Présidente de l’I.S.A.S.F. (International Society for the Advancement of Supercritical Fluids).
Responsable formation: Master génie des procédés appliqués au nucléaire.
Editrice associée - Journal of Supercritical Fluids, Elsevier
Activités
Mise en forme de principes actifs
pharmaceutiques en milieu supercritique
Extraction supercritique et
fractionnement supercritique de produits naturels
Stérilisation en
milieu supercritique
Publications scientifiques au M2P2
2024
Aymeric Fabien, Guillaume Lefebvre, Elisabeth Badens, Brice Calvignac, Damien Chaudanson, et al.. Contact angle of ethanol, water, and their mixtures on stainless steel surfaces in dense carbon dioxide. Journal of Colloid and Interface Science, 2024, 655, pp.535-545. ⟨10.1016/j.jcis.2023.10.163⟩. ⟨hal-04316090⟩ Plus de détails...
Hypothesis Contact angle can be a key parameter in chemical engineering. However, the development and the optimization of numerous processes using supercritical CO2, considered as environmentally friendly, requires new measurements under dense CO2 atmosphere. Besides, the influence of the roughness or the wetting regime on the contact angle is known at ambient conditions but remains to be discussed for systems under high pressure. Experimental Contact angle measurements of ethanol, water, and their mixtures, with ethanol mass fractions ranging from 0.25 to 0.75, on two stainless steels in saturated CO2 at pressures ranging from 0.1 MPa to 15.1 MPa, and at 313 K and 333 K were carried out in a set-up improving mass transfer between the studied liquid and the continuous fluid phase. Stainless steel surfaces have been characterized by atomic force and scanning electron microscopies allowing the application of the Wenzel equation. Findings Ethanol wetted totally both stainless steels while contact angles of all other liquids were increased by the rise of pressure, with contact angles up to 128 ° for water at 15.1 MPa. Trapped bubbles were observed at the solid/liquid interface and the bubble formation is discussed. Furthermore, the potential influence of bubble presence on the wetting regime is prospected through the question: could the pressure rise modify the wetting regime?
Aymeric Fabien, Guillaume Lefebvre, Elisabeth Badens, Brice Calvignac, Damien Chaudanson, et al.. Contact angle of ethanol, water, and their mixtures on stainless steel surfaces in dense carbon dioxide. Journal of Colloid and Interface Science, 2024, 655, pp.535-545. ⟨10.1016/j.jcis.2023.10.163⟩. ⟨hal-04316090⟩
Vénicia Numa, Christelle Crampon, Arnaud Bellon, Adil Mouahid, Elisabeth Badens. Valorization of food side streams by supercritical fluid extraction of compounds of interest from apple pomace. Journal of Supercritical Fluids, 2023, 202, pp.106056. ⟨10.1016/j.supflu.2023.106056⟩. ⟨hal-04294235⟩ Plus de détails...
Supercritical CO2 (scCO2) extraction, a green technology still little applied to side streams, has been used to explore the potential recovery of beneficial compounds from apple pomace, a food industry byproduct. The study examines the potential of scCO2 extraction on freeze-dried and airflow dried apple pomace, using laboratory-scale equipment with varying pressures (200–400 bar), temperatures (35–55 °C) with a fixed CO2 flow rate. Extracts were analyzed through LC-MS and GC-MS, while antioxidant capacity was assessed using the ABTS assay. The results were compared to those from Soxhlet n-hexane extraction. Optimal conditions of 300 bar and 55 °C with freeze-dried apple pomace yielded the highest mass loss. The main compounds identified included glyceryl dilinoleate, linoleic acid, and diacyl glycerol, with significant ursolic acid content. A preliminary higher scale feasibility test under optimal conditions demonstrated promising, duplicable outcomes, supporting prior claim that apple pomace contains valuable ingredients that can be reused in various industrial sectors.
Vénicia Numa, Christelle Crampon, Arnaud Bellon, Adil Mouahid, Elisabeth Badens. Valorization of food side streams by supercritical fluid extraction of compounds of interest from apple pomace. Journal of Supercritical Fluids, 2023, 202, pp.106056. ⟨10.1016/j.supflu.2023.106056⟩. ⟨hal-04294235⟩
Vénicia Numa, Christelle Crampon, Arnaud Bellon, Adil Mouahid, Elisabeth Badens. Valorization of food side streams by supercritical fluid extraction of compounds of interest from apple pomace. Journal of Supercritical Fluids, 2023, 202, pp.106056. ⟨10.1016/j.supflu.2023.106056⟩. ⟨hal-04543465⟩ Plus de détails...
Supercritical CO2 (scCO2) extraction, a green technology still little applied to side streams, has been used to explore the potential recovery of beneficial compounds from apple pomace, a food industry byproduct. The study examines the potential of scCO2 extraction on freeze-dried and airflow dried apple pomace, using laboratory-scale equipment with varying pressures (200–400 bar), temperatures (35–55 °C) with a fixed CO2 flow rate. Extracts were analyzed through LC-MS and GC-MS, while antioxidant capacity was assessed using the ABTS assay. The results were compared to those from Soxhlet n-hexane extraction. Optimal conditions of 300 bar and 55 °C with freeze-dried apple pomace yielded the highest mass loss. The main compounds identified included glyceryl dilinoleate, linoleic acid, and diacyl glycerol, with significant ursolic acid content. A preliminary higher scale feasibility test under optimal conditions demonstrated promising, duplicable outcomes, supporting prior claim that apple pomace contains valuable ingredients that can be reused in various industrial sectors.
Vénicia Numa, Christelle Crampon, Arnaud Bellon, Adil Mouahid, Elisabeth Badens. Valorization of food side streams by supercritical fluid extraction of compounds of interest from apple pomace. Journal of Supercritical Fluids, 2023, 202, pp.106056. ⟨10.1016/j.supflu.2023.106056⟩. ⟨hal-04543465⟩
Alejandra Gutiérez Márquez, Gatien Fleury, Alexandra Dimitriades-Lemaire, Pablo Alvarez, Gregory Santander, et al.. Potential of the worldwide-cultivated cyanobacterium Arthrospira platensis for CO2 mitigation: Impacts of photoperiod lengths and abiotic parameters on yield and efficiency. Bioresource Technology Reports, 2023, 22, pp.101439. ⟨10.1016/j.biteb.2023.101439⟩. ⟨hal-04702177⟩ Plus de détails...
This study reports A. platensis capacity to capture and convert CO2 into biomass. The cyanobacterium was cultivated under controlled conditions with a 5 % v/v CO₂-enriched atmosphere at different photoperiods (light/dark): 12 h/12 h, 20 h/4 h, and 24 h (continuous light). The photoperiod influence on biomass growth and its effect on CO₂ uptake was evaluated by analyzing the supernatant dissolved inorganic carbon and nitrate concentration. The experimental dissolved inorganic carbon values were compared with numerical computations obtained from an established model. While the control without biomass stabilized at 36 ± 1.07 mgC/L of dissolved inorganic carbon, the A. platensis cultures stabilized at 675 ± 44.5 mgC/L on average. These results suggest that the alkalinity induced by photosynthesis and nitrate bio-assimilation enhances CO₂ dissolution in the culture medium. The photoperiod increase from 12 h/12 h to 24 h proved to boost the biomass productivity and CO₂ fixation rate from 0.05 to 0.13 g/L/d and 71.92 to 216.84, respectively.
Alejandra Gutiérez Márquez, Gatien Fleury, Alexandra Dimitriades-Lemaire, Pablo Alvarez, Gregory Santander, et al.. Potential of the worldwide-cultivated cyanobacterium Arthrospira platensis for CO2 mitigation: Impacts of photoperiod lengths and abiotic parameters on yield and efficiency. Bioresource Technology Reports, 2023, 22, pp.101439. ⟨10.1016/j.biteb.2023.101439⟩. ⟨hal-04702177⟩
Christelle Crampon, Thibaud Detoisien, Lama Itani, Fréderic Nicolas, Emmanuelle Myotte, et al.. Novel crystal morphology for sodium bicarbonate obtained by using the supercritical anti-solvent process. Powder Technology, 2023, 418, pp.118313. ⟨10.1016/j.powtec.2023.118313⟩. ⟨hal-04546398⟩ Plus de détails...
Adil Mouahid, Magalie Claeys-Bruno, Isabelle Bombarda, Sandrine Amat, Andrea Ciavarella, et al.. Valorization of handmade argan press cake by supercritical CO2 extraction. Food and Bioproducts Processing, 2023, 137, pp.168-176. ⟨10.1016/j.fbp.2022.11.011⟩. ⟨hal-03992094⟩ Plus de détails...
The capability of supercritical CO2 to extract edible oil from handmade Argan press cake was investigated. The aim is to enable Moroccan cooperatives to improve their economic situation by valuing the handmade argan press cake, which is nowadays considered as a waste, applying a clean extraction process. Extraction experiments were conducted at 300 and 400 bar, 333 K and 0.14 kg/h on dried biomass. The fatty acids and tocopherols compositions of the extracted oil were found similar to previous studies and correspond to a commercial edible oil. The air flow dried biomass exhibits a higher extraction yield compared to the freeze-dried biomass. A pressure of 300 bar seems to be suffcient to allow the extraction of oil with a satisfactory extraction kinetic.
Adil Mouahid, Magalie Claeys-Bruno, Isabelle Bombarda, Sandrine Amat, Andrea Ciavarella, et al.. Valorization of handmade argan press cake by supercritical CO2 extraction. Food and Bioproducts Processing, 2023, 137, pp.168-176. ⟨10.1016/j.fbp.2022.11.011⟩. ⟨hal-03992094⟩
Mathieu Martino, Adil Mouahid, Michelle Sergent, Camille Desgrouas, Catherine Badens, et al.. Supercritical millifluidic process for siRNA encapsulation in nanoliposomes for potential Progeria treatment (ex-vivo assays). Journal of Drug Delivery Science and Technology, 2023, 87, ⟨10.1016/j.jddst.2023.104804⟩. ⟨hal-04254108⟩ Plus de détails...
A millifluidic process working in continuous mode for the preparation of nanoliposomes using supercritical CO2 has been developed. Nanoliposomes with an average diameter ranging between 123.9 ± 3.0 and 165.7 ± 1.6 nm depending on the operating conditions were obtained. The effects of pressure (90–150 bar), temperature (35–45 °C) and phospholipid mass ratio (0.1–1.9 wt%) in feed solution on liposome sizes were investigated. The concentration of phospholipids was found to be the most significant parameter for controlling the mean diameter of nanoliposomes while pressure and temperature had a minor influence on liposomes’ properties. The encapsulation of siRNAs targeting the LMNA gene by nanoliposomes obtained with the millifluidic process was achieved at optimized operating conditions (150 bar, 35 °C and a phospholipid mass ratio in the feed solution of 0.1 wt%). The resulting formulations were compared with commercial transfection agents in ex vivo assays. These assays showed a decrease in the expression of the encoded protein lamin A for the formulations obtained with the process developed in this work. Therefore, the use of siRNAs targeting LMNA, encapsulated by nanoliposomes represents a potential new therapeutic approach for the treatment of progeria.
Mathieu Martino, Adil Mouahid, Michelle Sergent, Camille Desgrouas, Catherine Badens, et al.. Supercritical millifluidic process for siRNA encapsulation in nanoliposomes for potential Progeria treatment (ex-vivo assays). Journal of Drug Delivery Science and Technology, 2023, 87, ⟨10.1016/j.jddst.2023.104804⟩. ⟨hal-04254108⟩
Journal: Journal of Drug Delivery Science and Technology
Victorine Warambourg, Adil Mouahid, Christelle Crampon, Anne Galinier, Magalie Claeys-Bruno, et al.. Supercritical CO2 sterilization under low temperature and pressure conditions. Journal of Supercritical Fluids, 2023, 203, pp.106084. ⟨10.1016/j.supflu.2023.106084⟩. ⟨hal-04233306⟩ Plus de détails...
