Process Optimization of Supercritical CO₂ Extraction for Enhanced Yield of Sarawak Black Pepper (Piper Nigrum L.) Essential Oil
Authors
Institute of Bioproduct Development, Universiti Teknologi Malaysia, 81310, Johor Bahru, Johor;Bioprocess Engineering Department, Faculty of Chemical and Energy Engineering, Universiti Teknologi Malaysia, 81310, Johor Bahru, Johor (Malaysia)
Institute of Bioproduct Development, Universiti Teknologi Malaysia, 81310, Johor Bahru, Johor;Bioprocess Engineering Department, Faculty of Chemical and Energy Engineering, Universiti Teknologi Malaysia, 81310, Johor Bahru, Johor (Malaysia)
Bioprocess Engineering Department, Faculty of Chemical and Energy Engineering, Universiti Teknologi Malaysia, 81310, Johor Bahru, Johor (Malaysia)
Institute of Bioproduct Development, Universiti Teknologi Malaysia, 81310, Johor Bahru, Johor (Malaysia)
Article Information
Publication Timeline
Submitted: 2026-01-20
Accepted: 2026-01-27
Published: 2026-02-06
Abstract
Supercritical fluid extraction (SFE) using carbon dioxide has become a green and efficient alternative to traditional methods for extracting essential oils and bioactive compounds from plant materials. However, extraction performance heavily depends on operating conditions, requiring systematic optimization. In this study, a One Factor At a Time (OFAT) approach was used to optimize the supercritical CO₂ extraction of Sarawak black pepper (Piper nigrum L.) oil, aiming to maximize oil yield and retain key bioactive compounds. The effects of extraction pressure (200-325 bar), temperature (20-70 °C), CO₂ flow rate (2-10 g min⁻¹), extraction time (30-180 min), and ethanol co-solvent concentration (0-25% w/w) were examined individually while keeping other parameters constant. Oil yield was measured gravimetrically, and piperine content was analyzed using high-performance liquid chromatography. Results indicated that all operating parameters significantly affected extraction efficiency. The optimal conditions were found at 300 bar pressure, 50 °C temperature, 6 g min⁻¹ CO₂ flow rate, 90 min extraction time, and 10% (w/w) ethanol as a co-solvent. Under these conditions, a maximum oil yield of 4.07 ± 0.10% was obtained. The optimized extract had a piperine content of 4.88% (w/w) and physicochemical properties consistent with high-quality, unadulterated black pepper oil. Compared to Sarawak-specific SFE studies without co-solvents, adding ethanol significantly improved extraction efficiency. Overall, this study shows that OFAT-based optimization offers valuable parametric insights and provides a practical, scalable strategy for producing high-quality Sarawak black pepper oil using supercritical CO₂.
Keywords
Optimization ,Supercritical , CO₂ ,Extraction ,Yield ,Sarawak Black Pepper
Downloads
References
1. Ajiboye, T.O., Salau, A.K., Afolayan, A.J., 2017. Supercritical fluid extraction of bioactive compounds from plant materials: A review. The Journal of Supercritical Fluids, 120, pp.75–87. [Google Scholar] [Crossref]
2. Arief, Z., Rahman, N.A., Jusoh, S., 2023. Economic and sustainability evaluation of supercritical fluid extraction processes. Chemical Engineering Research and Design, 189, pp.112–124. [Google Scholar] [Crossref]
3. Campone, L., Celano, R., Piccinelli, A.L., Pagano, I., Rastrelli, L., 2018. Extraction of polyphenols from plant matrices by pressurized liquid and supercritical fluid extraction. Journal of Chromatography A, 1569, pp.1–10. [Google Scholar] [Crossref]
4. Collings, G.J., Smith, R.M., Jackson, M.A., 2018. Carbon dioxide as a green solvent for extraction processes. Green Chemistry, 20, pp.537–553. [Google Scholar] [Crossref]
5. Dawid, L., Korekar, G., Pawar, R., 2012. Supercritical fluid extraction: A review of recent advances. Analytical Methods, 4, pp.2071–2081. [Google Scholar] [Crossref]
6. Dosoky, N.S., Setzer, W.N., 2019. Biological activities and safety of essential oils. Molecules, 24(17), 3046. [Google Scholar] [Crossref]
7. Dutta, S., Bhattacharjee, P., 2016. Supercritical carbon dioxide extraction of piperine from Piper nigrum L. and its kinetic modeling. Journal of Food Engineering, 178, pp.1–8. [Google Scholar] [Crossref]
