江汉大学学报(自然科学版) ›› 2013, Vol. 41 ›› Issue (6): 31-33.

• 化学 • 上一篇    下一篇

HPLC法测定奶粉中痕量炔雌醇

谭芳,黄璐,郑琦,陈燃   

  1. 江汉大学 化学与环境工程学院,湖北 武汉 430056
  • 出版日期:2013-12-12 发布日期:2014-01-09
  • 作者简介:谭芳(1973—),女,实验师,硕士,研究方向:仪器分析教学与科研。
  • 基金资助:
    湖北省科技厅项目 (2011CDC130);武汉市科技局项目 (201220837304-3)

Determination on Residue of Ethinylestradiol in Powdered Milk with HPLC

TAN Fang,HUANG Lu,ZHENG Qi,CHEN Ran   

  1. School of Chemistry and Environmental Engineering,Jianghan University, Wuhan 430056,Hubei,China
  • Online:2013-12-12 Published:2014-01-09

摘要: 建立了高效液相色谱 (HPLC) 法测定奶粉中炔雌醇残留量的方法。样品以乙腈振荡萃取、离心,提取液浓缩后经0.45 μm滤膜过滤,冷冻去脂,进高效液相色谱仪分析。研究了萃取溶剂、萃取及浓缩方式对萃取效率的影响,确立了色谱检测条件。乙腈-水 (50∶50) 为流动相,流速1 mL/min,柱温30 ℃,检测波长224 nm。方法的检出限为16 μg/kg,加标回收率在86.5%~97.0%之间,工作曲线的相关系数为0.999 0,相对标准偏差为0.95%~2.01%(n=3)。方法快速、灵敏度高、分离效果好,样品处理简单、无杂质干扰,能够满足奶粉中雌激素分析的需要。

关键词: HPLC, 奶粉检测, 炔雌醇, 食品安全

Abstract: A method was developed for the determination of ethinylestradiol residue in powdered milk with HPLC. Samples were extracted with acetonitrile,contrifugated,the extract was filtrated with 0.45 μm filter membrane after being concentrated,freezed and degreased,then carried out HPLC analysis. Extraction solution,extraction method and HPLC condition were optimized. Used acetonitrile-water (50∶50)as the mobile phase,flowing speed was 1 mL/min,column temperature was 30℃,detective wavelength was 224 nm. The detection limit of the method was 16 μg/kg, the recovery was 86.5%-97.0%,the related coefficient of the working curve was 0.999 0,the relative standard deviation was 0.95%-2.01%(n = 3) . The method is rapid,sensitive,good seperation effect,simple,no disturbance from impurity,can meet the request of etinylestradiol dectection in powdered milk.

Key words: HPLC, detection on powdered milk, ethinylestradiol, food security

中图分类号: