江汉大学学报(自然科学版) ›› 2014, Vol. 42 ›› Issue (1): 55-58.

• 化学 • 上一篇    下一篇

SPE-HPLC法检测食品中多种痕量雌激素

黄璐,张勇民,郑琦*   

  1. 江汉大学 交叉学科研究院,湖北 武汉 430056
  • 出版日期:2014-02-25 发布日期:2014-04-14
  • 通讯作者: 郑琦
  • 作者简介:黄璐(1989—),女,硕士生,研究方向:化学工程。
  • 基金资助:
    湖北省科技厅项目(2011CDC130);武汉市科技局项目(201220837304-3)

Determination of Trace Estrogens in Food by SPE-HPLC

HUANG Lu,ZHANG Yong-min,ZHENG Qi   

  1. Institute for Interdisciplinary Research,Jianghan University,Wuhan 430056,Hubei,China
  • Online:2014-02-25 Published:2014-04-14
  • Contact: ZHENG Qi

摘要: 建立了固相萃取-高效液相色谱(SPE-HPLC)法同时测定食品中炔雌醇、己烯雌酚、壬基酚、苯甲酸雌二醇残留量的方法。样品以乙腈超声萃取、离心,提取液经C18固相萃取柱浓缩净化后,采用高效液相色谱仪进行分析。对固相萃取条件进行了优化,4种组分均得到了良好的分离,方法的检出限为6~12 μg/kg,加标回收率为80. 3%~107. 8%,工作曲线的相关系数为0. 998 8~0.999 8,相对标准偏差是0. 124%~1. 72%。结果表明,方法灵敏度高,分离效果好,样品处理简单、可减少杂质干扰,能够满足食品中雌激素分析的需要。

关键词: 固相萃取, 高效液相色谱法, 痕量雌激素, 食品检测

Abstract: The residues of Ethinylestradiol,Diethylstilbestrol,4-Nonylphenol and Estradiol benzoate in food were determined simultaneously by SPE-HPLC.The samples were ultrasonic extracted with acetonitrile,centrifuged,concentrated and purified by C18 solid phase extraction column,analyzed with the HPLC method. This study optimized the conditions of SPE,and four components were well separated. The detection limit of the method was ranged from 6 to 12 μg/kg. The recovery rates were 80. 3%~107. 8%. The calibration curves were linear with correlation coefficient ranged from 0.998 8 to 0.999 8. The relative standard deviations were 0. 124%~1. 72%. This method has high sensitivity,fine separability,simple sample preparation,and can reduce the inteference of impurities,which is satisfied with the estrogen analysis.

Key words: solid phase extraction, HPLC, trace estrogen, food detection

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