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。
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 conditions. According to related standards,indium enthalpy change values,measurement repeatability,weighing process,instrument temperature 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）% measured by DSC. Weighing process,instrument temperature deviation and system software deviation had great effects on the total uncertainty. 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 control of the weighing process will help to improve the accuracy measured by DSC;and it provides a new analysis method for the determination of purity of bisacodyl.
出处
《中国药房》
CAS
北大核心
2015年第18期2581-2583,共3页
China Pharmacy
