柱前衍生化RP-HPLC测定L-去甲麻黄碱盐酸盐光学杂质  

Determination of Optical Impurity in L-Norephedrine Hydrochloride by RP-HPLC with Pre-Column Derivatizatio

作　　者：王金朝[1,2] 胡功允 曾苏[1] 

机构地区：[1]浙江大学药学院,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：《中国药学杂志》2009年第16期1266-1268,共3页Chinese Pharmaceutical Journal

基　　金：浙江省博士后择优资助项目(#2007-bsh-33)

摘　　要：目的采用柱前手性试剂衍生化反相高效液相色谱法测定L-去甲麻黄碱盐酸盐的光学纯度。方法采用手性衍生化试剂2,3,4,6-四乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯(GITC)对样品L-去甲麻黄碱盐酸盐进行柱前衍生化。衍生产物以乙腈-0.01mol.L-1磷酸二氢钾缓冲液(pH3.0)(40∶60)为流动相,在Agilent Zorbax C18(4.6mm×250mm,5μm)色谱柱上进行分离,流速为1.0mL.min-1,检测波长为210nm,柱温为30℃。结果D-去甲麻黄碱盐酸盐在0.3～5.0mg.L-1内线性关系良好,最低定量下限为0.3mg.L-1,平均回收率为98.0%,日内日间精密度考察中RSD均小于5.0%。结论该方法操作简便,衍生化产物稳定,结果准确,重现性好,灵敏度高,可用于L-去甲麻黄碱盐酸盐光学纯度的检查控制。OBJECTIVE To establish a ehiral precolumn derivatization method for optical purity test of L-norephedrine hydrochloride. METHODS The enantiomers of norephedrine hydrochloride were derivatized with a pre-column chiral derivatization reagent 2, 3, 4, 6-tetra-O-acetyl-β-D-glucopyranosyl -isothiocyanate （GITC）. The diastereoisomers produced were separated on an Agilent Zorbax C18 column （4.6 mm × 250 mm, 5 μm） with a mobile phase consisting of acetonitrile -0.01 mol·L^-1 phosphate buffer （pH 3.0） （40 ： 60）. The flow rate was set at 1.0 mL·min^-1 and the detection wavelength was set at 210 nm. RESULTS The method was linear in the range of 0.3 5.0 mg·L^-1 for the D-norephedrine hydrochloride. The lower limit of detection for D-norephedrine hydrochloride was 0.1 mg·L^-1 and the lower limit of quantification was 0.3 mg·L^-1. The inter- and intra-day precision （RSD） was below 5.0% and the average recovery was 98.0%. CONCLUSION The method is simple, accurate and suitable for the quality control of optical purity of L-norephedrine hydrochloride.

关 键 词：去甲麻黄碱 光学杂质 高效液相色谱法 柱前衍生化 

分 类 号：R917[医药卫生—药物分析学]