8. Elmaaty, T.A., Farag, M.A., Abdelhameed, R.E., 2023. Kinetics and optimization of essential oil extraction using supercritical CO₂. Food Chemistry, 405, 134823. [Google Scholar] [Crossref]
9. Feyzi, S., Varidi, M., Zare, F., 2016. Application of OFAT methodology for optimization of food extraction processes. Journal of Food Process Engineering, 39(6), pp.629–638. [Google Scholar] [Crossref]
10. Filippova, M., Kadyrov, R., Yashina, N., 2020. Determination of refractive index of essential oils using digital refractometry. Measurement, 152, 107259. [Google Scholar] [Crossref]
11. Gupta, S., Sharma, A., 2019. Physicochemical characterization of spice essential oils and their quality evaluation. Food Research International, 116, pp.138–147. [Google Scholar] [Crossref]
12. Hakim, S.I., Rahman, N.A., Al-Mahasneh, M., 2020. Green solvent applications in supercritical extraction of natural products. Journal of Cleaner Production, 273, 123148. [Google Scholar] [Crossref]
13. Han, X., Kang, Y., 2015. Influence of solvent flow rate on mass transfer behavior in supercritical extraction. The Journal of Supercritical Fluids, 99, pp.1–7. [Google Scholar] [Crossref]
14. He, Y., Zhao, L., Wang, S., 2024. Temperature effects on solute solubility and mass transfer during supercritical CO₂ extraction. Separation and Purification Technology, 337, 123456. [Google Scholar] [Crossref]
15. Herrero, M., Cifuentes, A., & Ibáñez, E. (2013). Sub- and supercritical fluid extraction of functional ingredients from different natural sources: Plants, food by-products, algae, and microalgae: A review. Food Chemistry, 98(1), 136–148. https://doi.org/10.1016/j.foodchem.2005.05.058 [Google Scholar] [Crossref]
16. Jamel, M.S., Mohamed, A.A., Rahman, R.A., 2012. Extraction of essential oils from spices using supercritical CO₂. Journal of Food Process Engineering, 35(5), pp.815–829. [Google Scholar] [Crossref]
17. Kapoor, I.P.S., Singh, B., Singh, G., Isidorov, V., 2009. Chemistry and in vitro antioxidant activity of volatile oil from black pepper (Piper nigrum L.). Journal of Agricultural and Food Chemistry, 57(12), pp.5358–5364. [Google Scholar] [Crossref]
18. Khan, M.S.A., Ahmad, I., Lee, Y.S., 2021. Antimicrobial activities of essential oils from spices. Food Control, 128, 108182. [Google Scholar] [Crossref]
19. Khaw, K.Y., Parat, M.O., Shaw, P.N., Falconer, J.R., 2017. Solvent supercritical fluid technologies for bioactive compound extraction: A review. The Journal of Supercritical Fluids, 121, pp.86–93. [Google Scholar] [Crossref]
20. Kırkın, C., Güneş, M., 2018. Bioactivity of spice-derived essential oils. Industrial Crops and Products, 111, pp.450–460. [Google Scholar] [Crossref]
21. Kumar, A., Prasad, K., Mishra, A.A., 2021. Drying characteristics and quality evaluation of spices. Journal of Food Processing and Preservation, 45(3), e15245. [Google Scholar] [Crossref]
22. Kumoro, A.C., Hasan, M., Singh, H., 2010. Extraction of essential oil from black pepper using supercritical CO₂. International Journal of Food Engineering, 6(3), pp.1–15. [Google Scholar] [Crossref]
23. Li, X., Zhang, Y., Luo, Y., 2022. Thermal stability of bioactive compounds during supercritical fluid extraction. Food Chemistry, 373, 131550. [Google Scholar] [Crossref]
24. Lin, X., Liu, J., Huang, H., Yu, L., 2013. Supercritical CO₂ extraction of black pepper oil: Process optimization and quality evaluation. The Journal of Supercritical Fluids, 77, pp.49–56. [Google Scholar] [Crossref]
25. Liu, Z., Wang, J., Yuan, Y., 2021. Density-driven solubility behavior in supercritical CO₂ extraction. Chemical Engineering Science, 229, 116095. [Google Scholar] [Crossref]
26. Luca, G., Marino, M., Bruno, M., 2023. Supercritical CO₂ extraction of spice oleoresins: Optimization and characterization. Food and Bioproducts Processing, 138, pp.163–174. [Google Scholar] [Crossref]
27. Maran, J.P., Priya, B., Al-Dhabi, N.A., 2014. Modeling and optimization of supercritical extraction processes. Journal of Food Science and Technology, 51(12), pp.3752–3764. [Google Scholar] [Crossref]
28. Martínez, J. L. (2007). Supercritical fluid extraction of nutraceuticals and bioactive compounds. CRC Press. [Google Scholar] [Crossref]
29. Montgomery, D. C. (2017). Design and analysis of experiments (9th ed.). John Wiley & Sons. [Google Scholar] [Crossref]
