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

摘要

OBJECTIVE:To establish the purity determination of bisacodyl by differential scanning calorimetry(DSC)and the valuation of uncertainty. METHODS:DSC was conducted to detect the purity of bisacodyl and determine the optimal testing condi-tions. According to related standards,indium enthalpy change values,measurement repeatability,weighing process,instrument tem-perature deviation and system software deviation were systematically analyzed. The results were verified by HPLC. RESULTS:When the fiducial probability P was 0.95,the standard value and uncertainty of content of bisacodyl was (99.88 ± 0.06)% mea-sured by DSC. Weighing process,instrument temperature deviation and system software deviation had great effects on the total un-certainty. The result of HPLC and DSC were the same. CONCLUSIONS:The established DSC can quickly and accurately determine the chemical purity of bisacodyl. The uncertainty evaluation is reliable. Regularly calibrated and verificated equipment and strict con-trol of the weighing process will help to improve the accuracy measured by DSC;and it provides a new analysis method for the de-termination of purity of bisacodyl.%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。