“…Figure 3 (untreated), represents the XRPD pattern of untreated CBZ. It shows a relatively high magnitude of peak intensities and the three highest peaks were in the characteristic positions of 2θ=15.9°, 24.0°and 27.5°respectively, which corresponds well with those reported for the monoclinic form (Form III) (22,23). Conversely, the SAS CO 2 treated CBZ exhibited different peaks that are uncharacteristic of Form III (Fig.…”
Section: Sas Co 2 System Operation Proceduressupporting
confidence: 87%
“…In general, a higher operational temperature can either vaporize the organic solvent easily to achieve a higher degree of supersaturation, or increase the solute solubility and there- The yields were calculated using the weight of generated particles divided by the input weight of untreated carbamazepine fore impede the precipitation of particles (20,(22)(23)(24). According to our results, the effect of temperature seemed to prevail in practice.…”
Section: Sas Co 2 System Operation Proceduresmentioning
confidence: 77%
“…Interestingly several new peaks did arise at positions that were in good agreement with other reported CBZ polymorphic forms. For example, peaks at 2θ=4.9°, 8.6°and 13.3°corresponded with those related to the trigonal form (Form II), peaks at 2θ=9.3°and 12.3°with the triclinic form (Form I) and those at 2θ=14.1°w ith the C-centered monoclinic form (Form IV) (22,27). Although the intensities had diminished, the indicative peaks for Form III occur again at 2θ=15.9°and 24.0°in the treated CBZ, with the peak at 27°shifting to 27°from 27.5° (Fig.…”
Abstract. The purpose of this study was to design and build a supercritical CO 2 anti-solvent (SAS) unit and use it to produce microparticles of the class II drug carbamazepine. The operation conditions of the constructed unit affected the carbamazepine yield. Optimal conditions were: organic solution flow rate of 0.15 mL/min, CO 2 flow rate of 7.5 mL/min, pressure of 4,200 psi, over 3,000 s and at 33°C. The drug solidstate characteristics, morphology and size distribution were examined before and after processing using X-ray powder diffraction and differential scanning calorimetry, scanning electron microscopy and laser diffraction particle size analysis, respectively. The in vitro dissolution of the treated particles was investigated and compared to that of untreated particles. Results revealed a change in the crystalline structure of carbamazepine with different polymorphs co-existing under various operation conditions. Scanning electron micrographs showed a change in the crystalline habit from the prismatic into bundled whiskers, fibers and filaments. The volume weighted diameter was reduced from 209 to 29 μm. Furthermore, the SAS CO 2 process yielded particles with significantly improved in vitro dissolution. Further research is needed to optimize the operation conditions of the self-built unit to maximize the production yield and produce a uniform polymorphic form of carbamazepine.
“…Figure 3 (untreated), represents the XRPD pattern of untreated CBZ. It shows a relatively high magnitude of peak intensities and the three highest peaks were in the characteristic positions of 2θ=15.9°, 24.0°and 27.5°respectively, which corresponds well with those reported for the monoclinic form (Form III) (22,23). Conversely, the SAS CO 2 treated CBZ exhibited different peaks that are uncharacteristic of Form III (Fig.…”
Section: Sas Co 2 System Operation Proceduressupporting
confidence: 87%
“…In general, a higher operational temperature can either vaporize the organic solvent easily to achieve a higher degree of supersaturation, or increase the solute solubility and there- The yields were calculated using the weight of generated particles divided by the input weight of untreated carbamazepine fore impede the precipitation of particles (20,(22)(23)(24). According to our results, the effect of temperature seemed to prevail in practice.…”
Section: Sas Co 2 System Operation Proceduresmentioning
confidence: 77%
“…Interestingly several new peaks did arise at positions that were in good agreement with other reported CBZ polymorphic forms. For example, peaks at 2θ=4.9°, 8.6°and 13.3°corresponded with those related to the trigonal form (Form II), peaks at 2θ=9.3°and 12.3°with the triclinic form (Form I) and those at 2θ=14.1°w ith the C-centered monoclinic form (Form IV) (22,27). Although the intensities had diminished, the indicative peaks for Form III occur again at 2θ=15.9°and 24.0°in the treated CBZ, with the peak at 27°shifting to 27°from 27.5° (Fig.…”
Abstract. The purpose of this study was to design and build a supercritical CO 2 anti-solvent (SAS) unit and use it to produce microparticles of the class II drug carbamazepine. The operation conditions of the constructed unit affected the carbamazepine yield. Optimal conditions were: organic solution flow rate of 0.15 mL/min, CO 2 flow rate of 7.5 mL/min, pressure of 4,200 psi, over 3,000 s and at 33°C. The drug solidstate characteristics, morphology and size distribution were examined before and after processing using X-ray powder diffraction and differential scanning calorimetry, scanning electron microscopy and laser diffraction particle size analysis, respectively. The in vitro dissolution of the treated particles was investigated and compared to that of untreated particles. Results revealed a change in the crystalline structure of carbamazepine with different polymorphs co-existing under various operation conditions. Scanning electron micrographs showed a change in the crystalline habit from the prismatic into bundled whiskers, fibers and filaments. The volume weighted diameter was reduced from 209 to 29 μm. Furthermore, the SAS CO 2 process yielded particles with significantly improved in vitro dissolution. Further research is needed to optimize the operation conditions of the self-built unit to maximize the production yield and produce a uniform polymorphic form of carbamazepine.
“…3-fold was identified. Partial density increases of this magnitude are only known for mixtures of ethanol and CO 2 below the mixture critical point [14,15]. Throughout all of the current experiments, the process conditions were set to exceed the mixture critical point of the pseudo-binary (without solute) mixture.…”
The manner in which the presence of a solute can affect the mixing behavior of a solute, solvent and antisolvent in a supercritical antisolvent (SAS) micronization process is demonstrated. The mixing behavior was analyzed by applying a two-dimensional (2D) Raman scattering technique. Mole fraction and partial density distributions were measured for the CO 2 antisolvent. The results originating from the optical investigations were correlated with the particle results. The experiments cover the variation of the solute concentration at fixed operating conditions of 10 MPa and 40°C.
“…GAS process is simple and particularly useful for the crystallization of sensitive materials, e.g. pharmaceuticals, biological products, explosives, etc, since it operates at moderate T [53]. However, a clear disadvantage of GAS process is the lack of effective control on the particle formation.…”
Section: Scf Pd Processes and Their Modificationsmentioning
Strategies for a particular drug delivery are always of great interest for the pharmaceutical industry, and efficient methods of preparing products with controlled particle microstructures are fundamental for the development and application of drug delivery. Supercritical fluid particle design (SCF PD) processes, as a green and effective alternative to traditional methods, have been effectively employed to produce particles with designated microstructures.Combining with research experiences in our research group, this review aims to provide a theoretical framework of SCF PD for particular drug delivery. For any drug delivery formulations, macroscopic properties are directly influenced by the particle microstructures, "Inverse" strategies are introduced at first to obtain the needed particle microstructures for a particular drug delivery in this paper. Then, how to produce particles with designated microstructures via SCF PD processes is discussed, mainly focus on the screening and selection of operating parameters according to thermodynamics and fluid dynamics study. Recent examples of SCF micronization and co-precipitation/ encapsulation processes are also summarized with an emphasis on how to tailor the particle microstructures by controlling the operating parameters.Finally, challenges and issues needed further study are briefly suggested for SCD PD.
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