Sterilization using supercritical carbon dioxide has been proven to be efficient for decades now. The aim of this work was to implement a process of sterilization adapted to thermosensitive polymeric materials and highlight the lowest conditions of pressure and temperature which would enable a bacterial reduction higher than 6-log. Inactivation experiments were performed on spores of Bacillus subtilis over a pressure range lying from 60 to 200 bar, and a temperature varying from 35° to 60°C, with and without additive. Preliminary experiments allowed us to determine a restricted experimental domain used for the design of the experiments, investigating the influence of pressure, temperature, process duration, and additive content on bacterial reduction. It was shown that sterilization conducted at 110 bar, 40 °C, for 20 min with 200 ppm of H2O2, leading to a bacterial reduction of 8.73-log, may be considered as optimal for IMD sterilization.
Victorine Warambourg, Adil Mouahid, Christelle Crampon, Anne Galinier, Magalie Claeys-Bruno, et al.. Supercritical CO2 sterilization under low temperature and pressure conditions. Journal of Supercritical Fluids, 2023, 203, pp.106084. ⟨10.1016/j.supflu.2023.106084⟩. ⟨hal-04233306⟩
Elisabeth Badens, Sara Spilimbergo, Lourdes Calvo. Special issue on sterilization with supercritical carbon dioxide. Journal of Supercritical Fluids, 2022, 190, pp.105716. ⟨10.1016/j.supflu.2022.105716⟩. ⟨hal-04063819⟩ Plus de détails...
Elisabeth Badens, Sara Spilimbergo, Lourdes Calvo. Special issue on sterilization with supercritical carbon dioxide. Journal of Supercritical Fluids, 2022, 190, pp.105716. ⟨10.1016/j.supflu.2022.105716⟩. ⟨hal-04063819⟩
Adil Mouahid, Pierre Boivin, Suzanne Diaw, Elisabeth Badens. Widom and extrema lines as criteria for optimizing operating conditions in supercritical processes. Journal of Supercritical Fluids, 2022, 186, pp.105587. ⟨10.1016/j.supflu.2022.105587⟩. ⟨hal-03797377⟩ Plus de détails...
Adil Mouahid, Pierre Boivin, Suzanne Diaw, Elisabeth Badens. Widom and extrema lines as criteria for optimizing operating conditions in supercritical processes. Journal of Supercritical Fluids, 2022, 186, pp.105587. ⟨10.1016/j.supflu.2022.105587⟩. ⟨hal-03797377⟩
Aymeric Fabien, Guillaume Lefebvre, Brice Calvignac, Pierre Legout, Elisabeth Badens, et al.. Interfacial tension of ethanol, water, and their mixtures in high pressure carbon dioxide: measurements and modeling. Journal of Colloid and Interface Science, 2022, 613, pp.847-56. ⟨10.1016/j.jcis.2022.01.058⟩. ⟨hal-03531186⟩ Plus de détails...
Hypothesis: It is particularly noteworthy to study interfacial tension behavior under pressurized carbon dioxide for supercritical processes such as crystallization or fractionation. For the latter, a liquid phase and a supercritical phase are in contact, and interfacial properties influence mass transfer phenomena and hydrodynamics. Ethanol-water mixture is a good theoretical study case also involved in a wide range of applications. Experimental: Interfacial tensions of ethanol, water and three mixtures, with an ethanol mass fraction from 0.25 to 0.75, under pressurized CO 2 were measured for pressures ranging from 0.1 MPa to 15.1 MPa at 313.15 K and 333.15 K. A specific experimental setup was used for CO 2 phase saturation. Findings: This work brings interfacial tension data of five different solutions including water and ethanol in contact with CO 2. Effects of pressure, temperature, carbon dioxide density and ethanol mass fraction are discussed regarding the literature. Significant discrepancies are found with previous literature data for ethanol-water mixtures. The "two-step" decrease observed when pressure or density increase is also discussed regarding both the concept of Widom line, and the polar and dispersive contributions of the surface tension of a component. For the first time, fair accurate interfacial tension modeling involving these contributions is addressed.
Aymeric Fabien, Guillaume Lefebvre, Brice Calvignac, Pierre Legout, Elisabeth Badens, et al.. Interfacial tension of ethanol, water, and their mixtures in high pressure carbon dioxide: measurements and modeling. Journal of Colloid and Interface Science, 2022, 613, pp.847-56. ⟨10.1016/j.jcis.2022.01.058⟩. ⟨hal-03531186⟩
Dao Le, Amélie Frison, Yasmine Masmoudi, Abir Bouledjouidja, Pierre Thureau, et al.. Supercritical CO 2 impregnation process applied to polymer samples preparation for dynamic nuclear polarization solid‐state NMR. Magnetic Resonance in Chemistry, 2022, 60 (12), pp.1171-1177. ⟨10.1002/mrc.5307⟩. ⟨hal-03777975⟩ Plus de détails...
In this study, supercritical CO2 (scCO2) was used to impregnate polymers with paramagnetic polarizing agents to prepare samples for dynamic nuclear polarization (DNP) solid-state NMR (ssNMR) experiments. As a proof of concept, we impregnated polystyrene samples with bTbK, which stands for bis-TEMPO-bisketal where TEMPO is 2,2,6,6-tetra-methylpiperindin-1-oxyl. Substantial DNP signal enhancements could be measured on DNP-enhanced 1H → 13C cross-polarization (CP) magic-angle spinning (MAS) spectra recorded at 9.4 T and ~100 K, reaching a maximum value of 8 in the most favorable case, which appeared comparable or even higher than what is typically obtained on similar systems for former sample preparation methods. These results highlight the potential of scCO2 impregnation as an efficient and possibly versatile methodology to prepare polymer samples for DNP ssNMR investigations.
Dao Le, Amélie Frison, Yasmine Masmoudi, Abir Bouledjouidja, Pierre Thureau, et al.. Supercritical CO 2 impregnation process applied to polymer samples preparation for dynamic nuclear polarization solid‐state NMR. Magnetic Resonance in Chemistry, 2022, 60 (12), pp.1171-1177. ⟨10.1002/mrc.5307⟩. ⟨hal-03777975⟩
Sébastien Clercq, Feral Temelli, Elisabeth Badens. In-Depth Study of Cyclodextrin Complexation with Carotenoids toward the Formation of Enhanced Delivery Systems. Molecular Pharmaceutics, 2021, 18 (4), pp.1720-1729. ⟨10.1021/acs.molpharmaceut.0c01227⟩. ⟨hal-03334353⟩ Plus de détails...
The goal of this study was molecular modeling of cyclodextrin (CD) and carotenoid complex formation. Distinction was made between complexes resulting from interactions between carotenoids and either molecularly dispersed CDs or solid crystalline CDs, considering that both cases can occur depending on the complex formation process pathways. First, the formation of complexes from dispersed CD molecules was investigated considering five different CDs (αCD, βCD, methyl-βCD, hydroxypropyl-βCD, and γCD) and lutein, as a model carotenoid molecule. The interactions involved and the stability of the different complexes formed were evaluated according to the CD size and steric hindrance. Second, the formation of complexes between four different crystalline CDs (βCD with three different water contents and methyl-βCD) and three carotenoid molecules (lutein, lycopene, and β-carotene) was studied. The docking/adsorption of the carotenoid molecules was modeled on the different faces of the CD crystals. The findings highlight that all the CD faces, and thus their growth rates, were equally impacted by the adsorption of the carotenoids. This is due to the fact that all the CD faces are exhibiting similar chemical compositions, the three studied carotenoid molecules are rather chemically similar, and last, the water–carotenoid interactions appear to be weak compared to the CD–carotenoid interactions.
Sébastien Clercq, Feral Temelli, Elisabeth Badens. In-Depth Study of Cyclodextrin Complexation with Carotenoids toward the Formation of Enhanced Delivery Systems. Molecular Pharmaceutics, 2021, 18 (4), pp.1720-1729. ⟨10.1021/acs.molpharmaceut.0c01227⟩. ⟨hal-03334353⟩
Sébastien Clercq, Feral Temelli, Elisabeth Badens. In-Depth Study of Cyclodextrin Complexation with Carotenoids toward the Formation of Enhanced Delivery Systems. Molecular Pharmaceutics, 2021, 18 (4), pp.1720-1729. ⟨10.1021/acs.molpharmaceut.0c01227⟩. ⟨hal-03600451⟩ Plus de détails...
The goal of this study was molecular modeling of cyclodextrin (CD) and carotenoid complex formation. Distinction was made between complexes resulting from interactions between carotenoids and either molecularly dispersed CDs or solid crystalline CDs, considering that both cases can occur depending on the complex formation process pathways. First, the formation of complexes from dispersed CD molecules was investigated considering five different CDs (αCD, βCD, methyl-βCD, hydroxypropyl-βCD, and γCD) and lutein, as a model carotenoid molecule. The interactions involved and the stability of the different complexes formed were evaluated according to the CD size and steric hindrance. Second, the formation of complexes between four different crystalline CDs (βCD with three different water contents and methyl-βCD) and three carotenoid molecules (lutein, lycopene, and β-carotene) was studied. The docking/adsorption of the carotenoid molecules was modeled on the different faces of the CD crystals. The findings highlight that all the CD faces, and thus their growth rates, were equally impacted by the adsorption of the carotenoids. This is due to the fact that all the CD faces are exhibiting similar chemical compositions, the three studied carotenoid molecules are rather chemically similar, and last, the water–carotenoid interactions appear to be weak compared to the CD–carotenoid interactions.
Sébastien Clercq, Feral Temelli, Elisabeth Badens. In-Depth Study of Cyclodextrin Complexation with Carotenoids toward the Formation of Enhanced Delivery Systems. Molecular Pharmaceutics, 2021, 18 (4), pp.1720-1729. ⟨10.1021/acs.molpharmaceut.0c01227⟩. ⟨hal-03600451⟩
Mathieu Martino, Adil Mouahid, Paolo Trucillo, Elisabeth Badens. Elaboration of Lutein‐Loaded Nanoliposomes Using Supercritical CO2. European Journal of Lipid Science and Technology, 2021, 123 (4), pp.2000358. ⟨10.1002/ejlt.202000358⟩. ⟨hal-03334357⟩ Plus de détails...
A batch process for producing lutein-loaded liposomes using supercritical CO2 is studied. The effects of the variation of pressure (10 and 15 MPa), temperature (308, 313, and 318 K), and lutein to lipid ratio (0.5 and 1 wt%) on the liposome average size and size distribution are investigated, as well as on the encapsulation efficiency (EE) of lutein. This process is worked in a repeatable manner and is allowed the production of nanoliposomes with mean diameters (MDs) ranging from 65 ± 33 to 77 ± 40 nm, obtaining lutein EEs ranging from 82.1 ± 3.7% to 91.9 ± 2.9%. Temperature, pressure, and lutein to lipid ratio seem to have no impact on size, size distribution, and EE on formed liposomes. The use of low temperatures and low pressures allows the obtainment of liposomes with diameters less than 100 nm and limits the process energy cost. Moreover, the supercritical CO2-assisted batch process effectively encapsulates lutein into liposome, an antioxidant molecule used for the prevention of retinal damage. Liposomes formed by this supercritical process have the desired characteristics for human target delivery. Practical applications: This work on the optimization of a process for developing liposomes in a supercritical environment has applications in medicine. Indeed, the liposomes formed with this process are nanoliposomes with a size of less than 80 nm. In addition, excellent lutein EEs (hydrophobic molecules) show that the liposomes formed constitute excellent coating matrices for the protection of active ingredients. These reasons make these liposome matrices applicable in nanomedicine (injection of sensitive drugs requiring protection before injection). The elaboration process also makes it possible to form liposomes with desired properties by changing pressure, temperature, or lecithin concentration. Therefore, this work focuses on the properties of liposomes as a function of the operating conditions.
Mathieu Martino, Adil Mouahid, Paolo Trucillo, Elisabeth Badens. Elaboration of Lutein‐Loaded Nanoliposomes Using Supercritical CO2. European Journal of Lipid Science and Technology, 2021, 123 (4), pp.2000358. ⟨10.1002/ejlt.202000358⟩. ⟨hal-03334357⟩
Journal: European Journal of Lipid Science and Technology
Mathieu Martino, Adil Mouahid, Paolo Trucillo, Elisabeth Badens. Elaboration of Lutein‐Loaded Nanoliposomes Using Supercritical CO2. European Journal of Lipid Science and Technology, 2021, 123 (4), pp.2000358. ⟨10.1002/ejlt.202000358⟩. ⟨hal-03597665⟩ Plus de détails...
