色谱

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万古霉素键合手性固定相高效液相色谱法直接分离泰妥拉唑对映体

关瑾1,2,杨晶1,毕玉金1,石爽2,李发美1

  

  1. 1.School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China; 2.School of Applied Chemistry, Shenyang Institute of Chemical Technology, Shenyang 110124, China

  • 收稿日期:2007-02-14 修回日期:2007-05-16 出版日期:2007-09-30 发布日期:1985-03-25
  • 通讯作者: 李发美

Chiral Separation of Tenatoprazole Enantiomers Using High Performance Liquid Chromatography on Vacomycin-Bonded Chiral Stationary Phase

GUAN Jin1,2, YANG Jing1, BI Yujin1, SHI Shuang2, LI Famei1

  

  1. 1.School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China; 2.School of Applied Chemistry, Shenyang Institute of Chemical Technology, Shenyang 110124, China

  • Received:2007-02-14 Revised:2007-05-16 Online:2007-09-30 Published:1985-03-25

摘要:

利用反相高效液相色谱法在大环抗生素类手性固定相万古霉素键合手性固定相(Chirobiotic V)上直接分离了泰妥拉唑对映体。考察了缓冲溶液的种类、浓度和pH值,有机改性剂的种类和浓度,柱长和柱温等对手性分离的影响。优化后的色谱条件为:Chirobiotic V色谱柱(150 mm×4.6 mm,5 μm),流动相为0.02 mol/L 醋酸铵缓冲液(pH 6.0)-四氢呋喃(体积比为93∶7),流速为0.5 mL/min,柱温为20 ℃,检测波长为306 nm。在此条件下泰妥拉唑对映体达到了基线分离,分离度达1.68;对映体保留时间的相对标准偏差分别为0.48%和0.49%(n=6),峰面积的相对标准偏差分别为0.45%和0.55%(n=6)。所建立的手性分离方法具有简便快速及重复性好等优点。

关键词: 高效液相色谱, 手性分离, 手性固定相, 泰妥拉唑对映体

Abstract:

Vacomycin-bonded chiral stationary phase was used for the direct chiral separation of tenatoprazole enantiomers using reversed-phase high performance liquid chromatography (HPLC). The influences of the kinds and concentration of buffer and organic modifier, the pH value of buffer, column length and column temperature on the separation were examined. The chiral HPLC method for the separation of tenatoprazole enantiomers on a Chirobiotic V column (150 mm×4.6 mm, 5 μm) was established with simplicity and good reproducibility using 0.02 mol/L ammonium acetate buffer (pH 6.0)-tetrahydrofuran (93∶7, v/v) as the mobile phase at a flow rate of 0.5 mL/min and 20 ℃. Under the above conditions, the enantiomers were separated on baseline with the resolution of 1.68. The relative standard deviations (RSDs) for the retention times of tenatoprazole enantiomers were 0.48% and 0.49% (n=6). The RSDs for the peak areas of tenatoprazole enantiomers were 0.45% and 0.55% (n=6).

Key words: chiral separation, chiral stationary phase, tenatoprazole enantiomers , high performance liquid chromatography (HPLC)