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  

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

作　　者：王金朝[1,2] 曾苏[1] 王丹华 胡功允 

机构地区：[1]浙江大学药学院,浙江杭州310058 [2]浙江华海药业股份有限公司质量研究部,浙江台州317024

出　　处：《色谱》2009年第3期376-378,共3页Chinese Journal of Chromatography

基　　金：浙江省博士后科研择优资助项目(No.2007-bsh-33)

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(pH3.0)(体积比为58:42),流速1.0mL/min,检测波长241nm,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0.15～15.0mg/L范围内呈现良好的线性关系。方法的检出限为0.05mg/L,定量限为0.15mg/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。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.

关 键 词：高效液相色谱法 手性衍生试剂 柱前衍生化 Α-苯乙胺 光学纯度 

分 类 号：O658[理学—分析化学]