色谱

色谱

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凝胶渗透色谱净化-高效液相色谱法测定鱼肉中的5种激素类药物残留

谢维平*, 欧阳燕玲, 黄盈煜, 陈春祝   

  1. 泉州市疾病预防控制中心理化检验科, 福建 泉州 362000
  • 收稿日期:2009-09-14 修回日期:2009-11-14 出版日期:2010-04-28 发布日期:1980-12-25
  • 通讯作者: 谢维平

Determination of five hormone drug residues in fish tissue by high performance liquid chromatography with gel permeation chromatographic clean-up

XIE Weiping*, OUYANG Yanling, HUANG Yingyu, CHEN Chunzhu   

  1. Department of Physical and Chemical Analysis, Quanzhou Center for Disease Control and Prevention, Quanzhou 362000, China
  • Received:2009-09-14 Revised:2009-11-14 Online:2010-04-28 Published:1980-12-25
  • Contact: XIE Weiping

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摘要： 建立了凝胶渗透色谱净化-高效液相色谱法测定鱼肉中己烯雌酚、雌二醇、炔雌醇、炔诺酮、炔诺孕酮5种激素类药物残留的方法。样品用乙酸乙酯-甲醇(8:2, v/v)溶液提取,提取液经Pharmadex LH-20凝胶柱(450 mm×15 mm)净化,并用甲醇-乙酸乙酯-乙酸(800:200:2, v/v/v)溶液洗脱。采用Agilent TC-C18柱(250 mm×4.6 mm, 5 μm)分离净化后的样品,用乙腈-水(45:55, v/v)溶液洗脱,流速为1.2 mL/min,双检测波长为245 nm和222 nm。5种激素类药物在0.05～2.5 mg/L范围内有良好的线性关系(r ＞0.999),检出限为10～24 μg/kg,平均加标回收率为60.1%～89.0%,相对标准偏差为2.0%～7.4%。该方法快速、简单,可应用于鱼肉中激素类药物残留量的检测。

关键词: 残留, 高效液相色谱, 激素类药物, 凝胶渗透色谱, 鱼肉

Abstract: A method was developed for the determination of five hormone residues in fish tissue by high performance liquid chromatography (HPLC) with gel permeation chromatographic (GPC) clean-up. The sample was extracted with ethyl acetate-methanol (8:2, v/v). The extract was cleaned-up on a Pharmadex LH-20 gel permeation column (450 mm×15 mm) and eluted with methanol-ethyl acetate-acetic acid (800:200:2, v/v/v). The analysis was performed on an Agilent TC-C18 column (250 mm×4.6 mm, 5 μm) using acetonitrile-water (45:55, v/v) as the mobile phase at a flow rate of 1.2 mL/min and the detection wavelengths were set at 222 nm and 245 nm. All of the 5 hormone residues had good linear relationships (r＞0.999) in the range of 0.05~2.5 mg/L. The limits of detection (LOD) were from 10 to 24 μg/kg. The average recoveries for all the five hormone residues were from 60.1% to 89.0%, with relative standard deviations (RSDs) from 2.0% to 7.4%. The method is simple, rapid, and can be applied for the analysis of the five hormone residues in fish tissue.

Key words: fish tissue , high performance liquid chromatography (HPLC), hormone drugs, residues, gel permeation chromatography (GPC)