Publication
Simultaneous determination of dapsone and clofazimine in nanoformulations by HPLC
| dc.contributor.author | Fernandes, Sara R. | |
| dc.contributor.author | Fernandes, Sara | |
| dc.contributor.author | Chaves, Luíse L. | |
| dc.contributor.author | Lima, Sofia A. C. | |
| dc.contributor.author | Silva, Eduarda M. P. | |
| dc.contributor.author | Barreiros, Luísa | |
| dc.contributor.author | Reis, Salette | |
| dc.contributor.author | Segundo, Marcela A. | |
| dc.date.accessioned | 2025-07-08T08:45:46Z | |
| dc.date.available | 2025-07-08T08:45:46Z | |
| dc.date.issued | 2018-03 | |
| dc.description.abstract | The multidrug therapy with dapsone (DAP) and clofazimine (CLZ) is known as an effective treatment against Mycobacterium leprae. However, the low bioavailability and non-specific distribution can reduce therapy efficacy and produce side effects. The use of nanotechnological approaches was explored as a promising carrier for delivery enhancement of these drugs. Therefore, a simple and precise highperformance liquid chromatography (HPLC) method with UV/Vis detection has been developed and validated for the simultaneous determination of DAP and CLZ loaded in solid dispersion and poly(D,L-lactide-co-glycolic acid) nanoparticles, respectively, targeting therapy improvement. A reversed phase Kinetex core-shell C18 column at room temperature followed by UV/Vis detection at 280 nm was used for chromatographic separation. The elution was performed in gradient mode using aqueous acetate buffer (50 mol L-1, pH 4.8) and an increasing acetonitrile content from 27 to 63% (v/v), at a flow rate of 1.0 mL min-1. The injection volume was fixed at 20 µL and total run time was 23.0 min, with a retention time of 6.0 min for DAP and 14.0 min for CLZ. The method was validated according to EMA guideline and showed specificity, accuracy (between 99.6 and 114.0% of nominal values) and precision for intra-day (RSD ≤1.8%) and inter-day assays (RSD ≤12.5%). Calibration curves were linear (r2 >0.9979) and LOD ≤0.03 and LOQ ≤0.06 mg L-1 were obtained. Stability was studied after 24 h at room temperature and over three freeze-thaw cycles, and recovery values ≥86.2% were obtained. Precipitation of CLZ was observed at low temperatures (4 °C). Entrapment efficiency in nanoformulations was evaluated as 54.8 ± 0.1% for DAP and 24.9 ± 0.2% for CLZ. The developed method was successfully validated for the simultaneous determination of DAP and CLZ in nanoparticles. | por |
| dc.description.sponsorship | NORTE-01-0145-FEDER-000011 | |
| dc.identifier.citation | Machado, S., Fernandes, S. R., Chaves, L. L., Lima, S. A. C., Silva, E. M. P., Barreiros, L., Reis, S., & Segundo, M. A. (2018). Simultaneous determination of dapsone and clofazimine in nanoformulations by HPLC. Book of Abstracts Analítica 2018 - 9th Meeting of Division of Analytical Chemistry, 85. https://analitica2018.eventos.chemistry.pt/images/book.pdf | |
| dc.identifier.isbn | 978-989-8124-21-0 | |
| dc.identifier.uri | http://hdl.handle.net/10400.22/30214 | |
| dc.language.iso | eng | |
| dc.peerreviewed | n/a | |
| dc.publisher | Sociedade Portuguesa de Química | |
| dc.relation | PT2020 UID/QUI/50006/2013 - POCI/01/0145/FEDER/007265 | |
| dc.relation.hasversion | https://analitica2018.eventos.chemistry.pt/images/book.pdf | |
| dc.rights.uri | N/A | |
| dc.subject | Dapsone (DAP) | |
| dc.subject | Clofazimine (CLZ) | |
| dc.title | Simultaneous determination of dapsone and clofazimine in nanoformulations by HPLC | por |
| dc.type | conference poster | |
| dspace.entity.type | Publication | |
| oaire.citation.conferenceDate | 2018 | |
| oaire.citation.conferencePlace | FFUP/ICBAS – UNIVERSITY OF PORTO | |
| oaire.citation.startPage | 85 | |
| oaire.citation.title | Book of Abstracts Analítica 2018 - 9th Meeting of Division of Analytical Chemistry | |
| oaire.version | http://purl.org/coar/version/c_970fb48d4fbd8a85 | |
| person.familyName | Fernandes | |
| person.givenName | Sara | |
| person.identifier.ciencia-id | 1C12-D800-38A4 | |
| person.identifier.orcid | 0000-0001-7042-1941 | |
| person.identifier.scopus-author-id | 57203278917 | |
| relation.isAuthorOfPublication | 6c2ed5f0-c3fd-4559-99a3-b8d78d019b47 | |
| relation.isAuthorOfPublication.latestForDiscovery | 6c2ed5f0-c3fd-4559-99a3-b8d78d019b47 |