色谱

色谱

• 技术与应用 • 上一篇    下一篇

手性试剂柱前衍生化高效液相色谱法测定α-苯乙胺的光学纯度

王金朝1,2, 曾苏1, 王丹华2, 胡功允2*   

  1. 1.College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310058, China; 2.Department of Quality Research, Zhejiang Huahai Pharmaceutical Co., Ltd., Taizhou 317024, China
  • 收稿日期:2008-11-07 修回日期:2009-01-07 出版日期:2009-05-30 发布日期:1982-09-25
  • 通讯作者: 胡功允

Determination of optical purity of α-phenylethylamine by high performance liquid chromatography with pre-column derivatization

WANG Jinzhao1,2, ZENG Su1, WANG Danhua2, HU Gongyun2*   

  1. 1.College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310058, China; 2.Department of Quality Research, Zhejiang Huahai Pharmaceutical Co., Ltd., Taizhou 317024, China
  • Received:2008-11-07 Revised:2009-01-07 Online:2009-05-30 Published:1982-09-25
  • Contact: HU Gongyun

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929

被引次数

12

摘要： 建立了一种简便的手性试剂柱前衍生化反相高效液相色谱测定α-苯乙胺光学纯度的方法。采用2,3,4,6-四-O-β-D-吡喃葡萄糖异氰酸酯(GITC)对α-苯乙胺进行衍生化,优化了衍生化反应参数;使用Agilent Zorbax C18色谱柱分离衍生化产物,流动相为甲醇-磷酸盐缓冲溶液(pH 3.0)(体积比为58:42),流速1.0 mL/min,检测波长241 nm,柱温为30 ℃。实验结果表明,α-苯乙胺两个对映体的衍生化产物分离良好,在0.15～15.0 mg/L范围内呈现良好的线性关系。方法的检出限为0.05 mg/L,定量限为0.15 mg/L,日内和日间精密度考察中测定值的相对标准偏差(RSD)均小于0.5%。建立的方法适用于α-苯乙胺的质量控制。

关键词: α-苯乙胺, 高效液相色谱法, 光学纯度 , 手性衍生试剂, 柱前衍生化

Abstract: A simple pre-column derivatization-high performance liquid chromatographic (HPLC) method was established for the determination of optical purity of α-phenylethylamine. The enantiomers of α-phenylethylamine were derivatized with 2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl isothiocyanate (GITC). The resulted diastereoisomers were separated on an Agilent Zorbax C18 column (250 mm×4.6 mm, 5 μm) with a mobile phase of methanol-phosphate buffer (1.36 g/L aqueous solution of potassium dihydrogen phosphate, adjusted to pH 3.0 with concentrated phosphoric acid) (58:42, v/v). The flow rate was set at 1.0 mL/min and the detection wavelength was set at 241 nm. The method was linear from 0.15~15.0 mg/L for both enantiomers. The limit of detection and the limit of quantification were 0.05 mg/L and 0.15 mg/L, respectively. The relative standard deviations (RSDs) of inter- and intra-day determination were below 0.5%. The method is easy to handle, accurate, and suitable for the quality control of the optical purity of α-phenylethylamine.

Key words: chiral derivatization reagent, optical purity , pre-column derivatization, α-phenylethylamine, high performance liquid chromatography (HPLC)