Development of a new sodium diclofenac certified reference material using the mass balance approach and 1H qNMR to determine the certified property value
Development of a new sodium diclofenac certified reference material using the mass balance approach and 1H qNMR to determine the certified property value
复制标题
DOI：
10.1016/j.ejps.2012.11.005
复制
发表时间：
2013-02-14
影响因子：
4.6
通讯作者：
Cunha, Valnei S.
中科院分区：
文献类型：
--
作者：
Nogueira, Raquel;Garrido, Bruno C.;Cunha, Valnei S.
认证标准物质(CRM)是保证测量结果在国际单位制(SI)中的计量可追溯性的必要工具，这意味着结果在时间和空间上的准确性和可比性。在制药领域，只有少数几种标准物质可用，使用(非认证的)标准物质是一种更为常见的做法。本文介绍了基于ISO指南34：2009和35：2005的双氯芬酸钠新候选标准物质的研究情况。项目步骤包括表征、同质性测试、稳定性研究和不确定度估计。在表征中，测定了有机、无机和挥发性杂质的质量分数，并通过独立参考方法或实验室间研究对结果进行了交叉验证。用质量平衡法计算原料药的质量分数，用定量质子核磁共振(H-1q核磁共振)进行交叉验证。文中还给出了用蒙特卡罗模拟来估计测量不确定度的方法，作为验证H-1定量核磁共振中GUM结果的一种方法。验证了批处理单元之间的一致性，并在短期和长期稳定性研究中评估了在运输和储存条件下的候选CRM稳定性。在置信度为95%的情况下，标准不确定度乘以覆盖系数(k=2)得到的标准物质认证属性值和相应的扩展不确定度为(999.76±0.1)mg g(-1)。(C)2012爱思唯尔B.V.保留所有权利。
Certified reference materials (CRMs) are essential tools to guarantee the metrological traceability of measurement results to the International System of Units (SI), which means the accuracy and comparability of results over time and space. In the pharmaceutical area, only a few CRMs are available and the use of (non-certified) reference materials is a much more common practice. In this paper, the studies on a new candidate CRM of sodium diclofenac based on the ISO Guides 34:2009 and 35:2005 are described. The project steps included characterization, homogeneity test, stability studies, and uncertainties estimation. In the characterization, the mass fractions of organic, inorganic, and volatile impurities were determined, and the results were cross-checked by independent reference methods or interlaboratorial study. The API mass fraction was calculated by mass balance and cross-checked by quantitative proton nuclear magnetic resonance (H-1 qNMR). The paper also presents a Monte Carlo simulation to estimate the measurement uncertainty as an approach to validate the GUM results in H-1 qNMR. The homogeneity between batch units was verified, and the candidate CRM stability under transport and storage conditions was evaluated in short- and long-term stability studies. The CRM certified property value and corresponding expanded uncertainty, obtained from the combined standard uncertainty multiplied by the coverage factor (k = 2), for a confidence level of 95%, was (999.76 + 0.10) mg g(-1). (C) 2012 Elsevier B.V. All rights reserved.