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Pharmaceutics
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Supercritical Techniques for Pharmaceutical Applications
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Supercritical Techniques for Pharmaceutical Applications

A special issue of Pharmaceutics (ISSN 1999-4923). This special issue belongs to the section "Pharmaceutical Technology, Manufacturing and Devices".

Deadline for manuscript submissions: closed (10 October 2024) | Viewed by 8524

Special Issue Editors

Dr. Mauro Banchero

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Guest Editor
Department of Applied Science and Technology, Politecnico di Torino, corso Duca degli Abruzzi, 24, 10129 Torino, Italy
Interests: solubility of drugs in supercritical fluids; supercritical techniques for the preparation of drug delivery systems; supercritical drying and aerogels; supercritical-CO2-mediated inclusion complexation of cyclodextrins; drug delivery
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Barbara Onida

E-Mail Website
Guest Editor
Department of Applied Science and Technology, Politecnico di Torino, Corso Duca degli Abruzzi, 24, 10129 Turin, Italy
Interests: nanoporous materials; surface chemistry of materials; nanostructured materials for drug delivery; drug adsorption by means of supercritical carbon dioxide; nanoporous materials in adsorption and purification processes; nanostructured materials in heterogeneous catalysis
Special Issues, Collections and Topics in MDPI journals
Dr. Marta Gallo

E-Mail Website
Guest Editor
DISAT Department, Politecnico di Torino, corso Duca degli Abruzzi 29, 10129 Torino, Italy
Interests: silica particles; polymer; oxide-based and hybrid systems
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Supercritical fluid technologies, by achieving a perfect separation of the solvent and the processed products, are undoubtedly attractive to pharmaceutics. They perfectly fit several issues related to the delivery of unstable or poorly water-soluble drugs since, with respect to conventional techniques, they offer the possibility of controlling particle size and morphology of the carriers and allow thermolabile compounds to be processed. Different approaches may be pursued, which depend on whether the solvent or the antisolvent power of the supercritical medium is exploited. These may range from micronization techniques, supercritical solvent impregnation of organic and inorganic carriers, preparation of drug-releasing microporous polymeric foams as well as liposome or solid-lipid nanoparticles. The use of aerogels is another popular approach in drug delivery since the supercritical medium can be used both to synthesize the carrier and to load the active ingredients.

This Special Issue aims to collect an up-to-date selection of the different techniques that employ a supercritical fluid for Pharmaceutical Applications. Research or review articles that cover innovative aspects of established techniques as well as new approaches, or the preparation of novel carriers, are particularly welcome.

We look forward to receiving your contributions.

Dr. Mauro Banchero
Prof. Dr. Barbara Onida
Dr. Marta Gallo
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Pharmaceutics is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2900 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • supercritical carbon dioxide
  • drug delivery systems
  • micronization techniques
  • supercritical solvent impregnation
  • organic, inorganic, and hybrid carriers
  • microporous polymeric foams
  • liposomes
  • solid-lipid nanoparticles
  • aerogels

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Published Papers (6 papers)

