差示扫描量热法测定比沙可啶原料药纯度及不确定度评定

发布时间：2018-07-24 16:08

【摘要】：目的:建立测定比沙可啶原料药纯度及不确定度评定的方法。方法:采用差示扫描量热(DSC)法对比沙可啶原料药纯度进行测定,确定最优检测条件;依据相关标准,对仪器校准铟标定焓变、测量重复性、称量过程、仪器温度偏差、系统软件偏差5个不确定度分量进行系统分析。采用高效液相色谱(HPLC)法对结果进行验证。结果:置信概率P为0.95时,采用DSC法测定比沙可啶原料药纯度结果的标准值及其不确定度为(99.88±0.06)%。其中称量过程、仪器温度偏差和系统软件偏差对总不确定度影响较大。DSC法与HPLC法测定结果一致。结论:所建立的DSC法可以快速、准确地测定比沙可啶原料药纯度,为其纯度测定提供了一种新的分析方法。DSC仪器的定期校准检定和称量过程的严格控制有利于提高DSC法测定的准确度。
[Abstract]:Objective: to establish a method for the determination of the purity and uncertainty of Bizacodine. Methods: using differential scanning calorimetry (DSC) to compare the purity of sackadine raw material to determine the optimal detection conditions, calibrating the indium enthalpy change, measuring repeatability, weighing process and instrument temperature deviation according to the relevant standards. The system software deviation is analyzed by 5 uncertainty components. The results were verified by high performance liquid chromatography (HPLC). Results: when the confidence probability P was 0. 95, the standard value and uncertainty of the determination of the purity of Bizacodine by DSC was (99.88 卤0.06). Among them, the weighing process, the temperature deviation of the instrument and the deviation of the system software have great influence on the total uncertainty. The results obtained by DSC method and HPLC method are in agreement with each other. Conclusion: the established DSC method can be used to determine the purity of Bizacodine. This paper provides a new analytical method for the determination of its purity. The periodic calibration and calibration of the DSC instrument and the strict control of the weighing process are helpful to improve the accuracy of the determination by the DSC method.
【作者单位】：河北省药品检验研究院;天津农学院基础科学系;
【分类号】：R927.1

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