容量滴定法测定去羟肌苷含量的分析方法验证与认可

目的: 建立容量滴定法测定去羟肌苷的含量。方法: 采用非水溶液滴定法,以冰醋酸-醋酐混合溶液(4:1)为滴定介质,电位滴定指示终点,每次加液体积为0.05 mL,等当点突跃幅度EPC设定为30,进行含量测定,并对分析方法进行验证,具体阐述了容量滴定法的方法验证过程和验证结果的认可标准。结果: 去羟肌苷测定的成比例系统误差、额外系统误差及精密度均符合规范要求。结论: 本法经方法学验证,可用于去羟肌苷原料的含量测定。

Objective: To establish a volumetric titration method for determination of didanosine. Methods: The non-water determination method was established for the content of didanosine with 40 mL glacial acetic acid and 10 mL anhydride acetic acid as the titration medium,the end point was determined potentiometrically,the volume step was 0.05 mL and EPC was set at 30.The established method was used for content determination and the analytical method was verified.The procedures and approval criteria of volumetric titration for determination of didanosine was described in this article. Results: The good proportional systematic,the additional proportional systematic and the statistical error acquired in this method met the requirement of related standards. Conclusion: It is proved that the method can be applied for the determination of dianosine by the methodology validation.

[1] JIANG WM(蒋卫民).AIDS antivirus theray headway(艾滋病的抗病毒治疗进展)[J].Foreign Med:Microbiol Sect(国外医学:微生物分册),2000,23(1):215
[2] LU YW(卢云雯),CHEN FE(陈芬儿).Graphical synthetic routes of dideoxyinosine(去羟肌苷的化学合成路线图解)[J].Chin J Pharm(中国医药工业杂志),2002,33(6):310
[3] PATRICK YN.Update on HAART in HIV [J].J Hepatol,2005,44:S100
[4] ZHANG LQ(张龙琪),TONG ZW(童照威),SHI BN(师柏年),et al.Observation of the curative effects of didanosine/stavudine and nevirapine in HIV infected patients(去羟肌苷、司他夫定联合奈韦拉平治疗A IDS患者疗效观察)[J].Zhejiang J Integr Tradit Chin West Med(浙江中西医结合杂志),2010,20(5):287
[5] WS₁-(X -007) -2008Z National Standards(国家食品药品监督管理局药品标准)[S].2008
[6] USP 34-NF 29[S].2010:3072
[7] The International Pharmacopoeia[S].2014:874
[8] BP 2013[S].2013:1024
[9] Guidance on the Formalized Process of Setting Specification for Chemical Drugs(化学药物质量标准建立的规范化过程技术指导原则)[S].2005
[10] Guidance for Validation of Analytical Methods in the Quality Control of Chemical Drugs(化学药物质量控制分析方法验证技术指导原则)[S].2005
[11] European Directorate for the Quality of Medicines.Technical Guide for the Elaboration of Monographs 4th[S].2005:65