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Ball-Free Mechanochemistry: In situ Real-Time Monitoring of Pharmaceutical co-Crystal Formation by Resonant Acoustic Mixing Full article

Journal Chemical Communications
ISSN: 1359-7345 , E-ISSN: 1364-548X
Output data Year: 2018, Volume: 54, Number: 32, Pages: 4033-4036 Pages count : 4 DOI: 10.1039/c8cc02187b
Tags COCRYSTAL; CARBAMAZEPINE; SPECTROSCOPY; NICOTINAMIDE; POLYMORPHISM; TEMPERATURE; ACTIVATION; STABILITY; MECHANISM; IMPACT
Authors Michalchuk Adam A.L. 1,2,3 , Hope Karl S. 1,4 , Kennedy Stuart R. 1 , Blanco Maria V. 5 , Boldyreva Elena V. 3,6 , Pulham Colin R. 1,2
Affiliations
1 EaStCHEM School of Chemistry and Centre for Science at Extreme Conditions, University of Edinburgh, Edinburgh, UK
2 EPSRC Centre for Continuous Manufacturing and Crystallisation (CMAC), UK
3 REC-008 Novosibirsk State University, Novosibirsk, Russian Federation
4 ISIS Neutron and Muon Source, Harwell Science & Innovation Campus, Didcot, UK
5 European Synchrotron Radiation Facility (ESRF), Grenoble, France
6 Institute of Solid State Chemistry and Mechanochemistry SB RAS, Novosibirsk, Russian Federation

Funding (5)

1 The University of Edinburgh
2 Engineering and Physical Sciences Research Council CMAC 1/1033459/1
3 The Ministry of Education and Science of the Russian Federation
4 Rutherford Appleton Laboratory WSTC/0047
5 Federal Agency for Scientific Organizations 0301-2018-0007

Abstract: Resonant acoustic mixing (RAM) is a new technology designed for intensive mixing of powders that offers the capability to process powders with minimal damage to particles. This feature is particularly important for mixing impact-sensitive materials such as explosives and propellants. While the RAM technique has been extensively employed for the mixing of powders and viscous polymers, comparatively little is known about its use for mechanosynthesis. We present here the first in situ study of RAM-induced co-crystallisation monitored using synchrotron X-ray powder diffraction. The phase profile of the reaction between nicotinamide and carbamazepine in the presence of a small amount of water was monitored at two different relative accelerations of the mixer. In marked contrast to ball-milling techniques, the lack of milling bodies in the RAM experiment does not hinder co-crystallisation of the two starting materials, which occurred readily and was independent of the frequency of oscillation. The reaction could be optimised by enhancing the number of reactive contacts through mixing and comminution. These observations provide new insight into the role of various experimental parameters in conventional mechanochemistry using liquid-assisted grinding techniques.
Cite: Michalchuk A.A.L. , Hope K.S. , Kennedy S.R. , Blanco M.V. , Boldyreva E.V. , Pulham C.R.
Ball-Free Mechanochemistry: In situ Real-Time Monitoring of Pharmaceutical co-Crystal Formation by Resonant Acoustic Mixing
Chemical Communications. 2018. V.54. N32. P.4033-4036. DOI: 10.1039/c8cc02187b WOS Scopus РИНЦ AN OpenAlex
Files: Full text from publisher
Dates:
Submitted: Mar 19, 2018
Accepted: Mar 28, 2018
Published online: Mar 29, 2018
Published print: Apr 18, 2018
Identifiers:
Web of science: WOS:000435250100027
Scopus: 2-s2.0-85045576903
Elibrary: 35496954
Chemical Abstracts: 2018:683187
OpenAlex: W2794912075
Citing:
DB Citing
Web of science 88
Scopus 92
OpenAlex 105
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