TY  - JOUR
AU  - Milovanović, Stoja
AU  - Lukić, Ivana
AU  - Stamenić, Marko
AU  - Kamiński, Piotr
AU  - Florkowski, Grzegorz
AU  - Tyśkiewicz, Katarzyna
AU  - Konkol, Marcin
PY  - 2022
UR  - http://TechnoRep.tmf.bg.ac.rs/handle/123456789/5175
AB  - The present study was focused on improving the supercritical fluid extraction process dedicated to the recovery of highly valuable extract from Silybum marianum seeds. At first, the process was tested using supercritical CO2 at temperatures of 40 and 80 °C and pressures ranging from 100 to 300 bar. Obtained values were described using two literature models with acceptable agreement of experimental and calculated data. Further, the effect of the equipment design and process scale-up was investigated in four high-pressure units having volumes in the range from 280 mL to 40 L resulting in extraction yields up to 26 %. Based on the values of the parameters determined at the laboratory scale, the extraction process was successfully transferred to a semi-industrial scale. Finally, estimated costs for supercritical extract production in Poland for the year 2021 using a 1000 L high-pressure unit amounted to the price of 35.9 EUR per kg of extract.
PB  - Elsevier B.V.
T2  - Journal of Supercritical Fluids
T1  - The effect of equipment design and process scale-up on supercritical CO2 extraction: Case study for Silybum marianum seeds
SP  - 105676
VL  - 188
DO  - 10.1016/j.supflu.2022.105676
ER  - 

@article{
author = "Milovanović, Stoja and Lukić, Ivana and Stamenić, Marko and Kamiński, Piotr and Florkowski, Grzegorz and Tyśkiewicz, Katarzyna and Konkol, Marcin",
year = "2022",
abstract = "The present study was focused on improving the supercritical fluid extraction process dedicated to the recovery of highly valuable extract from Silybum marianum seeds. At first, the process was tested using supercritical CO2 at temperatures of 40 and 80 °C and pressures ranging from 100 to 300 bar. Obtained values were described using two literature models with acceptable agreement of experimental and calculated data. Further, the effect of the equipment design and process scale-up was investigated in four high-pressure units having volumes in the range from 280 mL to 40 L resulting in extraction yields up to 26 %. Based on the values of the parameters determined at the laboratory scale, the extraction process was successfully transferred to a semi-industrial scale. Finally, estimated costs for supercritical extract production in Poland for the year 2021 using a 1000 L high-pressure unit amounted to the price of 35.9 EUR per kg of extract.",
publisher = "Elsevier B.V.",
journal = "Journal of Supercritical Fluids",
title = "The effect of equipment design and process scale-up on supercritical CO2 extraction: Case study for Silybum marianum seeds",
pages = "105676",
volume = "188",
doi = "10.1016/j.supflu.2022.105676"
}

Milovanović, S., Lukić, I., Stamenić, M., Kamiński, P., Florkowski, G., Tyśkiewicz, K.,& Konkol, M.. (2022). The effect of equipment design and process scale-up on supercritical CO2 extraction: Case study for Silybum marianum seeds. in Journal of Supercritical Fluids
Elsevier B.V.., 188, 105676.
https://doi.org/10.1016/j.supflu.2022.105676

Milovanović S, Lukić I, Stamenić M, Kamiński P, Florkowski G, Tyśkiewicz K, Konkol M. The effect of equipment design and process scale-up on supercritical CO2 extraction: Case study for Silybum marianum seeds. in Journal of Supercritical Fluids. 2022;188:105676.
doi:10.1016/j.supflu.2022.105676 .

Milovanović, Stoja, Lukić, Ivana, Stamenić, Marko, Kamiński, Piotr, Florkowski, Grzegorz, Tyśkiewicz, Katarzyna, Konkol, Marcin, "The effect of equipment design and process scale-up on supercritical CO2 extraction: Case study for Silybum marianum seeds" in Journal of Supercritical Fluids, 188 (2022):105676,
https://doi.org/10.1016/j.supflu.2022.105676 . .

TY  - CONF
AU  - Milovanović, Stoja
AU  - Kamiński, Piotr
AU  - Dębczak, Agnieszka
AU  - Klimkowska, Kamila
AU  - Florkowski, Grzegorz
AU  - Tyśkiewicz, Katarzyna
AU  - Konkol, Marcin
PY  - 2022
UR  - http://TechnoRep.tmf.bg.ac.rs/handle/123456789/6901
AB  - Milk thistle (Silybum marianum, Asteraceae) is a plant used in traditional medicine from ancient times mostly for treatment of liver disorders [1,2]. Nowadays it is an industrially valuable crop for preparation of herbal supplements reaching total sales of 16 million USD in the USA market [2]. The separation of valuable bioactive compounds from plant materials can be performed by several methods using organic and inorganic solvents. Nevertheless, supercritical fluid extraction (SFE) that employs CO2 is considered a green alternative to other conventional extraction methods. In order to be economically viable, the SFE process should be optimized by selection of appropriate pressure and temperature conditions followed by a scale-up. The scale-up of the SFE process can be performed by keeping constant: the ratio of scCO2 flow rate to mass of bed raw material, the ratio of bed length and bed diameter or dimensionless number such as Reynolds number [3]. This study presents the scale-up of the SFE process, first by selection of optimal pressure (100, 200 and 300 bar) at moderate temperature of 40 °C using a lab scale unit (0.6 L), following by selection of optimal CO2 consumption per used plant material as well as optimal ratio of plant material mass per volume of extractor. Optimal parameters were further tested using a semi-industrial scale unit (40 L). The highest extraction yield obtained was 27%. The performed scale-up study showed a good agreement between lab and pilot scale units. The qualitative analysis performed using GC/MS showed that obtained extracts contained around 80% of unsaturated fatty acids. The quantitative analysis performed using GC/FID confirmed that predominant fatty acids were oleic and linoleic acids with a content in the range of 191-234 mg/g and 445-514 mg/g, respectively (depending on the SFE pressure). Total phenolic compounds were estimated in each extract by the Folin–Ciocalteu assay reaching ca. 90 mg GAE/g. The free radical scavenging capacity was analyzed by the DPPH assay showing value of IC50 (concentration of extract required for the 50% decrease in absorbance of the blank) to be ca. 13 mg/mL.
PB  - Coimbra : Universidade, Faculty of Sciences and Technology
C3  - Book of Abstracts / 2nd Iberian Meeting on Supercritical Fluids (2º Encontro Ibérico de Fluidos Supercríticos) (EIFS2022), Coimbra, Portugal, 28 February - 2 March 2022
T1  - Scale-up of supercritical CO2 extraction process for production of milk thistle extract
EP  - 29
SP  - 28
UR  - https://hdl.handle.net/21.15107/rcub_technorep_6901
ER  - 

