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Projeto de investigação
MOLECULARY IMPRINTED POLYMERS - THEIR APPLICATION IN THE MANUFACTURING OF ACTIVE PHARMACEUTICAL INGREDIENTS APIS
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Development of affinity polymeric particles for the removal of 4-dimethylaminopyridine (DMAP) from active pharmaceutical ingredient crude streams using a green technology
Publication . Viveiros, Raquel; Pinto, José J.; Costa, Nuno; Heggie, William; Casimiro, Teresa; LAQV@REQUIMTE; DQ - Departamento de Química; Elsevier
Polymeric particles with affinity for 4-dimethylaminipyridine (DMAP) were developed by molecular imprinting using supercritical carbon dioxide (scCO2) technology, for cleanup of this potentially genotoxic impurity from crude mixtures of Active Pharmaceutical Ingredients (APIs). DMAP-molecularly imprinted polymer (DMAP-MIP) and the respective control, the non-molecularly imprinted polymer (NIP) were produced by free radical polymerization using methacrylic acid as monomer, ethylene glycol dimethacrylate as crosslinker and AIBN as free-radical initiator in scCO2. The materials were obtained in high yield and were characterized chemically, physically and morphologically. Their extraction efficiency was evaluated by dynamic binding experiments using two solutions: i) a solution containing 104 ppm DMAP solution; ii) model pharmaceutical mixture containing 104 ppm of DMAP and 1018 ppm of Mometasone furoate (API). Particles were able to remove 18.3 µmol DMAP/g polymer from a 104 ppm DMAP solution (i) and 1004.6 µmol DMAP/g API (ii). In addition, high recoveries of both DMAP and API were obtained, above 99%.
Molecularly Imprinted Polymers – Their Application in the Manufacturing of Active Pharmaceutical Ingredients (APIs)
Publication . Viveiros, Raquel Filipa da Costa; Casimiro, Teresa; Heggie, William
Enzyme-inspired dry-powder polymeric catalyst for green and fast pharmaceutical manufacturing processes
Publication . Viveiros, Raquel; Maia, Luísa B.; Corvo, Marta C.; Bonifácio, Vasco D. B.; Heggie, William; Casimiro, Teresa; LAQV@REQUIMTE; DQ - Departamento de Química; DCM - Departamento de Ciência dos Materiais; CENIMAT-i3N - Centro de Investigação de Materiais (Lab. Associado I3N); Elsevier
Catalysis in pharma manufacturing processes is typically homogeneous, expensive and with hard catalyst recovery/regeneration. Herein an enzyme-inspired dry-powder molecularly imprinted polymeric (MIP) system was designed for fast, selective oxidation of a cholesterol derivative and easy catalyst regeneration. The strategy involved the synthesis of a template-monomer (T:M) complex followed by the crosslinked polymerization in supercritical carbon dioxide (scCO2). A 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO)-MIP catalyst is obtained after the template cleavage from the matrix, and the oxidation of the N[sbnd]H groups turns available TEMPO moieties within the MIP. The oxidation of benzyl alcohol, 5α-cholestan-3β-ol and cholic acid was fast, in high yield and with selective oxidation capacity.
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Entidade financiadora
Fundação para a Ciência e a Tecnologia
Programa de financiamento
OE
Número da atribuição
SFRH/BDE/51907/2012