Determination of volatiles in pharmaceutical certified reference materials

Journal of the Brazilian Chemical Society

Raquel Nogueira²  Suzane M. Queiroz²  Gisele E. B. Silva²  Werickson F. C. Rocha²  Gabriel F. Sarmanho²  Renato R. R. Almeida²  Gabriela F. Moreira¹ 

[1] ,National Institute of Metrology, Quality and Technology Chemical Metrology Division Xerém RJ ,Brazil

关键词: volatiles;    water;    residual solvents;    active pharmaceutical ingredient (API);    certified reference materials (CRM);    analytical quality control;   

DOI  :  10.1590/S0103-50532012005000021

来源: SciELO

【 摘 要 】

This work compares the results obtained for the determination of volatiles (water and residual solvents) in new certified reference materials (CRM) or candidate CRMs of the active pharmaceutical ingredients (API) captopril, metronidazole, sodium diclofenac, potassium diclofenac and furosemide, by means of different techniques: loss on drying (LOD), Karl Fischer (KF) coulometric titration, static headspace gas chromatography with flame ionization detection (sHS-GC-FID) and with mass spectrometry (sHS-GC-MS), thermogravimetric analysis (TGA) and near infrared spectroscopy (NIR) with multivariate chemometric analysis of results. The first three methods led to complementary results. The two other techniques were not sufficiently sensitive to determine volatiles in the concentration range evaluated. The loss on drying method was considered the most appropriate to determine the mass fraction of the volatiles to be used in the mass balance calculation of the API mass fraction in the pharmaceutical CRMs.

【 授权许可】

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