A batch process for producing lutein-loaded liposomes using supercritical CO2 is studied. The effects of the variation of pressure (10 and 15 MPa), temperature (308, 313, and 318 K), and lutein to lipid ratio (0.5 and 1 wt%) on the liposome average size and size distribution are investigated, as well as on the encapsulation efficiency (EE) of lutein. This process is worked in a repeatable manner and is allowed the production of nanoliposomes with mean diameters (MDs) ranging from 65 ± 33 to 77 ± 40 nm, obtaining lutein EEs ranging from 82.1 ± 3.7% to 91.9 ± 2.9%. Temperature, pressure, and lutein to lipid ratio seem to have no impact on size, size distribution, and EE on formed liposomes. The use of low temperatures and low pressures allows the obtainment of liposomes with diameters less than 100 nm and limits the process energy cost. Moreover, the supercritical CO2-assisted batch process effectively encapsulates lutein into liposome, an antioxidant molecule used for the prevention of retinal damage. Liposomes formed by this supercritical process have the desired characteristics for human target delivery. Practical applications: This work on the optimization of a process for developing liposomes in a supercritical environment has applications in medicine. Indeed, the liposomes formed with this process are nanoliposomes with a size of less than 80 nm. In addition, excellent lutein EEs (hydrophobic molecules) show that the liposomes formed constitute excellent coating matrices for the protection of active ingredients. These reasons make these liposome matrices applicable in nanomedicine (injection of sensitive drugs requiring protection before injection). The elaboration process also makes it possible to form liposomes with desired properties by changing pressure, temperature, or lecithin concentration. Therefore, this work focuses on the properties of liposomes as a function of the operating conditions.
Mathieu Martino, Adil Mouahid, Paolo Trucillo, Elisabeth Badens. Elaboration of Lutein‐Loaded Nanoliposomes Using Supercritical CO2. European Journal of Lipid Science and Technology, 2021, 123 (4), pp.2000358. ⟨10.1002/ejlt.202000358⟩. ⟨hal-03597665⟩
Journal: European Journal of Lipid Science and Technology
Adil Mouahid, Isabelle Bombarda, Magalie Claeys-Bruno, Sandrine Amat, Emmanuelle Myotte, et al.. Supercritical CO2 extraction of Moroccan argan (Argania spinosa L.) oil: Extraction kinetics and solubility determination. Journal of CO2 Utilization, 2021, 46, pp.101458. ⟨10.1016/j.jcou.2021.101458⟩. ⟨hal-03142714⟩ Plus de détails...
Experimental and modelling investigations of supercritical CO 2 extraction of oil from Argania spinosa L. kernels were conducted at pressure range from 200 to 400 bar, temperature range of 313-333 K at a CO 2 flow rate of 0.14 kg/h. Regardless of the pressure and the temperature, the highest achievable yield was estimated at 0.63 kg oil / kg biomass. The extraction kinetics were modeled with Sovová's broken and intact cells model. The extraction of type B was found to be the most suited extraction type. Argan oil solubility in supercritical CO 2 was determined and modelled with the Chrastil equation. A retrograde solubility behaviour was observed at 200 bar and the faster extraction kinetics were found at 400 bar and 333 K. The total tocopherols concentration was found between 389.7 and 1688.6 mg/kg extract. Experiments were performed on unroasted and roasted kernels.
Adil Mouahid, Isabelle Bombarda, Magalie Claeys-Bruno, Sandrine Amat, Emmanuelle Myotte, et al.. Supercritical CO2 extraction of Moroccan argan (Argania spinosa L.) oil: Extraction kinetics and solubility determination. Journal of CO2 Utilization, 2021, 46, pp.101458. ⟨10.1016/j.jcou.2021.101458⟩. ⟨hal-03142714⟩
Sébastien Clercq, Adil Mouahid, Gérard Pèpe, Elisabeth Badens. Prediction of Crystal–Solvent Interactions in a Supercritical Medium: A Possible Way to Control Crystal Habit at High Supersaturations with Molecular Modeling. Crystal Growth & Design, 2020, 20 (10), pp.6863-6876. ⟨10.1021/acs.cgd.0c00920⟩. ⟨hal-03334336⟩ Plus de détails...
The purpose of this work is to contribute to a better control of the crystallization process which occurs in a supercritical medium, especially during the Supercritical AntiSolvent (SAS) process. It also aims to improve the prediction of crystal habit, thanks to the use of the molecular modeling software GenMol. The first part of the work was devoted to the crystal modeling of the two main forms of sulfathiazole in vacuo, considering Hartman’s attachment energy formalism. The second part considers solvent–crystal interactions throughout adsorption simulations to investigate the effect of growth environments on crystal habits. Lastly, modeling predictions were compared with grown crystals of sulfathiazole, observed after recrystallization with the SAS process from acetonitrile, acetone, tetrahydrofuran and acetic acid solutions. These comparisons demonstrated good predictions of crystal habit taking into consideration the growth environment. Neither carbon dioxide (antisolvent of the SAS process) nor acetonitrile leads to a modification of the isometric, in vacuo predicted habit of both forms. Acetone and tetrahydrofuran adsorb preferentially on some identified faces and lead to flat, leaflike, or tabular crystals. Acetic acid adsorbs on every one of the faces and hinders the phase transition to a more stable form, thus leading to crystals of the least stable, kinetically favored form I. Experimental observations were also rationalized by considering the different possible crystallization pathways, in particular Crystallization by Particle Attachment and Droplet Drying mechanisms occurring in the SAS process. This work confirms that solvent nature is one of the key elements to consider in order to better control the characteristics of particles grown using the SAS process and provides a new method to help to control it.
Sébastien Clercq, Adil Mouahid, Gérard Pèpe, Elisabeth Badens. Prediction of Crystal–Solvent Interactions in a Supercritical Medium: A Possible Way to Control Crystal Habit at High Supersaturations with Molecular Modeling. Crystal Growth & Design, 2020, 20 (10), pp.6863-6876. ⟨10.1021/acs.cgd.0c00920⟩. ⟨hal-03334336⟩
Kanjana Ongkasin, Yasmine Masmoudi, Thierry Tassaing, Gwenaelle Le-Bourdon, Elisabeth Badens. Supercritical loading of gatifloxacin into hydrophobic foldable intraocular lenses - Process control and optimization by following in situ CO2 sorption and polymer swelling. International Journal of Pharmaceutics, 2020, 581, pp.119247. ⟨10.1016/j.ijpharm.2020.119247⟩. ⟨hal-02513973⟩ Plus de détails...
The supercritical impregnation process was used as a green technology for the elaboration of drug delivery intraocular lenses to mitigate the risk of post-operatory endophthalmitis after cataract surgery. Commercially available hydrophobic acrylic (copolymer of benzyl methacrylate and methyl methacrylate) intraocular lenses (IOLs) were impregnated with gatifloxacin, a fourth generation fluoroquinolone drug, using pure supercritical CO 2 (scCO 2) to obtain solvent-free loaded implants. The interaction phenomena involved in the supercritical impregnation were studied by following in situ scCO 2 sorption within the polymer support and the subsequent IOL swelling, and by taking into account drug solubility in the supercritical fluid phase. The drug impregnation yields determined though in-vitro release studies varied between 0.33 and 1.07 ± 0.07 μg•mg −1 IOL in the studied experimental conditions (8 to 25 MPa, 308 to 328 K and 30 to 240 min impregnation duration). An impregnation duration longer or equal to the time required for a complete CO 2 uptake by the polymer as well as a higher pressure or a higher temperature over the crossover pressure delimiting the upper limit of the retrograde solubility zone, led to higher drug impregnation yields.
Kanjana Ongkasin, Yasmine Masmoudi, Thierry Tassaing, Gwenaelle Le-Bourdon, Elisabeth Badens. Supercritical loading of gatifloxacin into hydrophobic foldable intraocular lenses - Process control and optimization by following in situ CO2 sorption and polymer swelling. International Journal of Pharmaceutics, 2020, 581, pp.119247. ⟨10.1016/j.ijpharm.2020.119247⟩. ⟨hal-02513973⟩
C. Dufour, Christelle Crampon, C. Delbecque, P-P. Garry, Elisabeth Badens. Sclareol purification using the supercritical fractionation process: A modeling case study. Journal of Supercritical Fluids, 2020, 159, pp.104754. ⟨10.1016/j.supflu.2020.104754⟩. ⟨hal-02892487⟩ Plus de détails...
The aim of this study was to model experimental results obtained for the supercritical CO2 fractionation of a liquid mixture containing 24% of sclareol in order to recover a raffinate with increased sclareol content. First, supercritical CO2 fractionation experiments were carried out at pressures (10-12) MPa, and temperatures (313-338) K. Secondly, the modeling of the raffinate and extract compositions for 12 selected compounds including sclareol was performed using the group method. The modeling was carried out at a temperature of 323 K and pressures of (10-11) MPa, and at a temperature of 338 K and a pressure of 12 MPa. The calculation of the raffinate and extract compositions required the adjustment of the number of theoretical stages and of the distribution coefficients for the selected compounds. Experimental raffinate and extract compositions were represented by the model with a relative error of about 15%.
C. Dufour, Christelle Crampon, C. Delbecque, P-P. Garry, Elisabeth Badens. Sclareol purification using the supercritical fractionation process: A modeling case study. Journal of Supercritical Fluids, 2020, 159, pp.104754. ⟨10.1016/j.supflu.2020.104754⟩. ⟨hal-02892487⟩
Kanjana Ongkasin, Yasmine Masmoudi, Christian Wertheimer, Anna Hillenmayer, Kirsten Eibl-Lindner, et al.. Supercritical fluid technology for the development of innovative ophthalmic medical devices: Drug loaded intraocular lenses to mitigate posterior capsule opacification. European Journal of Pharmaceutics and Biopharmaceutics, 2020, 149, pp.248-256. ⟨10.1016/j.ejpb.2020.02.011⟩. ⟨hal-02513976⟩ Plus de détails...
Kanjana Ongkasin, Yasmine Masmoudi, Christian Wertheimer, Anna Hillenmayer, Kirsten Eibl-Lindner, et al.. Supercritical fluid technology for the development of innovative ophthalmic medical devices: Drug loaded intraocular lenses to mitigate posterior capsule opacification. European Journal of Pharmaceutics and Biopharmaceutics, 2020, 149, pp.248-256. ⟨10.1016/j.ejpb.2020.02.011⟩. ⟨hal-02513976⟩
Journal: European Journal of Pharmaceutics and Biopharmaceutics
Adil Mouahid, Kanitta Seengeon, Mathieu Martino, Christelle Crampon, Avery Kramer, et al.. Selective extraction of neutral lipids and pigments from Nannochloropsis salina and Nannochloropsis maritima using supercritical CO2 extraction: Effects of process parameters and pre-treatment. Journal of Supercritical Fluids, 2020, 165, pp.104934. ⟨10.1016/j.supflu.2020.104934⟩. ⟨hal-03232116⟩ Plus de détails...
Supercritical CO2 extraction experiments were conducted to investigate the effects of pretreatment and process parameters on neutral lipids, chlorophylls and carotenoids recovery on two species of Nannochloropsis. For Nannochloropsis maritima, a factorial experimental design was performed (P: [100-300] bar, T: [313-333] K). The highest extraction yields were obtained at the highest pressures and temperatures. Two drying modes, ring drying and air flow drying, were compared. Although total extraction yield and extraction kinetics were observed to be greater using air flow dried microalgae, extracts from this drying method resulted in partial degradation of glycerides in free fatty acids. Ring dried extracts maintained the same neutral lipid composition as the initial biomass. Based on these results, ring dried Nannochloropsis salina was extracted using supercritical CO2 at 333 K and both 300-400 bar. Extraction curves were modelled using the Sovova's mathematical model.
Adil Mouahid, Kanitta Seengeon, Mathieu Martino, Christelle Crampon, Avery Kramer, et al.. Selective extraction of neutral lipids and pigments from Nannochloropsis salina and Nannochloropsis maritima using supercritical CO2 extraction: Effects of process parameters and pre-treatment. Journal of Supercritical Fluids, 2020, 165, pp.104934. ⟨10.1016/j.supflu.2020.104934⟩. ⟨hal-03232116⟩
Adil Mouahid, Kanitta Seengeon, Mathieu Martino, Christelle Crampon, Avery Kramer, et al.. Selective extraction of neutral lipids and pigments from Nannochloropsis salina and Nannochloropsis maritima using supercritical CO2 extraction: Effects of process parameters and pre-treatment. Journal of Supercritical Fluids, 2020, 165, pp.104934. ⟨10.1016/j.supflu.2020.104934⟩. ⟨hal-02960133⟩ Plus de détails...