30. Morsy, N.F.S., El-Salam, A.M.A., 2017. Chemical composition and biological activities of black pepper essential oil. Journal of Essential Oil Research, 29(5), pp.418–426. [Google Scholar] [Crossref]
31. Nagavekar, N., Singhal, R.S., 2017. Supercritical fluid extraction of essential oils and oleoresins from spices. Food Engineering Reviews, 9, pp.12–27. [Google Scholar] [Crossref]
32. Obek, E., Saptoro, A., 2023. Effect of particle size on mass transfer in supercritical extraction of plant materials. The Journal of Supercritical Fluids, 194, 105784. [Google Scholar] [Crossref]
33. Olalere, O.A., Abdurrahman, N.H., Yunus, R.M., 2021. Optimization strategies in supercritical fluid extraction. Journal of Cleaner Production, 296, 126465. [Google Scholar] [Crossref]
34. Paracampo, A., Johari, N.A., Rahman, R.A., 2022. Quality characteristics of Sarawak black pepper. Journal of Food Quality, 2022, 9876543. [Google Scholar] [Crossref]
35. Ravindran, P.N., Kallupurackal, J.A., 2012. Black Pepper. CRC Press, Boca Raton. [Google Scholar] [Crossref]
36. Reverchon, E., De Marco, I., 2006. Supercritical fluid extraction and fractionation of natural matter. The Journal of Supercritical Fluids, 38(2), pp.146–166. [Google Scholar] [Crossref]
37. Ruslan, N., Rahman, R.A., Salleh, L.M., 2020. Effect of operating parameters on supercritical fluid extraction efficiency. Separation Science and Technology, 55(7), pp.1223–1235. [Google Scholar] [Crossref]
38. Salea, R., Widjojokusumo, E., Hartanti, A.W., 2014. Supercritical fluid extraction of essential oils from spices: Yield and quality evaluation. International Food Research Journal, 21(5), pp.1767–1774. [Google Scholar] [Crossref]
39. Setyaningsih, D., Yuliana, N., Purnomo, E.H., 2021. HPLC determination of piperine in black pepper extracts. Food Analytical Methods, 14, pp.324–332. [Google Scholar] [Crossref]
40. Shrestha, P., Zhang, Y., Tsai, T.Y., 2020. Piperine extraction and quantification from black pepper by supercritical CO₂. Journal of Food Composition and Analysis, 92, 103540. [Google Scholar] [Crossref]
41. Silva, E.A., Meireles, M.A.A., 2016. Supercritical CO₂ extraction of bioactive compounds from spices. Food and Bioprocess Technology, 9(12), pp.1941–1956. [Google Scholar] [Crossref]
42. Sovová, H., 2012. Modeling of supercritical fluid extraction kinetics of plant materials. The Journal of Supercritical Fluids, 66, pp.73–85. [Google Scholar] [Crossref]
43. Sweata, R., 2023. Functional properties and nutraceutical applications of black pepper oil. Journal of Food Science, 88(4), pp.1501–1512. [Google Scholar] [Crossref]
44. Tran, T.T.X., Pham, Q.L., Nguyen, T.T., 2019. Comparison of extraction methods for essential oils from spices. Separation Science and Technology, 54(10), pp.1612–1622. [Google Scholar] [Crossref]
45. Tiong, J.H., Rosazlina, K., 2011. Maturity effects on piperine content in Piper nigrum L. Malaysian Journal of Agricultural Research, 40(2), pp.135–142. [Google Scholar] [Crossref]
46. Uwineza, P.A., Waśkiewicz, A., 2020. Recent advances in supercritical fluid extraction of bioactive compounds. Food Chemistry, 310, 125943. [Google Scholar] [Crossref]
47. Vinod, K., Manju, S., Bansal, T., 2014. Advances in supercritical fluid extraction technology. Journal of CO₂ Utilization, 6, pp.61–70. [Google Scholar] [Crossref]
48. Yang, L., Chen, J., Zhang, H., 2015. Influence of temperature and pressure on supercritical extraction of essential oils. The Journal of Supercritical Fluids, 104, pp.98–104. [Google Scholar] [Crossref]
49. Yadav, A., Singh, S., 2020. Rheological behavior and viscosity analysis of essential oils. Journal of Food Engineering, 278, 109933. [Google Scholar] [Crossref]
Metrics
Views & Downloads
Similar Articles
- Green Synthesis of Calcium Oxide Nanoparticles from Pigeon Eggshells for Cement Composites
- Needs Analysis: Development of an Interactive Digital Storybook in Teaching Mixtures and their Characteristics among Grade 6 Learners
- Thickness Dependent Structural, Optical, Electrical and Gas Sensing properties of ZnO thin film
- Forensic Chemistry Laboratory Works from Home: Challenges Encountered by Criminology Students During the Conduct of their Laboratory Activities at Home
- The Concept of Wellness Club and How it Differs from the Present Gym?