@conference{
author = "Milovanović, Stoja and Kamiński, Piotr and Dębczak, Agnieszka and Klimkowska, Kamila and Florkowski, Grzegorz and Tyśkiewicz, Katarzyna and Konkol, Marcin",
year = "2022",
abstract = "Milk thistle (Silybum marianum, Asteraceae) is a plant used in traditional medicine from ancient times mostly for treatment of liver disorders [1,2]. Nowadays it is an industrially valuable crop for preparation of herbal supplements reaching total sales of 16 million USD in the USA market [2]. The separation of valuable bioactive compounds from plant materials can be performed by several methods using organic and inorganic solvents. Nevertheless, supercritical fluid extraction (SFE) that employs CO2 is considered a green alternative to other conventional extraction methods. In order to be economically viable, the SFE process should be optimized by selection of appropriate pressure and temperature conditions followed by a scale-up. The scale-up of the SFE process can be performed by keeping constant: the ratio of scCO2 flow rate to mass of bed raw material, the ratio of bed length and bed diameter or dimensionless number such as Reynolds number [3]. This study presents the scale-up of the SFE process, first by selection of optimal pressure (100, 200 and 300 bar) at moderate temperature of 40 °C using a lab scale unit (0.6 L), following by selection of optimal CO2 consumption per used plant material as well as optimal ratio of plant material mass per volume of extractor. Optimal parameters were further tested using a semi-industrial scale unit (40 L). The highest extraction yield obtained was 27%. The performed scale-up study showed a good agreement between lab and pilot scale units. The qualitative analysis performed using GC/MS showed that obtained extracts contained around 80% of unsaturated fatty acids. The quantitative analysis performed using GC/FID confirmed that predominant fatty acids were oleic and linoleic acids with a content in the range of 191-234 mg/g and 445-514 mg/g, respectively (depending on the SFE pressure). Total phenolic compounds were estimated in each extract by the Folin–Ciocalteu assay reaching ca. 90 mg GAE/g. The free radical scavenging capacity was analyzed by the DPPH assay showing value of IC50 (concentration of extract required for the 50% decrease in absorbance of the blank) to be ca. 13 mg/mL.",
publisher = "Coimbra : Universidade, Faculty of Sciences and Technology",
journal = "Book of Abstracts / 2nd Iberian Meeting on Supercritical Fluids (2º Encontro Ibérico de Fluidos Supercríticos) (EIFS2022), Coimbra, Portugal, 28 February - 2 March 2022",
title = "Scale-up of supercritical CO2 extraction process for production of milk thistle extract",
pages = "29-28",
url = "https://hdl.handle.net/21.15107/rcub_technorep_6901"
}

Milovanović, S., Kamiński, P., Dębczak, A., Klimkowska, K., Florkowski, G., Tyśkiewicz, K.,& Konkol, M.. (2022). Scale-up of supercritical CO2 extraction process for production of milk thistle extract. in Book of Abstracts / 2nd Iberian Meeting on Supercritical Fluids (2º Encontro Ibérico de Fluidos Supercríticos) (EIFS2022), Coimbra, Portugal, 28 February - 2 March 2022
Coimbra : Universidade, Faculty of Sciences and Technology., 28-29.
https://hdl.handle.net/21.15107/rcub_technorep_6901

Milovanović S, Kamiński P, Dębczak A, Klimkowska K, Florkowski G, Tyśkiewicz K, Konkol M. Scale-up of supercritical CO2 extraction process for production of milk thistle extract. in Book of Abstracts / 2nd Iberian Meeting on Supercritical Fluids (2º Encontro Ibérico de Fluidos Supercríticos) (EIFS2022), Coimbra, Portugal, 28 February - 2 March 2022. 2022;:28-29.
https://hdl.handle.net/21.15107/rcub_technorep_6901 .

Milovanović, Stoja, Kamiński, Piotr, Dębczak, Agnieszka, Klimkowska, Kamila, Florkowski, Grzegorz, Tyśkiewicz, Katarzyna, Konkol, Marcin, "Scale-up of supercritical CO2 extraction process for production of milk thistle extract" in Book of Abstracts / 2nd Iberian Meeting on Supercritical Fluids (2º Encontro Ibérico de Fluidos Supercríticos) (EIFS2022), Coimbra, Portugal, 28 February - 2 March 2022 (2022):28-29,
https://hdl.handle.net/21.15107/rcub_technorep_6901 .