Supercritical CO2 extraction experiments were conducted to investigate the effects of pretreatment and process parameters on neutral lipids, chlorophylls and carotenoids recovery on two species of Nannochloropsis. For Nannochloropsis maritima, a factorial experimental design was performed (P: [100-300] bar, T: [313-333] K). The highest extraction yields were obtained at the highest pressures and temperatures. Two drying modes, ring drying and air flow drying, were compared. Although total extraction yield and extraction kinetics were observed to be greater using air flow dried microalgae, extracts from this drying method resulted in partial degradation of glycerides in free fatty acids. Ring dried extracts maintained the same neutral lipid composition as the initial biomass. Based on these results, ring dried Nannochloropsis salina was extracted using supercritical CO2 at 333 K and both 300-400 bar. Extraction curves were modelled using the Sovova's mathematical model.
Adil Mouahid, Kanitta Seengeon, Mathieu Martino, Christelle Crampon, Avery Kramer, et al.. Selective extraction of neutral lipids and pigments from Nannochloropsis salina and Nannochloropsis maritima using supercritical CO2 extraction: Effects of process parameters and pre-treatment. Journal of Supercritical Fluids, 2020, 165, pp.104934. ⟨10.1016/j.supflu.2020.104934⟩. ⟨hal-02960133⟩
Joana Silva, Salah Akkache, Ana Araújo, Yasmine Masmoudi, Rui Reis, et al.. Development of innovative medical devices by dispersing fatty acid eutectic blend on gauzes using supercritical particle generation processes. Materials Science and Engineering: C, 2019, 99, pp.599-610. ⟨hal-02016548⟩ Plus de détails...
Joana Silva, Salah Akkache, Ana Araújo, Yasmine Masmoudi, Rui Reis, et al.. Development of innovative medical devices by dispersing fatty acid eutectic blend on gauzes using supercritical particle generation processes. Materials Science and Engineering: C, 2019, 99, pp.599-610. ⟨hal-02016548⟩
Alessia Di Capua, Renata Adami, Emanuela Cosenza, Vincent Jalaber, Christelle Crampon, et al.. β-Carotene/PVP microspheres produced by Supercritical Assisted Atomization. Powder Technology, 2019, 346, pp.228-236. ⟨10.1016/j.powtec.2019.01.069⟩. ⟨hal-02176986⟩ Plus de détails...
Beta-carotene (BC) is one of the best known and used bioactive compounds with antioxidant activity. In this work coprecipitation of BC with polyvinylpyrrolidone (PVP) by Supercritical Assisted Atomization (SAA) has been studied. to enhance BC bioavailability and to provide its protection against oxidation. Two solvents have been used: ethanol and a mixture acetone/ethanol 70/30 (v/v). In both cases SAA produced spherical and amorphous microspheres with d(50) ranging between 0.42 and 0.84 mu m using ethanol, and 0.28 and 0.48 mu m using the solvent mixture. UV-vis analyses revealed a BC content up to 94% and high scavenging activities confirm that PVP is able to protect it from degradation. BC dissolution rate in a phosphate buffered saline solution (PBS) was up to 22 times faster than that of physical mixture. The major difference between coprecipitates was in their dissolution rate: it depended also on the kind solvent used, indicating a possible different internal particles organization during droplet drying.
Alessia Di Capua, Renata Adami, Emanuela Cosenza, Vincent Jalaber, Christelle Crampon, et al.. β-Carotene/PVP microspheres produced by Supercritical Assisted Atomization. Powder Technology, 2019, 346, pp.228-236. ⟨10.1016/j.powtec.2019.01.069⟩. ⟨hal-02176986⟩
Kanjana Ongkasin, Martial Sauceau, Yasmine Masmoudi, Jacques Fages, Elisabeth Badens. Solubility of cefuroxime axetil in supercritical CO2: measurement and modeling. Journal of Supercritical Fluids, 2019, 152, pp.art.104498. ⟨10.1016/j.supflu.2019.03.010⟩. ⟨hal-02125332⟩ Plus de détails...
In this study, an analytical dynamic method was optimized for small amounts of drugs and used to measure the solubility of cefuroxime axetil in supercritical CO2. After validating the experimental procedure with nimesulide, an active ingredient already studied in the literature, the solubility of cefuroxime axetil in supercritical CO2 was measured at temperatures varying from 308 to 328 K and pressures ranging between 8 and 25 MPa. Experimental values varied between 2.2 × 10-7 and 11.24 × 10-6 (in mole fraction) and a retrograde solubility behavior was observed. The solubility was correlated with semi-empirical density-based models: Kumar and Johnston, Mendez-Santiago and Teja, and Chrastil models. All three models successfully correlated the solubilities of cefuroxime axetil with an average deviation lower than 15 %.
Kanjana Ongkasin, Martial Sauceau, Yasmine Masmoudi, Jacques Fages, Elisabeth Badens. Solubility of cefuroxime axetil in supercritical CO2: measurement and modeling. Journal of Supercritical Fluids, 2019, 152, pp.art.104498. ⟨10.1016/j.supflu.2019.03.010⟩. ⟨hal-02125332⟩
I. García-Casas, Christelle Crampon, A. Montes, C. Pereyra, E.J. Martínez de La Ossa, et al.. Supercritical CO2 impregnation of silica microparticles with quercetin. Journal of Supercritical Fluids, 2019, 143, pp.157-161. ⟨hal-01946903⟩ Plus de détails...
Supercritical carbon dioxide has been used to develop two methods for the impregnation of porous silica beads with a natural antioxidant, quercetin. These methods involved batch and semi-continuous supercritical impregnations. The first experiments performed in batch mode helped to understand the influence of pressure, temperature, duration, and the presence of a co-solvent on the impregnation efficiency. A co-solvent was added due to the low solubility of quercetin in supercritical CO2 under the operating conditions studied. In the range of temperatures and pressures studied, the best operating conditions, i.e., those that led to the highest quantity of quercetin impregnated (300 mu g of quercetin per g of silica), were 10 MPa and 323 K with ethanol as co-solvent for 2 h. These operating conditions, highlighted through the batch mode experiments, were subsequently applied to the semi-continuous process. This approach provided an impregnation ratio of 240 mu g of quercetin per g of silica.
I. García-Casas, Christelle Crampon, A. Montes, C. Pereyra, E.J. Martínez de La Ossa, et al.. Supercritical CO2 impregnation of silica microparticles with quercetin. Journal of Supercritical Fluids, 2019, 143, pp.157-161. ⟨hal-01946903⟩
Elisabeth Badens, Stéphane Sarrade, Jacques Fages, Gerd Brunner, Erdogan Kiran. In memoriam Prof. Dr. Michel Perrut (March 29, 1947–July 7, 2018). Journal of Supercritical Fluids, 2019, 145, pp.A1-A2. ⟨10.1016/j.supflu.2018.12.015⟩. ⟨hal-01980378⟩ Plus de détails...
Elisabeth Badens, Stéphane Sarrade, Jacques Fages, Gerd Brunner, Erdogan Kiran. In memoriam Prof. Dr. Michel Perrut (March 29, 1947–July 7, 2018). Journal of Supercritical Fluids, 2019, 145, pp.A1-A2. ⟨10.1016/j.supflu.2018.12.015⟩. ⟨hal-01980378⟩
Adil Mouahid, Halima Bouanga, Christelle Crampon, Elisabeth Badens. Supercritical CO2 extraction of oil from Jatropha curcas: An experimental and modelling study. Journal of Supercritical Fluids, 2018, 141, pp.2-11. ⟨10.1016/j.supflu.2017.11.014⟩. ⟨hal-02114700⟩ Plus de détails...
Experimental and modelling investigations of supercritical CO 2 extraction of oil from Jatropha curcas were conducted at a pressure range of 20-40 MPa and a temperature range of 313-333 K at a CO 2 flow rate of 0.4 kg/ h. The extraction yield was estimated to be about 0.6 kg oil /kg biomass for all experiments. The model of broken and intact cells published by Sovová was applied. It was found that the extraction of type B was the most suited extraction type to apply as the experimental extraction curves exhibit three parts. Whatever the pressure and the temperature applied, the asymptotic yield at infinite time was found to be the same. At 20 MPa, increasing the temperature from 313 to 323 K enhances the extraction kinetics. A retrograde solubility zone was found at 30 and 40 MPa. The Jatropha curcas oil solubility in SC-CO 2 was determined and the data were modelled with the Chrastil equation.
Adil Mouahid, Halima Bouanga, Christelle Crampon, Elisabeth Badens. Supercritical CO2 extraction of oil from Jatropha curcas: An experimental and modelling study. Journal of Supercritical Fluids, 2018, 141, pp.2-11. ⟨10.1016/j.supflu.2017.11.014⟩. ⟨hal-02114700⟩
Sébastien Clercq, Adil Mouahid, Pèpe Gérard, Elisabeth Badens. Investigation of crystallization mechanisms for polymorphic and habit control from the Supercritical AntiSolvent process. Journal of Supercritical Fluids, 2018, 141, pp.29-38. ⟨10.1016/j.supflu.2017.11.025⟩. ⟨hal-02113962⟩ Plus de détails...
In this work, the Supercritical AntiSolvent (SAS) process has been used to generate micronized crystals of Sulfathiazole (STZ) from different organic solutions, namely acetone, acetonitrile, tetrahydrofuran and acetic acid. The flow rates of CO2 (2–21 g min−1) and of the organic solution (0.19–6 mL min−1), as well as STZ concentration in the organic solution (20–70% under the saturation), have been varied to identify the conditions leading to powders exhibiting only one polymorphic form. Pressure (10 MPa) and temperature (313 K) have been kept constant. In this paper, thermodynamic and hydrodynamic aspects are discussed so as to rationalize the obtained crystal characteristics and provide a new way to control the SAS process applied to drug pre-formulation. The influence of the organic solvent nature on both the polymorphic form and the habit of generated crystals, has been particularly discussed.
Sébastien Clercq, Adil Mouahid, Pèpe Gérard, Elisabeth Badens. Investigation of crystallization mechanisms for polymorphic and habit control from the Supercritical AntiSolvent process. Journal of Supercritical Fluids, 2018, 141, pp.29-38. ⟨10.1016/j.supflu.2017.11.025⟩. ⟨hal-02113962⟩
Elisabeth Badens, Yasmine Masmoudi, Adil Mouahid, Christelle Crampon. Current situation and perspectives in drug formulation by using supercritical fluid technology. Journal of Supercritical Fluids, 2018, 134, pp.274-283. ⟨10.1016/j.supflu.2017.12.038⟩. ⟨hal-02111546⟩ Plus de détails...
Supercritical fluid (SCF) technology has been applied to drug product development over the last thirty years and drug particle generation using SCFs appears to be an efficient way to carry out drug formulation which will form end-products meeting targeted specifications. This article presents an overview of drug particle design using SCFs from a rather different perspective than usual, more focused on chemical and process engineering aspects. The main types of existing processes are described in a concise way and a focus is put on how to choose the right operating conditions considering both thermodynamic and hydrodynamic aspects. It is shown that the operating conditions and parameters can be easily optimized so as to facilitate the further process scale-up. Furthermore, the new trends in particle generation using SCFs are introduced, related either to new types of drug medicines that are treated or new ways of process implementation methods.
Elisabeth Badens, Yasmine Masmoudi, Adil Mouahid, Christelle Crampon. Current situation and perspectives in drug formulation by using supercritical fluid technology. Journal of Supercritical Fluids, 2018, 134, pp.274-283. ⟨10.1016/j.supflu.2017.12.038⟩. ⟨hal-02111546⟩
Frederique Bertaud, Christelle Crampon, Elisabeth Badens. Volatile terpene extraction of spruce, fir and maritime pine wood: supercritical CO2 extraction compared to classical solvent extractions and steam distillation
. Holzforschung, 2017, 71 (7-8), pp.667-763. ⟨10.1515/hf-2016-0197⟩. ⟨hal-01596420⟩ Plus de détails...
