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| Content Provider | Springer Nature Link |
|---|---|
| Author | Rodrigues, Miguel A. Tiago, João M. Padrela, Luis Matos, Henrique A. Nunes, Teresa G. Pinheiro, Lídia Almeida, António J. Azevedo, Edmundo Gomes |
| Copyright Year | 2014 |
| Abstract | To prepare and thoroughly characterize a new polymorph of the broad-spectrum antibiotic minocycline from its hydrochloride dehydrate salts.The new minocycline hydrochloride polymorph was prepared by means of the antisolvent effect caused by carbon dioxide. Minocycline recrystallized as a red crystalline hydrochloride salt, starting from solutions or suspensions containing CO$_{2}$ and ethanol under defined conditions of temperature, pressure and composition.This novel polymorph (β-minocycline) revealed characteristic PXRD and FTIR patterns and a high melting point (of 247 ºC) compared to the initial minocycline hydrochloride hydrates (α-minocycline). Upon dissolution the new polymorph showed full anti-microbial activity. Solid-state NMR and DSC studies evidenced the higher chemical stability and crystalline homogeneity of β-minocycline compared to the commercial chlorohydrate powders. Molecular structures of both minocyclines present relevant differences as shown by multinuclear solid-state NMR.This work describes a new crystalline structure of minocycline and evidences the ability of ethanol-CO$_{2}$ system in removing water molecules from the crystalline structure of this API, at modest pressure, temperature and relatively short time (2 h), while controlling the crystal habit. This process has therefore the potential to become a consistent alternative towards the control of the solid form of APIs. |
| Starting Page | 3136 |
| Ending Page | 3149 |
| Page Count | 14 |
| File Format | |
| ISSN | 07248741 |
| Journal | Pharmaceutical Research |
| Volume Number | 31 |
| Issue Number | 11 |
| e-ISSN | 1573904X |
| Language | English |
| Publisher | Springer US |
| Publisher Date | 2014-05-20 |
| Publisher Place | Boston |
| Access Restriction | One Nation One Subscription (ONOS) |
| Subject Keyword | Pharmacology/Toxicology Pharmacy Biochemistry Medical Law Biomedical Engineering |
| Content Type | Text |
| Resource Type | Article |
| Subject | Organic Chemistry Pharmacology Molecular Medicine Pharmacology (medical) Biotechnology Pharmaceutical Science |
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