色谱

色谱

• 研究论文 • 上一篇    下一篇

微乳液相色谱法同时测定4种脂溶性维生素

杨建锐, 黄丽娜, 黄光亮, 李宁*   

  1. 广东药学院, 广东 广州 510006
  • 收稿日期:2011-04-11 修回日期:2011-07-03 出版日期:2011-10-28 发布日期:2011-10-13
  • 通讯作者: 李宁,副教授,从事药物分析及色谱学应用研究. Tel: (020)39352136,
  • 基金资助:
    国家自然科学基金项目(81173525).

Simultaneous determination of four fat-soluble vitamins by microemulsion liquid chromatography

YANG Jianrui, HUANG Lina, HUANG Guangliang, LI Ning*   

  1. Guangdong College of Pharmacy, Guangzhou 510006, China
  • Received:2011-04-11 Revised:2011-07-03 Online:2011-10-28 Published:2011-10-13

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摘要： 建立了一种新的微乳体系,并成功地应用于微乳液相色谱法(MELC)快速分析脂溶性维生素VA、VD2、VD3和VE。通过对影响分离选择性的主要因素进行考察,得到最佳微乳体系组成为98%(v/v)(50 g/L十二烷基硫酸钠(SDS)-10%(质量分数)正丁醇-1.0%(质量分数)正辛烷-84%水(质量分数))-2%(v/v)乙腈。该微乳体系中,表面活性剂类型和浓度、油相正辛烷的含量、有机添加剂乙腈对脂溶性维生素的分离起到了重要的作用。以Venusil ASB C18色谱柱(150 mm×4.6 mm, 5 μm)为分离柱,流速为0.7 mL/min,检测波长为265 nm,柱温为40 ℃, VA、VD2、VD3和VE在20 min内达到基线分离。4种脂溶性维生素的保留时间和峰面积的相对标准偏差(RSD) (n=5)分别小于2.3%和3.0%; VA、VD2、VD3和VE的线性范围分别为22.0～88.0 mg/L、20.2～81.0 mg/L、24.3～97.2 mg/L和125.0～500.0 mg/L,相应的线性相关系数r2分别为0.9996、0.9994、0.9998、0.9998;检出限(S/N=3)分别为0.37、0.34、0.41和2.12 mg/L。本方法已成功应用于多维元素片(21)中VA与VE的测定,结果令人满意。

关键词: 微乳流动相, 微乳液相色谱, 脂溶性维生素

Abstract: A novel system was developed for the rapid determination of fat-soluble vitamins A, D2, D3 and E with microemulsion liquid chromatography (MELC). The effects of operating parameters on the separation selectivity were investigated. The optimized microemulsion system consisted of 98%(v/v) of 50 g/L sodium dodecyl sulfate (SDS)-10%(w/w) n-butanol-1.0% (w/w) n-octane-84% water (w/w) and 2%(v/v) acetonitrile. The type and content of surfactant, the content of oil phase and the organic additive (acetonitrile) were found to play important roles in the separation of four fat-soluble vitamins. The four analytes were baseline separated within 20 min on a Venusil ASB C18 column (150 mm×4.6 mm, 5 μm) with a flow rate of 0.7 mL/min and the detection wavelength of 265 nm at 40 ℃. The relative standard derivations (RSDs, n=5) of retention times and peak areas of the analytes were less than 2.3% and 3.0%, respectively. The linear ranges of vitamins A, D2, D3 and E were 22.0~88.0 mg/L, 20.2~81.0 mg/L, 24.3~97.2 mg/L and 125.0~500.0 mg/L, with their correlation coefficients (r2) of 0.9996, 0.9994, 0.9998 and 0.9998, respectively. The detection limits (S/N=3) were 0.37, 0.34, 0.41 and 2.12 mg/L, respectively. This method was successfully applied to the determination of commercial Vitamins with Minerals Tablets (21), and the results were satisfactory.

Key words: fat-soluble vitamins, microemulsion mobile phase, microemulsion liquid chromatography (MELC)