Frederique Bertaud, Christelle Crampon, Elisabeth Badens. Volatile terpene extraction of spruce, fir and maritime pine wood: supercritical CO2 extraction compared to classical solvent extractions and steam distillation
. Holzforschung, 2017, 71 (7-8), pp.667-763. ⟨10.1515/hf-2016-0197⟩. ⟨hal-01596420⟩
Adil Mouahid, Cyril Dufour, Elisabeth Badens. Supercritical CO 2 extraction from endemic Corsican plants; comparison of oil composition and extraction yield with hydrodistillation method. Journal of CO2 Utilization, 2017, 20, pp.263 - 273. ⟨10.1016/j.jcou.2017.06.003⟩. ⟨hal-01596432⟩ Plus de détails...
Generally speaking, essential oils (EOs) and components of interest are extracted from plants using hydrodistillation (HD), steam distillation or organic solvent methods The Supercritical CO2 (SC-CO2) extraction technique is a good alternative to the three previously mentioned methods as it is able to be applied at temperatures close to ambient and shows no toxicity to humans or the environment. The aim of this study is to investigate the ability of supercritical CO2 extraction to extract bioactive components from four Corsican endemic plants: Rosmarinus officinalis, Juniperus communis ssp nana, Helichrysum italicum and Pistacia lentiscus. After the extracts were analyzed by gas chromatography, it would appear that SC-CO2 is the most adapted process for the extraction of such components of interest as verbenone, germacrene D, bornyl acetate, ferruginol, transcaryophyllene, elemol,gamma-cadinene, geraniol or beta-eudesmol in higher quantity. The SC-CO2 extraction curves were obtained using two models published by Sovova. These models give access to complementary information and help to estimate the values of some important data such as the possible maximal extraction yield for Helichrysum italicum and the end of the extraction period.
Adil Mouahid, Cyril Dufour, Elisabeth Badens. Supercritical CO 2 extraction from endemic Corsican plants; comparison of oil composition and extraction yield with hydrodistillation method. Journal of CO2 Utilization, 2017, 20, pp.263 - 273. ⟨10.1016/j.jcou.2017.06.003⟩. ⟨hal-01596432⟩
Abir Bouledjouidja, Yasmine Masmoudi, M. Sergent, Elisabeth Badens. Effect of operational conditions on the supercritical carbon dioxide impregnation of anti-inflammatory and antibiotic drugs in rigid commercial intraocular lenses. Journal of Supercritical Fluids, 2017, 130, pp.63 - 75. ⟨10.1016/j.supflu.2017.07.015⟩. ⟨hal-01578745⟩ Plus de détails...
Drug/lense combinations have proven significant in the field of ocular therapeutics. The development of innovative systems and elaboration processes is an upcoming issue for ocular drug delivery. One challenging issue is the elaboration of drug loaded intraocular lenses (IOLs) to combine cataract surgery and post-operative treatments in a single procedure. In this work, we are studying the elaboration of such systems while using a green process using supercritical fluids for impregnating ophthalmic drugs on commercial IOLs. More particularly, rigid commercial intraocular lenses made from Poly (Methyl MethAcrylate) (PMMA), used in cataract surgery, are loaded with dexamethasone 21- phosphate disodium salt (DXP, an anti-inflammatory drug) and ciprofloxacin (CIP, an antibiotic) in order to prevent short- and mid-term postoperative complications. Supercritical impregnations were carried out in a batch mode and impregnation yields were determined through drug release kinetic studies in a solution simulating the aqueous humor. Before performing an experimental design, preliminary impregnation assays were conducted in order to delimit the operating domain. Transparent IOLs presenting an effective impregnation were obtained. The highest impregnation yields for DXP and CIP in PMMA IOLs were 18.3 and 2.8 μgdrug/mgIOL respectively. Despite the low solubility of each drug in the fluid phase, homogeneous and in-depth impregnations were successfully obtained with a prolonged drug delivery (about 40 days) for most impregnation experiments.
Abir Bouledjouidja, Yasmine Masmoudi, M. Sergent, Elisabeth Badens. Effect of operational conditions on the supercritical carbon dioxide impregnation of anti-inflammatory and antibiotic drugs in rigid commercial intraocular lenses. Journal of Supercritical Fluids, 2017, 130, pp.63 - 75. ⟨10.1016/j.supflu.2017.07.015⟩. ⟨hal-01578745⟩
C. Dufour, Christelle Crampon, C. Delbecque, P-P. Garry, Elisabeth Badens. Purification of sclareol by supercritical CO2 fractionation process. Journal of Supercritical Fluids, 2017, 122, pp.35 - 42. ⟨10.1016/j.supflu.2016.12.001⟩. ⟨hal-01596425⟩ Plus de détails...
The implementation and optimization of continuous supercritical CO2 fractionation of a clary sage extract containing 25 wt% of sclareol were performed in order to increase its sclareol content. After preliminary experiments confirming the feasibility of the process, different operating conditions were studied: CO(2-)over-feed mass ratio from 25 up to 115, and pressure between 11 and 13 MPa, with an internal reflux due to a thermal gradient 323-338 K along the column, through an experimental design. Four responses were highlighted: sclareol mass fraction in the raffinate, sclareol mass fraction in the extract, sclareol yield in the raffinate, and the amount of an undesirable compound exhibiting a similar behaviour to sclareol and thus, hard to separate from sclareol by conventional techniques. This work allowed us to highlight the best operating conditions: a pressure of 12.6 MPa and a CO2-over-feed mass ratio of 114.5 leading to a sclareol mass fraction in raffinate and extract of 75.3% and 4.6% respectively, to a sclareol yield of 82.4% in the raffinate, and to an amount of 0.08% of the undesirable compound in the raffinate.
C. Dufour, Christelle Crampon, C. Delbecque, P-P. Garry, Elisabeth Badens. Purification of sclareol by supercritical CO2 fractionation process. Journal of Supercritical Fluids, 2017, 122, pp.35 - 42. ⟨10.1016/j.supflu.2016.12.001⟩. ⟨hal-01596425⟩
This article deals with the extraction of neutral lipids andă antioxidants from enriched Spirulina platensis microalgae usingă supercritical carbon dioxide (CO2), and more particularly with theă influence of experimental conditions on extraction yields and kineticsă at laboratory and pilot scales. Preliminary studies were carried out ată laboratory scale before the establishment of an experimental design:ă extraction curves were plotted for different autoclave fill rates, andă under different conditions of pressure and temperature. Using a Responseă Surface Methodology, the significant influence of pressure on extractionă efficiency was highlighted. Surface responses showed that, in theă studied experimental field, mass loss increased when pressure,ă temperature, and CO2/microalgae mass ratio increased. Extract analysesă showed that oil extracts contained chlorophylls a and b, as well asă beta-carotene. Finally, larger-scale experiments were carried out withă batches of 1 and 50 kg (scale-factors of 100 and 5000, respectively) andă the results were consistent with those obtained at laboratory scale. (C)ă 2016 Elsevier B.V. All rights reserved.
Rania Djerafi, Andri Swanepoel, Christelle Crampon, Lonji Kalombo, Philip Labuschagne, et al.. Supercritical antisolvent co-precipitation of rifampicin and ethyl cellulose. European Journal of Pharmaceutical Sciences, 2017, 102, pp.161 - 171. ⟨10.1016/j.ejps.2017.03.016⟩. ⟨hal-01524709⟩ Plus de détails...
Adil Mouahid, Christelle Crampon, Sid-Ali Amine Toudji, Elisabeth Badens. Effects of high water content and drying pre-treatment on supercritical CO2 extraction from Dunaliella salina microalgae: Experiments and modelling. Journal of Supercritical Fluids, 2016, 116, pp.271-280. ⟨10.1016/j.supflu.2016.06.007⟩. ⟨hal-01461796⟩ Plus de détails...
This study investigates the effects due to the water content and to the drying pre-treatment on the extraction kinetics of solutes extracted from Dunaliella sauna microalgae by supercritical CO2. The extraction experiments were conducted at pressure range from 20 up to 40 MPa at a temperature of 333 K on crushed samples with water content varying from 5.5 up to 23 wt%. Three drying pre-treatments were applied: air flow drying at 318 K, air flow drying followed by additional microwave treatment and freeze-drying. A water content up to 23 wt% helps to extract a higher content of carotenoids (mainly beta-carotene) and does not restrict the extraction process. Sovova's mathematical model was applied and the parameters were adapted for the description of the extraction curves from samples containing high water content with a deviation between experimental and calculated values comprised between 1.1% and 4.3%. (C) 2016 Elsevier B.V. All rights reserved.
Adil Mouahid, Christelle Crampon, Sid-Ali Amine Toudji, Elisabeth Badens. Effects of high water content and drying pre-treatment on supercritical CO2 extraction from Dunaliella salina microalgae: Experiments and modelling. Journal of Supercritical Fluids, 2016, 116, pp.271-280. ⟨10.1016/j.supflu.2016.06.007⟩. ⟨hal-01461796⟩
Ahmed Zermane, Ouassila Larkeche, Abdeslam-Hassen Meniai, Christelle Crampon, Elisabeth Badens. Optimization of Algerian rosemary essential oil extraction yield by supercritical CO2 using response surface methodology. Comptes Rendus. Chimie, 2016, 19 (4), pp.538-543. ⟨10.1016/j.crci.2015.08.011⟩. ⟨hal-01461780⟩ Plus de détails...
The present study deals with the determination of optimal values of operating parameters such as temperature and pressure leading to the best yield of a supercritical CO2 extraction of essential oil from local rosemary plants, using the response surface methodology (RSM). The maximum of essential oil recovery percentage relative to the initial mass of leaf powder was 3.52 wt%, and was obtained at 313 K and 22 MPa. A second-order polynomial was used to express the oil recovery and the calculated mass of recovered oil using the RSM was very close to the experimental value, confirming the reliability of this technique. The chemical composition of the Algerian rosemary oil under the obtained optimal conditions (313 K and 22 MPa), determined by GC-MS analysis, revealed the presence of camphor (major compound) (52.12%), 1,8-cineole (9.65%), camphene (7.55%), alpha-pinene (6.05%), borneol (3.52%), aroma dendrene (2.11%), verbenone (1.97%), alpha-caryophyllene (1.71%), and others. (C) 2016 Academie des sciences. Published by Elsevier Masson SAS. All rights reserved.
Ahmed Zermane, Ouassila Larkeche, Abdeslam-Hassen Meniai, Christelle Crampon, Elisabeth Badens. Optimization of Algerian rosemary essential oil extraction yield by supercritical CO2 using response surface methodology. Comptes Rendus. Chimie, 2016, 19 (4), pp.538-543. ⟨10.1016/j.crci.2015.08.011⟩. ⟨hal-01461780⟩
Abir Bouledjouidja, Yasmine Masmoudi, Michiel van Speybroeck, Laurent Schueller, Elisabeth Badens. Impregnation of Fenofibrate on mesoporous silica using supercritical carbon dioxide. International Journal of Pharmaceutics, 2016, 499, pp.1 - 9. ⟨hal-01266561⟩ Plus de détails...
Low oral bioavailability can be circumvented by the formulation of the poorly water soluble drug in ordered mesoporous silica (OMS-L-7). Fenofibrate is an orally administered, poorly water-soluble active pharmaceutical ingredient (API), used clinically to lower lipid levels. Fenofibrate was loaded into silica using two methods: incipient wetness and supercritical impregnation. This study investigates the impact of loading and the impact of varying supercritical carbon dioxide (scCO2) processing conditions. The objective is to enhance Fenofibrate loading into silica while reducing degree of the drug crystallinity, so as to increase the drug's dissolution rate and its bioavailability. The comparison of both impregnation processes was made in terms of impregnation yields and duration as well as physical characterization of the drug. While incipient wetness method led to a Fenofibrate loading up to 300 mgdrug/gsilica in 48 h of impregnation, the supercritical impregnation method yielded loading up to 485 mgdrug/gsilica in 120 min of impregnation duration, at 16 MPa and 308 K, with a low degree of crystallinity (about 1%) comparable to the crystallinity observed via the solvent method. In addition to the enhancement of impregnation efficiency, the supercritical route provides a solvent-free alternative for impregnation.
