (80+20) solution;⑤ desorption time:10 min. The C18 chromatographic column was used as stationary phase,and a mixture of methanol and water (85+15) was used as mobile phase. UV-detection at 224 nm was adopted in the determination. Linear relationship between values of peak area and mass concentration of bisphenol A was kept in the range of 5.0-500 μg·L-1,with detection limit (3S/N) of 1.0 μg·L-1. The proposed method was applied to the analysis of environmental water samples,giving values of recovery and RSD′s (n=6) in the ranges of 81.4%-109% and 5.7%-8.6%,respectively.
中图分类号 O652.63
所属栏目 试验与研究
基金项目 浙江省环保科研计划项目(2011B01)资助
收稿日期 2014/2/27
修改稿日期
网络出版日期
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备注胡文凌(1981-),女,江西九江人,工程师,硕士,主要从事环境监测工作.
引用该论文: HU Wen-ling,ZHANG Jie,YU Wei-juan,PANG Ming,JIANG Ran-ran,CHEN Li-qun,JIANG Sheng-liang. HPLC Determination of Bisphenol A in Environmental Water Samples with Magnetic Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(2): 153～156
胡文凌,张杰,余卫娟,庞明,江冉冉,陈利群,江胜良. 磁固相萃取-高效液相色谱法测定环境水样中双酚A[J]. 理化检验－化学分册, 2015, 51(2): 153～156
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【3】朱俐,董慧茹,章晴,等.溶剂浮选-高效液相色谱法测定水体中双酚A、辛基酚和壬基酚[J].理化检验-化学分册,2010,46(2):167-169.
【4】谭小旺,宋燕西,魏瑞萍,等.三相中空纤维膜液相微萃取-高效液相色谱法测定水中痕量双酚A[J].分析化学,2012,40(9):1409-1414.
【5】吴科盛,许恒毅,郭亮,等.磁性固相萃取在检测分析中的应用研究进展[J].食品科学,2011,32(3):317-320.
【6】程桂红.磁固相萃取在痕量重金属分析中的应用[J].广东化工,2011,38(8):137-138.
【7】庞晋山,邓爱华,彭晓俊,等.磁性碳包铁纳米粒子在重金属元素检测分离富集中的应用[J].分析测试学报,2012,31(1):51-55.
【8】焦艳娜,丁利,刘锦霞,等.磁性Fe3O4亚微米球固相萃取-HPLC检测水中植物生长调节剂残留[J].化学研究与应用,2012,24(4):555-559.
【9】付善良,丁利,戴华,等.磁固相萃取/气相色谱-质谱法分析水样中的16种邻苯二甲酸酯类化合物[J].分析测试学报,2011,30(8):847-852.
【10】SULEIMA J S,HU Bin,PENG Han-yong,et al. Separation/preconcentration of trace amounts of Cr,Cu and Pb in environmental samples by magnetic solid-phase extraction with Bismuthiol-II-immobilized magnetic nanoparticles and their determination by ICP-OES[J]. Talanta,2009,77(5):1579-1583.
【11】FARAJI M,YAMINI Y,SALEH A,et al. A nanoparticle-based solid-phase extraction procedure followed by flow injection inductively coupled plasma-optical emission spectrometry to determine some heavy metal ions in water samples[J]. Analytica Chimica Acta,2010,659(1/2):172-177.
【12】李金峰,李颖,蒋原,等.C18键合磁珠固相萃取-液质联用检测蜂王浆中磺胺二甲嘧啶残留[J].安徽农业科学,2012,40(27):13586-13587.
【13】黄维,丁俊冯,钰锜.磁固相萃取-高效液相色谱联用测定尿样中的1-羟基芘[J].分析化学,2012,40(6):830-834.
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