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Research

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16 pages, 4552 KiB  
Article
Synthesis of Self-Assembled Nanostructured Cisplatin Using the RESS Process
by Sudhir Kumar Sharma, Loganathan Palanikumar, Renu Pasricha, Thirumurugan Prakasam, Mazin Magzoub and Ramesh Jagannathan
Pharmaceutics 2024, 16(11), 1471; https://doi.org/10.3390/pharmaceutics16111471 - 18 Nov 2024
Viewed by 383
Abstract
Background/Objectives: The primary goal of our research is to develop a process to prepare an aqueous dispersion of Cisplatin, an important anticancer drug, with increased solubility and storage stability. Method: In this context, we report the use of a customized RESS process for [...] Read more.
Background/Objectives: The primary goal of our research is to develop a process to prepare an aqueous dispersion of Cisplatin, an important anticancer drug, with increased solubility and storage stability. Method: In this context, we report the use of a customized RESS process for the synthesis of a novel, amber-colored and viscous aqueous cisplatin solution, an important anticancer drug, which we have denoted as “liquid” cisplatin. Results: Using specialized liquid cell in situ transmission electron microscopy (Liquid in situ TEM) and Raman spectroscopy, we demonstrated that “liquid” cisplatin comprises a bi-modal distribution of a highly solvated network of stable cisplatin nanoclusters in water and exhibited 27 times greater water solubility than standard cisplatin. More importantly, “liquid” cisplatin was stable at ambient conditions for over two years. Extensive analytical characterization of “liquid” cisplatin confirmed that it retained the original chemical identity of cisplatin. Cell viability and apoptosis studies on human lung adenocarcinoma A549 cells provided compelling evidence that “liquid” cisplatin demonstrated a more sustained anticancer effect compared to standard cisplatin. Conclusions: Aqueous cisplatin solubility was increased by 27X in the “liquid” cisplatin medium which retained its bio efficacy over a 2-year period. Our experimental results suggest the possibility of developing non-invasive and highly effective novel cisplatin drug-delivery platforms. Full article
(This article belongs to the Special Issue Supercritical Techniques for Pharmaceutical Applications)
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19 pages, 6385 KiB  
Article
Osteoblastic Cell Sheet Engineering Using P(VCL-HEMA)-Based Thermosensitive Hydrogels Doped with pVCL@Icariin Nanoparticles Obtained with Supercritical CO2-SAS
by Rubén García-Sobrino, Isabel Casado-Losada, Carmen Caltagirone, Ana García-Crespo, Carolina García, Juan Rodríguez-Hernández, Helmut Reinecke, Alberto Gallardo, Carlos Elvira and Enrique Martínez-Campos
Pharmaceutics 2024, 16(8), 1063; https://doi.org/10.3390/pharmaceutics16081063 - 13 Aug 2024
Viewed by 1084
Abstract
New clinical strategies for treating severe bone and cartilage injuries are required, especially for use in combination with implant procedures. For this purpose, p(VCL-co-HEMA) thermosensitive hydrogels have been activated with icariin-loaded nanoparticles to be used as bone-cell-harvesting platforms. Supercritical CO2-SAS technology [...] Read more.
New clinical strategies for treating severe bone and cartilage injuries are required, especially for use in combination with implant procedures. For this purpose, p(VCL-co-HEMA) thermosensitive hydrogels have been activated with icariin-loaded nanoparticles to be used as bone-cell-harvesting platforms. Supercritical CO2-SAS technology has been applied to encapsulate icariin, a small molecule that is involved in osteoblastic differentiation. Thus, physical-chemical analysis, including swelling and transmittance, showed the impact of HEMA groups in hydrogel composition. Moreover, icariin (ICA) release from p(VCL-co-HEMA) platforms, including pVCL@ICA nanoparticles, has been studied to evaluate their efficacy in relevant conditions. Finally, the thermosensitive hydrogels’ cell compatibility, transplant efficiency, and bone differentiation capacity were tested. This study identifies the optimal formulations for icariin-activated hydrogels for both control and HEMA formulations. Using this technique, osteoblastic sheets that were rich in collagen type I were successfully transplanted and recultivated, maintaining an optimal extracellular matrix (ECM) composition. These findings suggest a new cell-sheet-based therapy for bone regeneration purposes using customized and NP-activated pVCL-based cell platforms. Full article
(This article belongs to the Special Issue Supercritical Techniques for Pharmaceutical Applications)
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14 pages, 5171 KiB  
Article
Curcumin/Carrier Coprecipitation by Supercritical Antisolvent Route
by Stefania Mottola and Iolanda De Marco
Pharmaceutics 2024, 16(3), 352; https://doi.org/10.3390/pharmaceutics16030352 - 2 Mar 2024
Viewed by 1036
Abstract
In this work, polyvinylpyrrolidone (PVP)- and β-cyclodextrin (β-CD)-based composite powders containing curcumin (CURC) were obtained through the supercritical antisolvent (SAS) technique. Pressure, total concentration of CURC/carrier in dimethylsulfoxide, and CURC/carrier ratio effects on the morphology and size of the precipitated powders were investigated. [...] Read more.
In this work, polyvinylpyrrolidone (PVP)- and β-cyclodextrin (β-CD)-based composite powders containing curcumin (CURC) were obtained through the supercritical antisolvent (SAS) technique. Pressure, total concentration of CURC/carrier in dimethylsulfoxide, and CURC/carrier ratio effects on the morphology and size of the precipitated powders were investigated. Using PVP as the carrier, spherical particles with a mean diameter of 1.72 μm were obtained at 12.0 MPa, 20 mg/mL, and a CURC/PVP molar ratio equal to 1/2 mol/mol; using β-CD as the carrier, the optimal operating conditions were 9.0 MPa and 200 mg/mL; well-defined micrometric particles with mean diameters equal to 2.98 and 3.69 μm were obtained at molar ratios of 1/2 and 1/1 mol/mol, respectively. FT-IR spectra of CURC/ β-CD inclusion complexes and coprecipitated CURC/PVP powders revealed the presence of some peaks of the active compounds. The stoichiometry of the complexes evaluated through the Job method revealed that β-CD formed inclusion complexes with CURC at a molar ratio equal to 1/1. Dissolution profiles revealed that in comparison with the curve of the pure ingredient, the SAS-processed powders obtained using both PVP and β-CD have an improved release rate. Full article