Abir Bouledjouidja, Yasmine Masmoudi, Michiel van Speybroeck, Laurent Schueller, Elisabeth Badens. Impregnation of Fenofibrate on mesoporous silica using supercritical carbon dioxide. International Journal of Pharmaceutics, 2016, 499, pp.1 - 9. ⟨hal-01266561⟩
Abir Bouledjouidja, Yasmine Masmoudi, Michelle Sergent, Vivek Trivedi, Abdeslam-Hassen Meniai, et al.. Drug loading of foldable commercial intraocular lenses using supercritical impregnation
. International Journal of Pharmaceutics, 2016, 500 (1-2), pp.85 - 99. ⟨10.1016/j.ijpharm.2016.01.016⟩. ⟨hal-01266557⟩ Plus de détails...
The drug delivery through intraocular lenses (IOLs) allows the combination of cataract surgery act and postoperative treatment in a single procedure. In order to prepare such systems, “clean” supercritical CO2 processes are studied for loading commercial IOLs with ophthalmic drugs. Ciprofloxacin (CIP, an antibiotic) and dexamethasone 21-phosphate disodium (DXP, an anti-inflammatory drug) were impregnated into foldable IOLs made from poly-2-hydroxyethyl methacrylate (P-HEMA). A first pre-treatment step was conducted in order to remove absorbed conditioning physiological solution. Supercritical impregnations were then performed by varying the experimental conditions. In order to obtain transparent IOLs and avoid the appearance of undesirable foaming, it was necessary to couple slow pressurization and depressurization phases during supercritical treatments. The impregnation yields were determined through drug release studies. For both drugs, release studies showdeep and reproducible impregnation for different diopters. For the system P-HEMA/CIP, a series of impregnations was performed to delimit the experimental range at two pressures (80 and 200 bar) in the presence or absence of ethanol as a co-solvent for two diopters (+5.0 D and +21.0 D). Increase in pressure in the absence of a co-solvent resulted in improved CIP impregnation. The addition of ethanol (5 mol%) produced impregnation yields comparable to those obtained at 200 bar without co-solvent. A response surface methodology based on experimental designs was used to study the influence of operating conditions on impregnation of IOLs (+21.0 D) in the absence of co-solvent. Two input variables with 5 levels each were considered; the pressure (80–200 bar) and the impregnation duration (30–240 min). CIP impregnation yields ranging between 0.92 and 3.83 μgCIP/mgIOL were obtained from these experiments and response surface indicated the pressure as a key factor in the process. The DXP impregnation in P-HEMA was higher than CIP at all the tested conditions (8.50–14.53 μgDXP/mgIOL). Furthermore, unlike CIP, highest DXP impregnation yields were obtained in the presence of ethanol as a co-solvent (5 mol%). NMR spectroscopy was performed to confirm complete removal of ethanol in the co-solvent-treated IOLs
Abir Bouledjouidja, Yasmine Masmoudi, Michelle Sergent, Vivek Trivedi, Abdeslam-Hassen Meniai, et al.. Drug loading of foldable commercial intraocular lenses using supercritical impregnation
. International Journal of Pharmaceutics, 2016, 500 (1-2), pp.85 - 99. ⟨10.1016/j.ijpharm.2016.01.016⟩. ⟨hal-01266557⟩
Carlos Ariel Pieck, Christelle Crampon, Frédéric Charton, Elisabeth Badens. Multi-scale experimental study and modeling of the supercritical fractionation process. Journal of Supercritical Fluids, 2015, 105, pp.158-169. ⟨10.1016/j.supflu.2015.01.021⟩. ⟨hal-01297564⟩ Plus de détails...
In this work, the fractionation of water–ethanol mixtures by supercritical carbon dioxide at 333 K and 10.1 MPa was used as a model system to compare experimental extract and raffinate compositions and overhead loadings at laboratory, pilot and industrial scales to contribute toward a sizing methodology for counter-current supercritical fractionation columns. A series of three columns with an internal diameter of 19, 58 and 126 mm and with a height of 2, 4 and 8 m respectively were used for the different scales, meaning scaling factors from 9 to 44 between columns. The massic solvent-to-feed ratio was varied between 5.2 and 78.8. Experimental results at the different scales are analyzed and compared from the thermodynamic, mass transfer and column hydrodynamics points of view; and also using process simulation by equilibrium-stage models. In total, 42 successful experimental runs are taken into account, including 6 at a pilot scale unit and 2 at an industrial scale.
Carlos Ariel Pieck, Christelle Crampon, Frédéric Charton, Elisabeth Badens. Multi-scale experimental study and modeling of the supercritical fractionation process. Journal of Supercritical Fluids, 2015, 105, pp.158-169. ⟨10.1016/j.supflu.2015.01.021⟩. ⟨hal-01297564⟩
Elisabeth Badens, Jacques Fages. Special Issue : 14th European Meeting on Supercritical Fluids - Préface. Journal of Supercritical Fluids, 2015, 105 (SI), p. XI-XII. ⟨10.1016/S0896-8446(15)00220-X⟩. ⟨hal-01618289⟩ Plus de détails...
Elisabeth Badens, Jacques Fages. Special Issue : 14th European Meeting on Supercritical Fluids - Préface. Journal of Supercritical Fluids, 2015, 105 (SI), p. XI-XII. ⟨10.1016/S0896-8446(15)00220-X⟩. ⟨hal-01618289⟩
Béatrice Perrier, Christelle Crampon, Olivier Guézet, Coralie Simon, François Maire, et al.. Production of a methyl ester from the microalgae Nannochloropsis grown in raceways on the French west coast. Fuel, 2015, 153, pp.640-649. ⟨10.1016/j.fuel.2015.03.011⟩. ⟨hal-01247077⟩ Plus de détails...
The present article describes the production of oil from autotrophic microalgae grown in raceways in France, and presents the bench test results of a Diesel monocylinder engine with the derived biodiesel (methyl ester).The cultivation of Nannochloropsis has been performed under nitrogen limitation in order to increase the lipid content of the microalgae. After harvesting, a drying operation has been carried out so as to obtain a dry microalgae powder with controlled water content. Neutral lipids were then recovered using supercritical carbon dioxide extraction technology applied to the dry powder. One hundred kilograms of dry microalgae has been treated leading to about five kilograms of algal oil, free of polar lipids, that has been transesterified with methanol. The fuel obtained has been blended with a standard biofuel-free Diesel fuel (10% algal fuel/90% standard Diesel fuel B0) and engine tests have been carried out with the resulting blend (B10). In order to compare with well-known fuels similar engine tests were performed with B0 and with a B10 fuel made of ten percent vegetable oil methyl ester complying with the European 14214 fuel standard (B10 EU-type). The B10 quality was rather close to Diesel fuel except for oxidation stability, which was well below the minimum limit for Diesel fuel. The behavior of the B10 fuel appears to be very similar in terms of combustion efficiency and pollutant emissions to the one of the standard Diesel fuel B0.
Béatrice Perrier, Christelle Crampon, Olivier Guézet, Coralie Simon, François Maire, et al.. Production of a methyl ester from the microalgae Nannochloropsis grown in raceways on the French west coast. Fuel, 2015, 153, pp.640-649. ⟨10.1016/j.fuel.2015.03.011⟩. ⟨hal-01247077⟩
L.M. Santiago, Y. Masmoudi, A. Tarancón, R. Djerafi, H. Bagán, et al.. Polystyrene based sub-micron scintillating particles produced by supercritical anti-solvent precipitation. Journal of Supercritical Fluids, 2015, 103, pp.18-27. ⟨10.1016/j.supflu.2015.04.015⟩. ⟨hal-01297575⟩ Plus de détails...
scintillation microspheres (PSm) are a novel material employed in the measurement of radioactivity (α and β emitters). This work is focused on the formation of plastic scintillation particles through the precipitation and encapsulation of two fluorescent solutes (2,5-diphenyloxazol (PPO) and 1,4-Bis(5-phenyloxazol-2-yl) benzene (POPOP)) and an aromatic solvent 2,6-diisopropyl-naphthalene (DIN), which acts as an enhancer for α and β emitters discrimination, into a polymeric matrix of Polystyrene (PS) by Supercritical Anti-Solvent process (SAS) using ethyl acetate (EtAc) for dissolving the PS and supercritical CO2 as antisolvent. Different process parameters were varied; solute concentration in the organic solution (W, wt%), injection velocity of the organic solution (u, ms−1), molar ratio of the organic solvent regarding to CO2 (XEA) and injection capillary tube diameter (μm). In the different experimental conditions tested, SAS coprecipitation was successfully achieved resulting in yields higher than 90% and very low quantities of residual solvent (600–1200 ppm). The different Polystyrene based particles obtained were nearly spherical sub-micron particles (ranged between 150 and 400 nm) and also agglomerates of a few micrometers were observed in most of the studied conditions. Radiometric capacities of particles were evaluated through measuring different beta and alpha emitting radionuclide. The coprecipitates showed scintillation behavior when fluorescent solutes were added, therefore confirming their encapsulation.
L.M. Santiago, Y. Masmoudi, A. Tarancón, R. Djerafi, H. Bagán, et al.. Polystyrene based sub-micron scintillating particles produced by supercritical anti-solvent precipitation. Journal of Supercritical Fluids, 2015, 103, pp.18-27. ⟨10.1016/j.supflu.2015.04.015⟩. ⟨hal-01297575⟩
O. Larkeche, A. Zermane, A.-H. Meniai, C. Crampon, E. Badens. Supercritical extraction of essential oil from Juniperus communis L. needles: Application of response surface methodology. Journal of Supercritical Fluids, 2015, 99, pp.8-14. ⟨10.1016/j.supflu.2015.01.026⟩. ⟨hal-01297558⟩ Plus de détails...
The extraction of oil from Juniperus communis needles was investigated using supercritical CO2. The extraction was carried out varying the pressure in the range of 10–30 MPa, the temperature within 308–328 K, with a solvent flow rate fixed at 0.42 kg h−1, and a mean particle diameter equal to 0.5 mm or less than 0.315 mm. The operating parameters have been optimized using the response surface methodology where a second order polynomial expression was used to express the oil recovery, and the results were satisfactory. The maximum oil recovery relative to the initial mass was 6.55 wt%. It was obtained for an extraction under 328 K, 30 MPa and a particle diameter less than 0.315 mm. Selected samples of extracts were analyzed using gas chromatography–mass spectrometry (GC/MS) and the results show that the most concentrated compounds were germacrene D and 1-octadecene.
O. Larkeche, A. Zermane, A.-H. Meniai, C. Crampon, E. Badens. Supercritical extraction of essential oil from Juniperus communis L. needles: Application of response surface methodology. Journal of Supercritical Fluids, 2015, 99, pp.8-14. ⟨10.1016/j.supflu.2015.01.026⟩. ⟨hal-01297558⟩
Maria Teresa Fernández-Ponce, Yasmine Masmoudi, Rania Djerafi, Lourdes Casas, Casimiro Mantell, et al.. Particle design applied to quercetin using supercritical anti-solvent techniques. Journal of Supercritical Fluids, 2015, 105, pp.119 - 127. ⟨hal-01266553⟩ Plus de détails...
Quercetin is a strong naturally occurring antioxidant that is exploited in pharmaceutical and cosmeticsapplications. Unfortunately, quercetin is highly susceptible to oxidation. Besides, its poor solubility inwater and low bioavailability upon oral administration limit the use in drug formulations for the treat-ment of human diseases. In an effort to overcome these drawbacks, the micronization and coprecipitationof quercetin particles with a low-cost biocompatible polymer (ethyl cellulose, EC) was studied by usingsupercritical anti-solvent process (SAS) with a non-toxic solvent ethyl acetate. The results showed thatSAS micronization of quercetin led to a reduction in the quercetin particle size and crystallinity withouta change in the needle-like habit. SAS coprecipitation of quercetin with EC at moderate pressure andtemperature (10 MPa and 35◦C) led to obtaining quasi-spherical particles. The coated polymer avoidthe growth of quercetin crystals, thus amorphous particles in the submicron range (mean size rangingbetween 150 and 350 nm) were formed. Promising coprecipitation results were reached with quite highprocess yields (above 85%) and encapsulation efficiencies up to 99% that provided a high stability to thecoated quercetin with EC against oxidation.
