Submerged Eutectic-Assisted, Solvent-Free Mechanochemical Formation of a Propranolol Salt and Its Other Multicomponent Solids
Salt preparation via a solid-state reaction offers a solution to challenges posed by current pharmaceutical research, which include combining development of novel forms of active pharmaceutical ingredients with greener, sustainable synthesis. This work investigated in detail the mechanism of salt fo...
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| Format: | Article |
| Language: | English |
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MDPI AG
2021-12-01
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| Series: | Pharmaceutics |
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| Online Access: | https://www.mdpi.com/1999-4923/13/12/2125 |
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| author | Klaudia Bialek Zaneta Wojnarowska Marcin Skotnicki Brendan Twamley Marian Paluch Lidia Tajber |
| author_facet | Klaudia Bialek Zaneta Wojnarowska Marcin Skotnicki Brendan Twamley Marian Paluch Lidia Tajber |
| author_sort | Klaudia Bialek |
| collection | DOAJ |
| description | Salt preparation via a solid-state reaction offers a solution to challenges posed by current pharmaceutical research, which include combining development of novel forms of active pharmaceutical ingredients with greener, sustainable synthesis. This work investigated in detail the mechanism of salt formation between propranolol (PRO) and capric acid (CAP) and explored the solid eutectic phases comprising this salt, propranolol caprate (PRC). The salt structure was solved by X-ray diffraction, and the properties in the crystalline and supercooled states were fully characterised using thermal analysis, nuclear magnetic resonance, Fourier-transform infrared spectroscopy and broadband dielectric spectroscopy (BDS). PRC forms via a submerged eutectic phase composed of PRO and CAP, below room temperature, by mechanochemistry without an extra input of energy. Two other solid eutectic phases are composed of PRC and either CAP or PRO, at 0.28 and 0.82 mol fraction of PRO, respectively. BDS indicated that the supercooled PRC has ionic character, whereas the supercooled PRC-PRO eutectic had predominantly non-ionic properties despite comprising the salt. In conclusion, knowledge of the mechanism of formation of multicomponent systems can help in designing more sustainable pharmaceutical processes. |
| first_indexed | 2024-03-10T03:19:30Z |
| format | Article |
| id | doaj.art-781c322c8c104359adcb2974de129286 |
| institution | Directory Open Access Journal |
| issn | 1999-4923 |
| language | English |
| last_indexed | 2024-03-10T03:19:30Z |
| publishDate | 2021-12-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Pharmaceutics |
| spelling | doaj.art-781c322c8c104359adcb2974de1292862023-11-23T10:06:14ZengMDPI AGPharmaceutics1999-49232021-12-011312212510.3390/pharmaceutics13122125Submerged Eutectic-Assisted, Solvent-Free Mechanochemical Formation of a Propranolol Salt and Its Other Multicomponent SolidsKlaudia Bialek0Zaneta Wojnarowska1Marcin Skotnicki2Brendan Twamley3Marian Paluch4Lidia Tajber5School of Pharmacy and Pharmaceutical Sciences, Trinity College Dublin, D02 PN40 Dublin, IrelandSchool of Pharmacy and Pharmaceutical Sciences, Trinity College Dublin, D02 PN40 Dublin, IrelandChair and Department of Pharmaceutical Technology, Poznan University of Medical Sciences, ul. Grunwaldzka 6, 60-780 Poznan, PolandSchool of Chemistry, Trinity College Dublin, D02 PN40 Dublin, IrelandInstitute of Physics, University of Silesia, SMCEBI, 75 Pulku Piechoty 1A, 41-500 Chorzow, PolandSchool of Pharmacy and Pharmaceutical Sciences, Trinity College Dublin, D02 PN40 Dublin, IrelandSalt preparation via a solid-state reaction offers a solution to challenges posed by current pharmaceutical research, which include combining development of novel forms of active pharmaceutical ingredients with greener, sustainable synthesis. This work investigated in detail the mechanism of salt formation between propranolol (PRO) and capric acid (CAP) and explored the solid eutectic phases comprising this salt, propranolol caprate (PRC). The salt structure was solved by X-ray diffraction, and the properties in the crystalline and supercooled states were fully characterised using thermal analysis, nuclear magnetic resonance, Fourier-transform infrared spectroscopy and broadband dielectric spectroscopy (BDS). PRC forms via a submerged eutectic phase composed of PRO and CAP, below room temperature, by mechanochemistry without an extra input of energy. Two other solid eutectic phases are composed of PRC and either CAP or PRO, at 0.28 and 0.82 mol fraction of PRO, respectively. BDS indicated that the supercooled PRC has ionic character, whereas the supercooled PRC-PRO eutectic had predominantly non-ionic properties despite comprising the salt. In conclusion, knowledge of the mechanism of formation of multicomponent systems can help in designing more sustainable pharmaceutical processes.https://www.mdpi.com/1999-4923/13/12/2125propranololcapric acidsalteutecticsubmerged eutecticmechanochemistry |
| spellingShingle | Klaudia Bialek Zaneta Wojnarowska Marcin Skotnicki Brendan Twamley Marian Paluch Lidia Tajber Submerged Eutectic-Assisted, Solvent-Free Mechanochemical Formation of a Propranolol Salt and Its Other Multicomponent Solids Pharmaceutics propranolol capric acid salt eutectic submerged eutectic mechanochemistry |
| title | Submerged Eutectic-Assisted, Solvent-Free Mechanochemical Formation of a Propranolol Salt and Its Other Multicomponent Solids |
| title_full | Submerged Eutectic-Assisted, Solvent-Free Mechanochemical Formation of a Propranolol Salt and Its Other Multicomponent Solids |
| title_fullStr | Submerged Eutectic-Assisted, Solvent-Free Mechanochemical Formation of a Propranolol Salt and Its Other Multicomponent Solids |
| title_full_unstemmed | Submerged Eutectic-Assisted, Solvent-Free Mechanochemical Formation of a Propranolol Salt and Its Other Multicomponent Solids |
| title_short | Submerged Eutectic-Assisted, Solvent-Free Mechanochemical Formation of a Propranolol Salt and Its Other Multicomponent Solids |
| title_sort | submerged eutectic assisted solvent free mechanochemical formation of a propranolol salt and its other multicomponent solids |
| topic | propranolol capric acid salt eutectic submerged eutectic mechanochemistry |
| url | https://www.mdpi.com/1999-4923/13/12/2125 |
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