Produção Nacional
Revisado por pares
Development of a new sodium diclofenac certified reference material using the mass balance approach and 1H qNMR to determine the certified property value
2012; Elsevier BV; Volume: 48; Issue: 3 Linguagem: Inglês
10.1016/j.ejps.2012.11.005
ISSN1879-0720
AutoresRaquel F. Pupo Nogueira, Bruno Carius Garrido, Ricardo M. Borges, Gisele E. B. Silva, Suzane M. Queiroz, Valnei S. Cunha,
Tópico(s)Chemical Thermodynamics and Molecular Structure
ResumoCertified 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 (1H qNMR). The paper also presents a Monte Carlo simulation to estimate the measurement uncertainty as an approach to validate the GUM results in 1H 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.
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