摘要
目的:建立测定鲑降钙素鼻喷雾剂中鲑降钙素含量不确定度的评定方法。方法:采用国家药品标准YBH05252003-2014Z中鲑降钙素含量测定方法进行测定,同时依据《测量不确定度评定与表示》JJF 1059.1-2012中的相关规定,建立测定鲑降钙素的不确定度数学模型,并对不确定度来源进行分析和评定。结果:鲑降钙素含量的不确定度来源主要有对照品称量(M_(R))、对照品溶液制备(C_(V))、供试品溶液制备(V_(S))、供试品测量重复性(S_(S))和对照品的积分峰面积重复性(R)。高效液相色谱(HPLC)外标法测定鲑降钙素鼻喷雾剂中鲑降钙素含量的合成不确定度为0.177 6μg·m L^(-1),扩展不确定度为0.355 2(k=2,置信概率为95%)。结论:测定鲑降钙素鼻喷雾剂中鲑降钙素含量的不确定度贡献主要来源于供试品溶液的配制及标准品测量重复性,而对照品称量和配制对不确定度的贡献较小。若减小鲑降钙素测定时的不确定度,应在实验过程中特别注意供试品的配制,规范实验人员试验操作,实验仪器需定期校准,才能减少不确定度的产生。本研究量化了此测定分析方法的不确定度,所建立的方法适用于HPLC外标法测定鲑降钙素鼻喷雾剂中鲑降钙素含量研究的不确定度评定。
Objective:To establish an evaluation method for the uncertainty in determination of salmon calcitonin content in salmon calcitonin nasal spray.Methods:The content determination of salmon calcitonin was carried out according to the national drug standard YBH05252003-2014Z.At the same time,according to the relevant provisions of"Evaluation and Representation of Measurement Uncer-tainty"JJF 1059.1-2012,an mathematical model for uncertainty in determining salmon calcitonin content was established,and the sources of uncertainty were analyzed and evaluated.Results:The main sources of uncertainty of salmon calcitonin content were reference substance weighing(M_(R)),reference substance solution preparation(C_(V)),test substance solution preparation(V_(S)),test substance mea-surement repeatability(S_(S))and the repeatability of the integrated peak area of the reference substance(R).The combined uncertainty of the determination of salmon calcitonin content in salmon calcitonin nasal spray by external standard HPLC was 0.1776µg·mL^(-1),and the expanded uncertainty was 0.3552(k=2,confidence probability was 95%).Conclusion:The contribution to the uncertainty in determi-nation of salmon calcitonin contern in salmon calcitonin nasal spray mainly comes from the preparation of the test solution and the repeat-ability of the test of standard substance,while the weighing and preparation of the reference substance have a small contribution to the uncertainty.To reduce the uncertainty in the determination of salmon calcitonin,special attention should be paid to the preparation of the test sample during the experiment,and the operation of the experimenter should be standardized.The experimental instruments need to be calibrated regularly to reduce the generation of uncertainty.This study quantified the uncertainty of this measurement and analysis method.The established method is suitable for the uncertainty evaluation of the determination of salmon calcitonin content in salmon cal-citonin nasal spray by external standard HPLC.
作者
朱春玥
肖斯婷
李雪梅
曹春然
ZHU Chunyue;XIAO Siting;LI Xuemei;CAO Chunran(Beijing Institute for Drug Control,Key Laboratory for Safety Research and Evaluation of Innovative Drugs,NMPA,Beijing Key Laboratory for Analysis and Biological Evaluation of Traditional Chinese Medicine,Beijing 102206,China)
出处
《中国医药导刊》
2025年第2期157-161,共5页
Chinese Journal of Medicinal Guide
关键词
鲑降钙素鼻喷雾剂
不确定度
鲑降钙素
含量测定
Salmon calcitonin nasal spray
Uncertainty
Salmon calcitonin
Content determination
