| Texto completo | |
| Autor(es): |
da Silva, Fernando Antunes
;
Lourenco, Felipe Rebello
;
Calixto, Leandro Augusto
Número total de Autores: 3
|
| Tipo de documento: | Artigo Científico |
| Fonte: | JOURNAL OF ANALYTICAL CHEMISTRY; v. 77, n. 7, p. 9-pg., 2022-07-01. |
| Resumo | |
In pharmaceutical analysis, the development of extraction procedures focuses mainly on the optimization of active pharmaceutical ingredients. However, this may lead to low recovery values for impurities, which is a disadvantage for the development of stability-indicating methods to assess the expiration time of drugs in stability studies. Here, we have proposed a multiple optimization for the extraction of ethinylestradiol, levonorgestrel, and their main impurities aiming to develop a stability-indicating chromatographic procedure. A mixture experimental design was adopted to optimize the recovery of ethinylestradiol, levonorgestrel, and 32 impurities. Mixtures of acetonitrile (0 to 60%), methanol (0 to 60%), and water (40 to 80%) were used to extract the analytes from samples subjected to dry thermal degradation. Recovery values for ethinylestradiol and levonorgestrel ranged between 12.5-100.0% and 47.4-100.0%, respectively. Optimal recovery values were achieved using a mixture of methanol (60%) and water (40%). The optimized extraction mixture provided significantly higher recoveries for 18 substances than the initial extraction mixture, including 10 unknown impurities. Most of these unknown impurities did not have a good recoverability. Thus, the multiple optimization of the extraction procedure exhibits great potential for application to optimize sample preparation for stability-indicating analytical procedures. (AU) | |
| Processo FAPESP: | 16/25256-6 - Determinação de metais pesados em produtos tradicionais fitoterápicos por técnicas analíticas alternativas empregando princípios da química verde |
| Beneficiário: | Leandro Augusto Calixto |
| Modalidade de apoio: | Auxílio à Pesquisa - Regular |