(This article belongs to the Special Issue Supercritical Techniques for Pharmaceutical Applications)
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22 pages, 9747 KiB  
Article
Exploring the Effects of Process Parameters during W/O/W Emulsion Preparation and Supercritical Fluid Extraction on the Protein Encapsulation and Release Properties of PLGA Microspheres
by Heejun Park
Pharmaceutics 2024, 16(3), 302; https://doi.org/10.3390/pharmaceutics16030302 - 21 Feb 2024
Cited by 3 | Viewed by 1755
Abstract
In this study, protein-loaded poly(lactic-co-glycolic acid) (PLGA) microspheres were prepared via supercritical fluid extraction of emulsion (SFEE) technology. To understand the correlation between process parameters and the main quality characteristics of PLGA microspheres, a comprehensive prior study on the influence of process variables [...] Read more.
In this study, protein-loaded poly(lactic-co-glycolic acid) (PLGA) microspheres were prepared via supercritical fluid extraction of emulsion (SFEE) technology. To understand the correlation between process parameters and the main quality characteristics of PLGA microspheres, a comprehensive prior study on the influence of process variables on encapsulation efficiency (EE), initial drug burst release (IBR), morphology, surface property, and particle size distribution (PSD) was conducted within a wide process condition range of each unit process step, from the double-emulsion preparation step to the extraction step. Bovine serum albumin (BSA), a high-molecular weight-protein that is difficult to control the IBR and EE of PLGA microspheres with, was used as a model material. As double-emulsion manufacturing process parameters, the primary (W/O) and secondary emulsion (W/O/W) homogenization speed and secondary emulsification time were evaluated. In addition, the effect of the SFEE process parameters, including the pressure (70–160 bar), temperature (35–65 °C), stirring rate (50–1000 rpm), and flow rate of supercritical carbon dioxide, SC-CO2 (1–40 mL/min), on PLGA microsphere quality properties were also evaluated. An increase in the homogenization speed of the primary emulsion resulted in an increase in EE and a decrease in IBR. In contrast, increasing the secondary emulsification speed resulted in a decrease in EE and an increase in IBR along with a decrease in microsphere size. The insufficient secondary emulsification time resulted in excessive increases in particle size, and excessive durations resulted in decreased EE and increased IBR. Increasing the temperature and pressure of SFEE resulted in an overall increase in particle size, a decrease in EE, and an increase in IBR. It was observed that, at low stirring rates or SC-CO2 flow rates, there was an increase in particle size and SPAN value, while the EE decreased. Overall, when the EE of the prepared microspheres is low, a higher proportion of drugs is distributed on the external surface of the microspheres, resulting in a larger IBR. In conclusion, this study contributes to the scientific understanding of the influence of SFEE process variables on PLGA microspheres. Full article
(This article belongs to the Special Issue Supercritical Techniques for Pharmaceutical Applications)
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19 pages, 6761 KiB  
Article
Instant Formulation of Inhalable Beclomethasone Dipropionate—Gamma-Cyclodextrin Composite Particles Produced Using Supercritical Assisted Atomization
by Hsien-Tsung Wu, Han-Cyuan Lin, Yi-Jia Tu and Kim Hoong Ng
Pharmaceutics 2023, 15(6), 1741; https://doi.org/10.3390/pharmaceutics15061741 - 15 Jun 2023
Cited by 1 | Viewed by 1021
Abstract
Medical composites derived from Gamma-cyclodextrin (γ-CD) and beclomethasone dipropionate−gamma-cyclodextrin (BDP−γ-CD) are synthesized over supercritical-assisted atomization (SAA) herein. Carbon dioxide, which serves the dual function of spraying medium and co-solute, is incorporated in this process along with the ethanolic solvent. [...] Read more.
Medical composites derived from Gamma-cyclodextrin (γ-CD) and beclomethasone dipropionate−gamma-cyclodextrin (BDP−γ-CD) are synthesized over supercritical-assisted atomization (SAA) herein. Carbon dioxide, which serves the dual function of spraying medium and co-solute, is incorporated in this process along with the ethanolic solvent. Results indicate that, for fine spherical particles, optimized aerosol performance could be obtained with 50.0% (w/w) ethanolic solvent, precipitator, and saturator at 373.2 K and 353.2 K, respectively, and carbon dioxide-to-γ-CD flow ratio of 1.8 in the presence of 10 wt% leucine (LEU) as dispersion enhancer. It is also noted that γ-CD solution at low concentration typically renders better aerosol performance of the particles. During drug particle-derivation, the solubility of drug BDP elevated considerably due to the formation of inclusion complexes, further assisted by the ethanolic solvent which increases the lipophilicity of BDP. Meanwhile, the in vitro aerosolization and dissolution performance of drug composites derived from varied γ-CD-to-BDP mass ratio (Z) were also evaluated. It was found that high Z promises higher fine particle fraction in the obtained drug composite while the dissolution rate of active ingredient (BDP) exhibits positive correlation to the content of water-soluble excipient (γ-CD) in the formulation. This study offers a new avenue for instant drug formulation with promising pulmonary delivery over the SAA technique. Full article
(This article belongs to the Special Issue Supercritical Techniques for Pharmaceutical Applications)
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Review