Maria Teresa Fernández-Ponce, Yasmine Masmoudi, Rania Djerafi, Lourdes Casas, Casimiro Mantell, et al.. Particle design applied to quercetin using supercritical anti-solvent techniques. Journal of Supercritical Fluids, 2015, 105, pp.119 - 127. ⟨hal-01266553⟩
Supercritical anti-solvent (SAS) process is considered to be a clean technology suitable for particle design. It is generally used in order to micronize compounds of interest under mild operating conditions of temperature and with very low residual solvent traces in the end-product. By varying the process parameters, the properties of the produced powders can be adjusted with defined size (generally micron or nanometer sized particles), morphology and a narrow particle size distribution. There is currently a growing interest for the elaboration of controlled delivery systems. For this purpose, the SAS process can also be applied in order to co-precipitate molecules of interest with biocompatible and/or biodegradable polymers. An experimental study dealing with supercritical anti-solvent (SAS) precipitation has been carried out in order to micronize a biocompatible polymer, ethyl cellulose, widely used as a drug carrier in controlled delivery systems for oral administration. Supercritical carbon dioxide was used as anti-solvent for the polymer and ethyl acetate (EtAc), generally recognized as safe (GRAS) by the FDA (Food and Drug Administration) as solvent. The influence of the variation of the main operating parameters upon the characteristics of the micronized polymer was evaluated. In particular, the temperature (308, 318 and 333 K), the polymer concentration (1, 3 and 4 wt%), the EtAc/CO2 molar ratio (5 and 8 mol%) and the capillary tube diameter (127 and 254 μm) while pressure was kept constant and equal to 10 MPa. Using a low organic solution concentration of 1 wt% and at a temperature of 308 K, ethyl cellulose was successfully micronized in submicron particles with a mean size of 300 nm. However, increasing the temperature or the polymer concentration in the organic solution favored the particle coalescence and even led to fiber formation.
Rania Djerafi, Yasmine Masmoudi, Christelle Crampon, Abdeslam-Hassen Meniai, Elisabeth Badens. Supercritical anti-solvent precipitation of ethyl cellulose. Journal of Supercritical Fluids, 2015, 105, pp.92-98. ⟨hal-01266175⟩
A. Zermane, O. Larkeche, Abdeslam-Hassen Meniai, Christelle Crampon, Elisabeth Badens. Optimization of essential oil supercritical extraction from Algerian Myrtus communis L. leaves using response surface methodology. Journal of Supercritical Fluids, 2014, 85, pp.89-94. ⟨10.1016/j.supflu.2013.11.002⟩. ⟨hal-01053268⟩ Plus de détails...
The present work deals with the application of the supercritical fluid extraction process to extract essential oils from the leaves of an Algerian myrtle plant (Myrtus communis L.). Using the surface response methodology, an optimization of the extraction recovery was carried out, varying the pressure in the range of [10-30 MPa], the temperature within [308-323 K], a solvent flow rate fixed at 0.42 kg h(-1) and a mean particle diameter equal to 0.5 mm or less than 0.315 mm. The maximum value of essential oil recovery relative to the initial mass of leaf powder was 4.89 wt%, and was obtained when the SC-CO2 extraction was carried out under 313 K, 30 MPa and with a particle diameter less than 0.315 mm. A second-order polynomial expression was used to express the oil recovery. The calculated mass of recovered oil using the response surface methodology was very close to the experimental value, confirming the reliability of this technique.
A. Zermane, O. Larkeche, Abdeslam-Hassen Meniai, Christelle Crampon, Elisabeth Badens. Optimization of essential oil supercritical extraction from Algerian Myrtus communis L. leaves using response surface methodology. Journal of Supercritical Fluids, 2014, 85, pp.89-94. ⟨10.1016/j.supflu.2013.11.002⟩. ⟨hal-01053268⟩
Christelle Crampon, Adil Mouahid, Sid-Ali Amine Toudji, Olivier Lépine, Elisabeth Badens. Influence of pretreatment on supercritical CO2 extraction from Nannochloropsis oculata. Journal of Supercritical Fluids, 2013, 79, pp.337-344. ⟨10.1016/j.supflu.2012.12.022⟩. ⟨hal-00993082⟩ Plus de détails...
This work demonstrates that supercritical carbon dioxide extraction is efficient for the complete recovery of neutral lipids from microalgae with a water content up to 20 wt%, allowing thus a further full characterization of this oil. This is a first useful step in the framework of lipid production from microalgae either for nutraceutical, food or for energy applications. This study is particularly focused on the influence of the pretreatments upon extraction kinetics and yields. This study proposes a complete study at laboratory scale (10 g per batch of dry biomass) of the influence of pretreatments (type of drying and grinding) and of water content on the extraction kinetics and yields as well as on the oil composition in terms of lipidic classes and profiles. Two drying pretreatments (drying under air flow and freeze-drying) applied on Nannochloropsis oculata were studied. Extraction experiments were carried out at 40 MPa, 333 K, with a carbon dioxide flow rate of 0.5 kg h−1 and for different granulometries. Results showed that drying under air flow at 308 K is the most adequate pretreatment leading to the most rapid kinetics. Whatever the pretreatment used, the extracted oil contains more than 90 wt% of triglycerides and does not contain phospholipids. As expected, the smaller the particle size, the faster the extraction kinetics. Finally, an increase in the biomass water content up to 20 wt% increases the global extraction kinetics (extraction of both water and oil) but appears to have no influence on oil extraction yields. Moreover, the extraction of neutral lipids happens to be complete for a CO2/charge mass ratio ranging from 30 to 130 depending on the operating conditions and on the characteristics of the treated biomass. Finally, pilot scale experiments were performed with batches up to 15 kg in order to evaluate the influence of pressure and particle size on the extraction kinetics and yields. Extracts obtained at 333 K with operating pressures of 50 MPa and 85 MPa have similar compositions and do not contain phospholipids.
Christelle Crampon, Adil Mouahid, Sid-Ali Amine Toudji, Olivier Lépine, Elisabeth Badens. Influence of pretreatment on supercritical CO2 extraction from Nannochloropsis oculata. Journal of Supercritical Fluids, 2013, 79, pp.337-344. ⟨10.1016/j.supflu.2012.12.022⟩. ⟨hal-00993082⟩
Adil Mouahid, Christelle Crampon, Sid-Ali Amine Toudji, Elisabeth Badens. Supercritical CO2 extraction of neutral lipids from microalgae: experiments and modelling. Journal of Supercritical Fluids, 2013, 77, pp.7-16. ⟨10.1016/j.supflu.2013.01.024⟩. ⟨hal-00993077⟩ Plus de détails...
The aim of this work is to show that the equations developed by Sovová, based on the concept of broken and intact cells for describing the supercritical extraction curves from plants and vegetables, can be applied for the modelling of the supercritical CO2 extraction curves obtained with microalgae. Experimental and modelling results of supercritical carbon dioxide extraction of lipids from four different microalgae: Nannochloropsis oculata, Cylindrotheca closterium, Chlorella vulgaris and Spirulina platensis, are presented. The experimental setup is a laboratory scale apparatus which allows an accurate monitoring of the mass loss of the microalgae sample during the extraction. The experimental data were obtained at a pressure of 40 MPa, a temperature of 333 K and CO2 flow rates from 0.3 to 0.5 kg/h. The extraction experiments were performed on samples having undergone different pretreatments: (i) after harvesting and centrifugation, microalgae were dried either by freeze-drying or air flow drying) and (ii) they were ground and sieved at different particle sizes (particle diameters ranging from 160 to 1000 μm). The complete extraction of neutral lipids was performed leading to mass losses up to 30% depending on the samples and on the operating conditions. Extracts were mainly composed of triglycerides (more than 90 wt% of extracts). The mathematical model published in 2005 and the simplified equations of extraction curves (using the characteristic times characterizing each extraction step) published in 2012 by Sovová were chosen to fit the experimental data. Among the hypotheses proposed by Sovovà, we considered that the flow pattern of supercritical CO2 in the extraction autoclave was plug flow and the extraction process was supposed to occur with negligible solute-matrix interactions. The adjustable parameters were calculated by minimizing the sum of least squares between experimental and calculated values of the extraction yield. Good agreement between the two models and our experimental measurements was obtained. The average absolute relative deviation ranges between 0.5 and 10.2%.
Adil Mouahid, Christelle Crampon, Sid-Ali Amine Toudji, Elisabeth Badens. Supercritical CO2 extraction of neutral lipids from microalgae: experiments and modelling. Journal of Supercritical Fluids, 2013, 77, pp.7-16. ⟨10.1016/j.supflu.2013.01.024⟩. ⟨hal-00993077⟩
Elisabeth Badens. Mise en forme de principes actifs pharmaceutiques en phase supercritique. Les Techniques de l'Ingenieur, 2012. ⟨hal-01300400⟩ Plus de détails...
Les procédés de mise en forme de principes actifs pharmaceutiques en phase supercritique permettent d'élaborer des produits ayant des caractéristiques contrôlées et homogènes. Le recours aux solvants organiques est limité voire totalement évité dans de nombreux cas. Des composés de différentes natures (principes actifs courants, biomolécules, polymères) peuvent être traités. Plusieurs de ces procédés arrivent à maturité et leur développement dans l'industrie est maintenant amorcé.
Elisabeth Badens. Mise en forme de principes actifs pharmaceutiques en phase supercritique. Les Techniques de l'Ingenieur, 2012. ⟨hal-01300400⟩
Stéphanie Careno, Olivier Boutin, Elisabeth Badens. Drug recrystallisation using supercritical anti-solvent (SAS) process with impinging jets: effects of process parameters. Journal of Crystal Growth, 2012, 342 (1), pp.34-41. ⟨10.1016/j.jcrysgro.2011.06.059⟩. ⟨hal-00993004⟩ Plus de détails...
The aim of this study is to improve mixing in supercritical anti-solvent process (SAS) with impinging jets in order to form finer particles of sulfathiazole, a poorly water-soluble drug. The influence of several process parameters upon the powder characteristics is studied. Parameters are jets' velocity (0.25 m/s to 25.92 m/s), molar ratio solvent/CO2 (2.5% to 20%), temperature (313 K to 343 K), pressure (10 MPa to 20 MPa) and sulfathiazole concentration in the organic solution (0.5% to 1.8%). Two solvents are used: acetone and methanol. Smaller particles with a more homogeneous morphology are obtained from acetone solutions. For the smallest jets' velocity, corresponding to a non-atomized jet, the stable polymorphic form is obtained, pure or in mixture. At this velocity, pressure is the most influential parameter controlling the polymorphic nature of the powder formed. The pure stable polymorph is formed at 20 MPa. Concerning the particle size, the most influential parameters are temperature and sulfathiazole concentration. The use of impinging jets with different process parameters allows the crystallization of four polymorphs among the five known, and particle sizes are varied. This work demonstrates the studied device ability of the polymorph and the size control. A comparison with the classical SAS process shows that particle size, size distribution and morphology of particles crystallized with impinging jets are different from the ones obtained with classical SAS introduction device in similar operating conditions. Mean particle sizes are significantly smaller and size distributions are narrower with impinging jets device.
Stéphanie Careno, Olivier Boutin, Elisabeth Badens. Drug recrystallisation using supercritical anti-solvent (SAS) process with impinging jets: effects of process parameters. Journal of Crystal Growth, 2012, 342 (1), pp.34-41. ⟨10.1016/j.jcrysgro.2011.06.059⟩. ⟨hal-00993004⟩
Yasmine Masmoudi, Louiza Ben Azzouk, Olivier Forzano, Jean-Marie Andre, Elisabeth Badens. Supercritical impregnation of intraocular lenses. Journal of Supercritical Fluids, 2011, Selected Papers from the 9th Conference on Supercritical Fluids and their Applications, September 05-08, 2010, Sorrento (Italy), 60, pp.98 - 105. ⟨hal-01266171⟩ Plus de détails...
