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- Title
Multiple Optimization for Extraction of Ethinylestradiol, Levonorgestrel, and Their Main Impurities using Mixture Design.
- Authors
Antunes da Silva, Fernando; Lourenço, Felipe Rebello; Calixto, Leandro Augusto
- Abstract
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.
- Subjects
ETHINYL estradiol; LEVONORGESTREL; DRUG stability; MIXTURES
- Publication
Journal of Analytical Chemistry, 2022, Vol 77, Issue 7, p844
- ISSN
1061-9348
- Publication type
Article
- DOI
10.1134/S1061934822070048