建立了一种毛细管电泳测定左旋多巴药片光学纯度的新方法.D,L-多巴(D,L-dopa)用2,4-二硝基氯苯(CDNB) 衍生,以β-环糊精(β-CD)为手性选择剂,在硼砂(pH 9.0)缓冲溶液中进行毛细管电泳手性分离.采用紫外检测,测定波长为220 nm.在测定条件下,对映体分离在9 min内完成.L-dopa中D-dopa的含量在0.10%~2.0%范围内,与D-dopa的峰面积呈现良好的线性关系.在L-dopa中加入不同量的D-dopa,测得回收率在96%~102% 之间,每个样品分别测定3次,其相对标准偏差(RSD)小于2.3%.方法用于市售左旋多巴药片的分析,测得左旋多巴药片中D-dopa的含量为0.20%.
A new capillary electrophoresis method was established for the optical purity analysis of levodopa. D,L-dopa was derivatized with 1-chloro-2,4-dinitrobenze (CDNB) and separated by capillary electrophoresis using β- cyclodextrin (β-CD) as chiral selector in a borate buffer at pH 9.0, followed by direct ultraviolet absorptive measurement at 220 nm. Under optimal conditions, enantiomeric separation of D, L-dopa was completed within less than 9 min, and the linear relationship between the peak area of D-dopa and the content of D-dopa in L-dopa was found in the range of 0. 10% -2.0%. The recovery for standard addition was estimated within the 96.0% - 102.0%. The relative standard deviation, for three independent analyses of each sample, was less than 2.3%. The presented method has been applied to the analysis of real levodopa drug, and allowed the determination of 0.20% D-dopa in levodopa with well peak identification.