Supercritical impregnation can be used for the elaboration of controlled release systems that may be applied to pharmaceutical and medicinal fields. The present work is dedicated to the impregnation of intraocular lenses (IOLs) with antibiotics using supercritical carbon dioxide as impregnation vector. Commercially available intraocular lenses have been impregnated with cefuroxime sodium in order to obtain ophthalmic drug delivery systems dedicated to the prevention of postoperative endophthalmitis in cataract surgery. The influence of the variation of some experimental operating conditions such as the pressure (8–20 MPa), the temperature (308 and 333 K), the impregnation duration (1–5 h), the addition of a cosolvent (ethanol) or the depressurisation rate (slow and rapid depressurisation) has been studied. In certain experimental conditions, foaming phenomena have been observed. In order to evaluate the impregnation efficiency, the impregnation yields were quantified gravimetrically and the drug release profiles were determined through in vitro drug release studies carried out at 310 K and in a solution simulating the aqueous humor. At rapid depressurisation rates, controlled drug release IOLs with impregnation yields varying between 0.002 and 0.063 mgdrug/mgIOL were obtained. Increasing the pressure or adding a cosolvent were favourable to enhance the impregnation yields. However, a non desired foaming phenomenon was observed for the most favourable conditions. By carrying out slow depressurisations, foaming phenomena were avoided. Nevertheless, in these conditions, the impregnation process was less efficient. The drug partition seems to be more favourable towards the supercritical phase than towards the polymer and the impregnation phenomena governed by a deposition mechanism rather than a molecular dispersion of the active ingredient. The drug is almost deposited within the porosity created during the rapid depressurisation phase. This result was confirmed by the results of the drug release studies.
Yasmine Masmoudi, Louiza Ben Azzouk, Olivier Forzano, Jean-Marie Andre, Elisabeth Badens. Supercritical impregnation of intraocular lenses. Journal of Supercritical Fluids, 2011, Selected Papers from the 9th Conference on Supercritical Fluids and their Applications, September 05-08, 2010, Sorrento (Italy), 60, pp.98 - 105. ⟨hal-01266171⟩
Laurène Lesoin, Olivier Boutin, Christelle Crampon, Elisabeth Badens. CO2/water/surfactant ternary systems and liposome formation using supercritical CO2: a review. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 2011, 377 (1-3), pp.1-14. ⟨10.1016/j.colsurfa.2011.01.027⟩. ⟨hal-01044546⟩ Plus de détails...
The aim of this review is to explain the various phenomena involved in liposome formation using dense gas processes and especially supercritical CO2. Before liposome formation, the review focuses on the phase behavior of CO2/water/surfactant ternary systems. First of all, the two main cases of CO2/water/surfactant fluid phase behavior are studied: reverse micelle systems and Winsor systems. Then, the various mechanisms of emulsion destabilization as a function of formulation variables (pressure, temperature and water content) are tackled. Influence of formulation variables is also addressed in the case of liposome formation during depressurization and CO2 release for dense gas techniques. Techniques using supercritical or subcritical conditions are classified according to the hydration way: in the first case, hydration is carried out under pressure and in the second one, hydration is achieved after depressurization. Hydration under pressure involves the formation of a CO2/water/surfactant system which is not the case when hydration is carried out during depressurization. An emergent tendency in liposome formation may be noted: (i) large unilamellar vesicles would appear when hydration is achieved under pressure, i.e. when liposomes are the result of two phase inversions (inversion phase from water-in-CO2 emulsion to CO2-in-water emulsion and inversion phase from CO2-in-water emulsion to liposomes); (ii) multilamellar vesicles would be formed when hydration is realized during depressurization, i.e. when liposomes are the result of one phase inversion (inversion phase from CO2-in-water to liposomes). Lastly, a model of liposome formation is developed.
Laurène Lesoin, Olivier Boutin, Christelle Crampon, Elisabeth Badens. CO2/water/surfactant ternary systems and liposome formation using supercritical CO2: a review. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 2011, 377 (1-3), pp.1-14. ⟨10.1016/j.colsurfa.2011.01.027⟩. ⟨hal-01044546⟩
Journal: Colloids and Surfaces A: Physicochemical and Engineering Aspects
Laurène Lesoin, Christelle Crampon, Olivier Boutin, Elisabeth Badens. Development of a continuous dense gas process for the production of liposomes. Journal of Supercritical Fluids, 2011, 60, pp.51-62. ⟨10.1016/j.supflu.2011.04.018⟩. ⟨hal-01044574⟩ Plus de détails...
A new process called Continuous Anti-Solvent (CAS) process was developed for the production of liposomes using supercritical CO2. Unlike the current dense gas technologies, CAS method is a single step and continuous process. Preliminary experiments were conducted in semi-batch mode to determine the most suitable operating conditions (stirring speed = 225 rpm; water/lecithin mass ratio = 21) to ensure an efficient phase mixing in the autoclave. Then, two procedures were developed for the CAS process in the continuous mode. According to the results, the single exit procedure enhances the phase mixing in the autoclave with the formation of a CO2-in-water emulsion which is a good precursor to liposome formation. Liposomes prepared with the CAS method (P = 9 MPa; T = 308 K; CO2 flow rate = 0.3 kg h−1; organic solution flow rate = 240 mL h−1; water flow rate = 180 mL h−1) are spherical and multilamellar with a medium diameter included between 10 and 100 μm.
Laurène Lesoin, Christelle Crampon, Olivier Boutin, Elisabeth Badens. Development of a continuous dense gas process for the production of liposomes. Journal of Supercritical Fluids, 2011, 60, pp.51-62. ⟨10.1016/j.supflu.2011.04.018⟩. ⟨hal-01044574⟩
Laurène Lesoin, Christelle Crampon, Olivier Boutin, Elisabeth Badens. Preparation of liposomes using the supercritical anti-solvent (SAS) process and comparison with a conventional method. Journal of Supercritical Fluids, 2011, 57 (2), pp.162-174. ⟨10.1016/j.supflu.2011.01.006⟩. ⟨hal-01044553⟩ Plus de détails...
Two methods to produce liposomes encapsulating a fluorescent marker were compared: the supercritical anti-solvent (SAS) method and a conventional one (Bangham). Liposome size and encapsulation efficiency were measured to assess the methods. Micronized lecithin produced by the SAS process was characterized in terms of particle size, morphology and residual solvent content in order to investigate the influence of experimental parameters (pressure, CO2/solvent molar ratio and solute concentration). It appears that when the lecithin concentration increases from 15 to 25 wt.%, at 9 MPa and 308 K, larger (20-60 μm) and less aggregated lecithin particles are formed. As concerns liposomes formed from SAS processed lecithin, size distribution curves are mainly bimodal, spreading in the range of 0.1-100 μm. Liposome encapsulation efficiencies are including between 10 and 20%. As concerns the Bangham method, more dispersed liposomes were formed; encapsulation efficiencies were about 20%, and problems of reproducibility have been raised.
Laurène Lesoin, Christelle Crampon, Olivier Boutin, Elisabeth Badens. Preparation of liposomes using the supercritical anti-solvent (SAS) process and comparison with a conventional method. Journal of Supercritical Fluids, 2011, 57 (2), pp.162-174. ⟨10.1016/j.supflu.2011.01.006⟩. ⟨hal-01044553⟩
Olivier Boutin, Axel de Nadai, Antonio Garcia Perez, Jean-Henry Ferrasse, Marina Beltran, et al.. Experimental and modelling of supercritical oil extraction from rapeseeds and sunflower seeds. Chemical Engineering Research and Design, 2011, 89 (11), pp.2477-2484. ⟨10.1016/j.cherd.2011.02.032⟩. ⟨hal-01044569⟩ Plus de détails...
The supercritical oil extraction from oleaginous seeds (sunflower and rapeseeds) is presented here through experimental and modelling results. The experimental setup allows an accurate following of the mass of the oil extracted and to derive the experimental influences of pressure, temperature and supercritical CO2 flowrate on the extraction curves. These parameters are very sensitive and highlight the necessity of precise optimisation of experimental conditions. In order to complete the behaviour of supercritical fluids extraction, an improved modelling is proposed. The modelling basic equations are based on others modelling published previously. In this work, the determination of several parameters comes from correlations and the other constants are fitted with all the experimental results. Thus the modelling is more representative and predictive as other ones. The modelling results present a good agreement with the experimental results, and hence it can be used for the dimensioning of some extraction autoclaves.
Olivier Boutin, Axel de Nadai, Antonio Garcia Perez, Jean-Henry Ferrasse, Marina Beltran, et al.. Experimental and modelling of supercritical oil extraction from rapeseeds and sunflower seeds. Chemical Engineering Research and Design, 2011, 89 (11), pp.2477-2484. ⟨10.1016/j.cherd.2011.02.032⟩. ⟨hal-01044569⟩
Christelle Crampon, Olivier Boutin, Elisabeth Badens. Supercritical carbon dioxide extraction of molecules of interest from microalgae and seaweeds. Industrial and engineering chemistry research, 2011, 50 (15), pp.8941-8953. ⟨10.1021/ie102297d⟩. ⟨hal-01044580⟩ Plus de détails...
The purpose of this paper is to guide lectors in the extraction of algal (microalgae and seaweeds) compounds using supercritical carbon dioxide (SC-CO2) from dry biomass. It proposes a review of 30 articles dealing with the SC-CO2 extraction of molecules of interest from microalgae and seaweeds. Among these papers, 20 are devoted to microalgae. The most extracted compounds are neutral lipids and antioxidants. Several operating conditions have been tested: pressures from 7.8 to 70 MPa, temperatures from 313.15 to 349.15 K, and CO2/algae mass ratio from 6 to 500. All extraction studies were performed at laboratory scale, with the masses of dry algae powder never exceeding 180 g. Extraction yields vary significantly with operating conditions: pressure seems to be the most influential parameter. The higher the pressure, the higher the yields and/or the faster the extraction kinetics. Temperature also has an influence, but its effect is dependent on pressure (retrograde behavior). Moreover, as expected, it is advised to work with a high CO2/algae mass ratio. From these works, it appears that, to perform an efficient extraction with SC-CO2, the influence of the algae pretreatment is highly significant. The first step is a centrifugation. The resulting concentrated algal suspension must then undergo a drying operation, which is generally freeze-drying or low-temperature drying. Finally, the algae are crushed. Concerning the influence of crushing, the reported results show that, as expected, the smaller the particles, the more rapid the extraction kinetics and/or the higher the yields.
Christelle Crampon, Olivier Boutin, Elisabeth Badens. Supercritical carbon dioxide extraction of molecules of interest from microalgae and seaweeds. Industrial and engineering chemistry research, 2011, 50 (15), pp.8941-8953. ⟨10.1021/ie102297d⟩. ⟨hal-01044580⟩
Journal: Industrial and engineering chemistry research
Elisabeth Badens, Stéphane A Veesler, Roland Boistelle, Dominique Chatain. Relation between Young’s Modulus of set plaster and complete wetting of grain boundaries by water. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 1999, 156 (1-3), pp.373 - 379. ⟨10.1016/S0927-7757(99)00097-7⟩. ⟨hal-01745672⟩ Plus de détails...
Elisabeth Badens, Stéphane A Veesler, Roland Boistelle, Dominique Chatain. Relation between Young’s Modulus of set plaster and complete wetting of grain boundaries by water. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 1999, 156 (1-3), pp.373 - 379. ⟨10.1016/S0927-7757(99)00097-7⟩. ⟨hal-01745672⟩
Journal: Colloids and Surfaces A: Physicochemical and Engineering Aspects
Elisabeth Badens, Stéphane A Veesler, Roland Boistelle. Crystallization of gypsum from hemihydrate in presence of additives. Journal of Crystal Growth, 1999, 198-199, pp.704 - 709. ⟨10.1016/S0022-0248(98)01206-8⟩. ⟨hal-01745659⟩ Plus de détails...
Elisabeth Badens, Stéphane A Veesler, Roland Boistelle. Crystallization of gypsum from hemihydrate in presence of additives. Journal of Crystal Growth, 1999, 198-199, pp.704 - 709. ⟨10.1016/S0022-0248(98)01206-8⟩. ⟨hal-01745659⟩
E. Badens, P. Llewellyn, J.M. Fulconis, C. Jourdan, S. Veesler, et al.. Study of Gypsum Dehydration by Controlled Transformation Rate Thermal Analysis (CRTA). Journal of Solid State Chemistry, 1998, 139 (1), pp.37 - 44. ⟨10.1006/jssc.1998.7797⟩. ⟨hal-01745522⟩ Plus de détails...
E. Badens, P. Llewellyn, J.M. Fulconis, C. Jourdan, S. Veesler, et al.. Study of Gypsum Dehydration by Controlled Transformation Rate Thermal Analysis (CRTA). Journal of Solid State Chemistry, 1998, 139 (1), pp.37 - 44. ⟨10.1006/jssc.1998.7797⟩. ⟨hal-01745522⟩
