HPLC-ELSD法与薄层色谱扫描法用于测定二硬脂酰磷脂酰胆碱有关物质的对比研究  

Comparative Study on The Related Substance of Distearoyl Phosphatidylcholineby HPLC-ELSD and TLC Scanning

作　　者：赵海云 王春芳 陈德俊 张丹丹 王松 李宁宁 刘文坤 Zhao Haiyun;Wang Chunfang;Chen Dejun;Zhang Dandan;Wang Song;Li Ningning;Liu Wenkun(Shandong Institute For Food and Drug Control,NMPA Key Laboratory for Research and Evaluation of Generic Drugs,ShandongResearch Center of Engineering and Technology for Consistency Evaluation of Generic Drugs,Jinan 250101,China;Shandong Center For Food and Drug Evaluation&Inspection,Jinan 250013,China)

机构地区：[1]山东省食品药品检验研究院,国家药品监督管理局仿制药研究与评价重点实验室,山东省仿制药一致性评价工程技术研究中心,山东济南250101 [2]山东省食品药品审评查验中心,山东济南250013

出　　处：《广东化工》2024年第18期164-166,221,共4页Guangdong Chemical Industry

基　　金：2018年国家药品药用辅料标准提高项目(2018Y032)。

摘　　要：目的:建立二硬脂酰磷脂酰胆碱有关物质的检测方法。方法:对比考察HPLC-ELSD液相色谱法与薄层色谱扫描法。薄层色谱扫描法,采用硅胶G60薄层板,以三氯甲烷-甲醇-水-浓氨溶液(65∶25∶4∶0.4)为展开剂,检测波长为450 nm。液相色谱法采用C8柱,以甲醇和水为流动相,梯度洗脱,蒸发光散射检测器,以浓度的对数值为横坐标,以峰面积的对数值为纵坐标,进行线性回归计算,并对建立的方法进行了方法学验证。结果:薄层色谱扫描法虽也可定量,但仅检出少量已知杂质,不能有效检出未知杂质。液相色谱法所需样品量少、杂质检出量高、操作简便,优于薄层色谱扫描法。结论:建立方法采用液相色谱法克服了原有薄层色谱法不能准确定量的弊端,检测灵敏度高,定值准确,可作为二硬脂酰磷脂酰胆碱质量控制方法。Objective:To establish a method of related substance in Distearoyl Phosphatidylcholine.Methods:Compared between TLC scanning and HPLC-ELSD.The TLC separation was achieved using a silica gel G60 plate,trichloromethane-methanol-water-ammonia(65∶25∶4∶0.4)as the developing agent,detection wavelength was 450 nm.The HPLC separation was achieved using a C8 column,the mobile phase was composed of methanol and water with gradient elution,the detector was evaporative light-scattering detector.The logarithm of the concentration was the x-axis,The logarithm of area was the y-axis,performed linear regression calculations.Then verified the established method by methodology.Results:Only a small amount of known impurities were detected by TLC scanning,the unknown impurity couldn’t effectively detected.In the aspect of sample amount,the detection of impurity and operation convinence,HPLC-ELSD was superior to TLC scanning.Conclusion:The new HPLC-ELSD method with high sensitivity and accurate determination overcomes the shortcoming of the original method which cannot be accurately quantified,can be used as quality control method of distearoyl phosphatidylcholine.

关 键 词：二硬脂酰磷脂酰胆碱 脂质体 有关物质 高效液相色谱法 薄层色谱扫描法 

分 类 号：R917[医药卫生—药物分析学]