HPLC法测定卡左双多巴缓释片中的有关物质  

Determination of the Related Substances in Carbidopa and Levodopa Sustained-release Tablets by HPLC

作　　者：时晓燕 庞余江 朱志祥 潘增玉 张丽萍 冯中 SHI Xiaoyan;PANG Yujiang;ZHU Zhixiang;PAN Zengyu;ZHANG Liping;FENG Zhong(School of Medicine,Ocean University of China,Qingdao 266003;Pharmaceutical Internationalization Engineering Lab.of Shandong Province,Lunan Pharmaceutical Group Co.,Ltd.,Linyi 273400)

机构地区：[1]中国海洋大学医药学院,山东青岛266003 [2]鲁南制药集团股份有限公司,山东省药物国际化工程实验室,山东临沂273400

出　　处：《中国医药工业杂志》2024年第2期275-282,共8页Chinese Journal of Pharmaceuticals

基　　金：基于抗肿瘤/心血管药物结晶与晶型控制的共性关键技术创新与产业化,山东省重大科技创新工程(2020CXGC010506)。

摘　　要：建立了HPLC法测定卡左双多巴(左旋多巴-卡比多巴)缓释片中的有关物质。采用Waters X-Bridge C_(18)柱(4.6mm×250mm,5μm),以pH1.8的磷酸盐缓冲液为流动相A、pH 1.8的磷酸盐缓冲液和甲醇(体积比250∶750)为流动相B,梯度洗脱。流速为1.0 mL/min,检测波长为280 nm,柱温为25℃,进样量为20μL。结果显示,主峰及各杂质峰均能良好分离,卡比多巴、左旋多巴和7个有关物质的线性关系良好,7个有关物质的平均回收率(n=9)分别为98.97%、100.79%、102.69%、98.13%、102.34%、95.97%、100.80%。强制性降解试验结果显示,该方法可指示各条件下的降解产物。相较于美国药典收录的有关物质检测方法,该方法专属性高、简便耐用,可用于卡左双多巴缓释片的生产控制及稳定性样品测定。An HPLC method was established for the determination of the related substances in carbidopa and levodopa sustained-release tablets.The Waters X-Bridge C_(18)column(4.6 mm×250 mm,5μm)was used,and the analysis was carried out in the gradient elution mode with pH 1.8 phosphate buffer solution as mobile phase A,and pH 1.8 phosphate buffer solution-methanol(250∶750)as mobile phase B.The flow rate was 1.0 mL/min,the detection wavelength was 280 nm,the column temperature was 25℃,and the injection volume was 20μL.The results showed that the main peaks and related substance peaks could be well separated,and it was linear for carbidopa,levodopa,and the seven related substances.The average recoveries(n=9)of seven related substances were 98.97%,100.79%,102.69%,98.13%,102.34%,95.97%,and 100.80%,respectively.The results of the forced degradation tests showed that this method could indicate the degradation products under various conditions.This method has higher specificity,simplicity,and durability than the methods included in the USP 43.It can be used for the production control and stability sample determination of carbidopa and levodopa sustained release tablet.

关 键 词：卡左双多巴缓释片 卡比多巴 左旋多巴 高效液相色谱 有关物质 强制性降解 

分 类 号：R917[医药卫生—药物分析学]