盐酸羟苄唑原料含量测定方法的改进及不确定度分析
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摘要
目的:改进盐酸羟苄唑原料含量测定方法,并对拟修订方法进行不确定度评价。方法:采用电位滴定法进行测定,用醋酐替代醋酸汞;通过分析试验过程,确定不确定度来源,计算拟修订方法合成不确定度和扩展不确定度。结果:线性方程为Y=38.532 73X-0.017 10(r=1.000),取样量在0.068~0.42 g范围内,测定结果呈良好线性关系;拟修订方法与原标准测定结果无显著差异,新方法相对合成不确定度为0.19%,扩展不确定度为±0.38%。结论:拟修订方法简单、准确、低毒,可以替代现行标准方法检验盐酸羟苄唑原料含量。
Objective: To improve the determination method of Hydrobenzole Hydrochloride and evaluate the uncertainty. Method: Potentiometric titration method was used with acetic anhydride in place of mercury acetate. By analyzing the test process,the source of uncertainty of the proposed method was determined,the combined uncertainty and expanded uncertainty were calculated. Result: The linear equation was good in the range of 0. 068- 0. 42 g,Y = 38. 532 73X- 0. 017 10( r = 1. 000). There was no significant difference in the measurement sample between the revised standard and the original standard; the combined uncertainty was 0. 19% and the expanded uncertainty was ± 0. 38% for the new method. Conclusion: The revised method is simple,accurate and lower toxicity,which can be used to replace the original method for the determination of Hydrobenzole Hydrochloride.
Objective: To improve the determination method of Hydrobenzole Hydrochloride and evaluate the uncertainty. Method: Potentiometric titration method was used with acetic anhydride in place of mercury acetate. By analyzing the test process,the source of uncertainty of the proposed method was determined,the combined uncertainty and expanded uncertainty were calculated. Result: The linear equation was good in the range of 0. 068- 0. 42 g,Y = 38. 532 73X- 0. 017 10( r = 1. 000). There was no significant difference in the measurement sample between the revised standard and the original standard; the combined uncertainty was 0. 19% and the expanded uncertainty was ± 0. 38% for the new method. Conclusion: The revised method is simple,accurate and lower toxicity,which can be used to replace the original method for the determination of Hydrobenzole Hydrochloride.
引文
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[2]中国药典[S].2015年版.二部.879
[3]中国药典[S].2015年版.二部.945-946
[4]中国实验室国家认可委员会.化学分析中不确定度的评估指南[M].北京:中国计量出版社,2002
[5]国家质量监督检验检疫总局.测量不确定度评定与表示(JJF1059.1-2012)[S].2012:28-47
[6]国家质量监督检验检疫总局.化学分析测量不确定度评定(JJF1135-2005)[S].2005:5-9
[4]国家药典委员会.国家药品标准工作手册(第四版)[M].北京:中国医药科技出版社,2013:157-161