Chinese Journal of Chromatography

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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

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)