四川农业大学学报 ›› 2014, Vol. 32 ›› Issue (02): 218-223.doi: 10.3969/j.issn.1000-2650.2014.02.016

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固相萃取-高效液相色谱法同时测定饲料中的3种雌激素

刘玲利1, 肖全伟2, 梁润2, 万渝平2, 曾英1, 吴文林2   

  1. 1. 成都理工大学材料与化学化工学院, 成都 610059;
    2. 成都市产品质量监督检验院食品中心, 成都 610100
  • 收稿日期:2014-04-14 出版日期:2014-06-30 发布日期:2017-02-28
  • 通讯作者: 肖全伟,博士,高级工程师,主要从事食品安全检测技术研究,E-mail:xqw66666@163.com。 E-mail:xqw66666@163.com
  • 作者简介:刘玲利,硕士研究生。
  • 基金资助:
    四川省科技基础条件平台建设专项

Simultaneous Determination of Three Estrogens in Feed by Solid Phase Extraction-High Performance Liquid Chromatography

LIU Ling-li1, XIAO Quan-wei2, LIANG Run2, WAN Yu-ping2, ZENG Ying1, WU Wen-lin2   

  1. 1. College of Material and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu 610059, China;
    2. Chengdu Product Quality Supervision and Inspection Institute, Chengdu 610100, China
  • Received:2014-04-14 Online:2014-06-30 Published:2017-02-28

摘要: [目的] 建立饲料中3种雌激素(17β-雌二醇、苯甲酸雌二醇和戊酸雌二醇)的固相萃取-高效液相色谱(SPEHPLC)测定方法。[方法] 饲料样品经甲醇+水提取,固相萃取柱净化,采用Dionex C18色谱柱,以乙腈和水为流动相进行梯度洗脱,流速1.0 mL/min,检测波长230 nm,柱温30℃。[结果] 3种雌激素的线性关系较好;检出限为0.5~1.0 mg/kg;平均回收率为89.3%~108.0%。[结论] SPE-HPLC法操作简便、线性范围宽、检出限低、准确度高,可同时测定饲料中3种雌激素的含量。

关键词: 17β-雌二醇, 苯甲酸雌二醇, 戊酸雌二醇, 固相萃取, 高效液相色谱法

Abstract: [Objective] Solid phase extraction-high performance liquid chromatography (SPEHPLC)method was established to determine three estrogens (17β-estradiol,estradiol benzoate,estradiol valerate)in feed simultaneously. [Method] Three estrogens were extracted by methanol/water,cleaned by SPE,and finally determined by high performance liquid chromatography (HPLC)which was performed on a Dionex C18 column with a mobile phase gradient elution (acetonitrile and water as mobile phases).The flow rate was 1.0 mL/min,the detection wavelength was 230 nm,and the column temperature was 30℃. [Results] The results revealed good linear responses of three estrogens,limit of detections were 0.5-1.0 mg/kg,and the average recovery ratio were 89.3%-108.0%. [Conclusion] The method can simultaneously determine three estrogens (17β-estradiol,estradiol benzoate,estradiol valerate)in feed with wide linear range,low detection limit and high accuracy.

Key words: 17β-estradiol, estradiol benzoate, estradiol valerate, solid phase extraction, high performance liquid chromatography

中图分类号: 

  • S-3