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31 pages, 9165 KiB  
Review
Aerogels as Carriers for Oral Administration of Drugs: An Approach towards Colonic Delivery
by Carlos Illanes-Bordomás, Mariana Landin and Carlos A. García-González
Pharmaceutics 2023, 15(11), 2639; https://doi.org/10.3390/pharmaceutics15112639 - 17 Nov 2023
Cited by 6 | Viewed by 2292
Abstract
Polysaccharide aerogels have emerged as a highly promising technology in the field of oral drug delivery. These nanoporous, ultralight materials, derived from natural polysaccharides such as cellulose, starch, or chitin, have significant potential in colonic drug delivery due to their unique properties. The [...] Read more.
Polysaccharide aerogels have emerged as a highly promising technology in the field of oral drug delivery. These nanoporous, ultralight materials, derived from natural polysaccharides such as cellulose, starch, or chitin, have significant potential in colonic drug delivery due to their unique properties. The particular degradability of polysaccharide-based materials by the colonic microbiota makes them attractive to produce systems to load, protect, and release drugs in a controlled manner, with the capability to precisely target the colon. This would allow the local treatment of gastrointestinal pathologies such as colon cancer or inflammatory bowel diseases. Despite their great potential, these applications of polysaccharide aerogels have not been widely explored. This review aims to consolidate the available knowledge on the use of polysaccharides for oral drug delivery and their performance, the production methods for polysaccharide-based aerogels, the drug loading possibilities, and the capacity of these nanostructured systems to target colonic regions. Full article
(This article belongs to the Special Issue Supercritical Techniques for Pharmaceutical Applications)
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