非水电位滴定法测定比沙可啶纯度及不确定度评定-中国药房.PDF

非水电位滴定法测定比沙可啶纯度及不确定度评定 ＊ 郭永辉 ，闫 凯，姜建国，韩学静（河北省药品检验研究院，石家庄 050011） 中图分类号 R917；R927.1 文献标志码 A 文章编号 1001-0408（2014）37-3510-03 DOI 10.6039/j.issn. 1001-0408.2014.37.18 摘 要 目的：建立非水电位滴定法测定比沙可啶纯度的不确定度评定方法。方法：对采用非水电位滴定法测定比沙可啶纯度过 程中引入的高氯酸滴定液浓度、方法重复性、仪器、比沙可啶摩尔质量、称量、滴定液消耗体积6个分量不确定度进行了系统分 析。结果：置信概率为95％时，采用非水电位滴定法测定比沙可啶纯度结果的标准值及其不确定度为99.82％±0.53％。其中滴 定液消耗体积、滴定液浓度和仪器不确定度3个分量对评定总不确定度贡献较大。结论：建立的非水电位滴定法不确定度评定结 果可靠，其结果有利于提高比沙可啶的质量评价与控制水平，同时为比沙可啶纯度标准物质的研制提供了科学依据。 关键词 比沙可啶；纯度；不确定度评定；非水电位滴定法 Purity Determination and Uncertainty Evaluation of Bisacodyl by Non-aqueous Electrolytic Titration GUO Yong-hui ，YAN Kai ，JIANG Jian-guo ，HAN Xue-jing （Hebei Institute for Drug Control ，Shijiazhuang 050011， China ） ABSTRACT OBJECTIVE ：To establish the non-aqueous titration method of uncertainty evaluation in purity determination of bi- sacodyl. METHODS ：Non-aqueous titration was selected for studying on valuation in purity determination of bisacodyl ，and the un- certainty of perchloric acid titration concentration ，method repeatability ，automatic potentiometric titration systematic deviation ，bi- sacodyl molar mass ，weighing and consumed titration volume in the determination was evaluated systematically. RESULTS ：When confidence probability was equal to 95％，the standard value and uncertainty of bisacodyl purity was 99.82％±0.53％. Those had significant impacts on uncertainty ，which were consumed titration volume and concentration and automatic potentiometric titrator systematic deviation. CONCLUSIONS ：Established non-aqueous titration method of uncertainty evaluation is reliable and helpful to improve the quality evaluation and control of bisacodyl ，and provide scientific basis for the development of bisacodyl purity refer- ence materials. KEYWORDS Bisacodyl ；Purity ；Uncertainty ；Non-aqueous titration 比沙可啶原料药为2010年版《中国药典》（二部）收载的品