色谱

色谱 ›› 2014, Vol. 32 ›› Issue (2): 194-197.DOI: 10.3724/SP.J.1123.2013.09048

• 技术与应用 • 上一篇    下一篇

基于溶胶凝胶技术的在线固相萃取与高效液相色谱联用测定饮用水中的雌激素残留

李龙飞, 苏敏, 石晓蕾, 王亚娜, 王玟玟, 何金兴   

  1. 齐鲁工业大学食品与生物工程学院, 山东 济南 250353
  • 收稿日期:2013-09-29 修回日期:2013-11-27 出版日期:2014-02-08 发布日期:2014-01-25
  • 通讯作者: 何金兴
  • 基金资助:

    国家自然科学基金项目(31301470)；山东省优秀中青年科学家科研奖励基金项目(BS2012SW018).

Determination of estrogen residues in drinking water by on-line solid phase extraction based on sol-gel technique coupled with high performance liquid chromatography

LI Longfei, SU Min, SHI Xiaolei, WANG Yana, WANG Minmin, HE Jinxing   

  1. College of Food and Biological Engineering, Qilu University of Technology, Jinan 250353, China
  • Received:2013-09-29 Revised:2013-11-27 Online:2014-02-08 Published:2014-01-25

PDF

486

被引次数

12

摘要：

建立了固相萃取与高效液相色谱在线联用测定水样中3种雌激素(己烯雌酚、己烷雌酚、双烯雌酚)痕量残留的方法。以溶胶凝胶技术合成的聚合物为固相萃取材料，对水样中的雌激素进行萃取富集，考察了样品溶液不同pH、上样流速及洗脱溶剂等条件对合成材料富集效果的影响。结果表明，在优化的条件下，该方法对3种雌激素的检出限(S/N=3)为0.07~0.13 μg/L，样品中的加标回收率为82.31%~99.43%，相对标准偏差(RSD)为1.61%~7.15%。方法简便可靠，适用于饮用水中雌激素的痕量残留检测。

关键词: 雌激素, 高效液相色谱, 饮用水, 在线固相萃取

Abstract:

A method for the determination of diethylstilbestrol (DES), hexestrol (HEX) and dienestrol (DS) residues in drinking water was established by on-line solid phase extraction (SPE) coupled with high performance liquid chromatography (HPLC). The material synthesized on the base of sol-gel technology was employed as adsorbent. This material was prepared using 3-aminopropyltriethoxysilane (APTES) as the functional monomer, tetraethoxysilane (TEOS) as the crosslinking agent, and acetic acid as the initiator. The synthesized adsorbent showed outstanding property for the estrogen extraction. The estrogen can be caught effectively from water samples and the extraction can be achieved rapidly. Some important parameters, such as pH of sample solution, eluent solvents, loading flow rate, which might influence extraction efficiency, were optimized. The results indicated that the limit of detection (S/N=3) of the developed method could reach 0.07-0.13 μg/L under the conditions of pH 7.0 of sample solution, methanol and 1% (v/v) acetic acid aqueous solution as the eluent solvent and the loading flow rate of 2 mL/min. The recoveries of the three estrogens from the water samples at three spiked levels ranged from 82.31% to 99.43% with RSD of 1.61%-7.15%. The method was simple, rapid, and suitable to detect the trace residues of estrogens in drinking water.

Key words: drinking water, estrogens, high performance liquid chromatography (HPLC), on-line solid phase extraction

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