Supercritical CO2 Extraction of Narcissus poeticus L. Flowers for the Isolation of Volatile Fragrance Compounds

The flowers of Narcissus poeticus are used for the isolation of valuable fragrance substances. So far, as the majority of these substances consist of volatile and sensitive to heat compounds, there is a need of developing effective methods for their recovery. In this study, freeze-dried N. poeticus inflorescences were extracted with pure supercritical CO2 (SFE-CO2) and its mixture with 5% co-solvent ethanol (EtOH) at 40 °C. Extract yields varied from 1.63% (12 MPa) to 3.12% (48 MPa, 5% EtOH). In total, 116 volatile compounds were identified by GC-TOF/MS in the extracts, which were divided into 20 different groups. Benzyl benzoate (9.44–10.22%), benzyl linoleate (1.72–2.17%) and benzyl alcohol (0.18–1.00%) were the major volatiles among aromatic compounds. The amount of the recovered benzyl benzoate in N. poeticus SFE-CO2 extracts varied from 58.98 ± 2.61 (24 MPa) to 91.52 ± 1.36 (48 MPa) mg/kg plant dry weight (pdw). α-Terpineol dominated among oxygenated monoterpenes (1.08–3.42%); its yield was from 9.25 ± 0.63 (12 MPa) to 29.88 ± 1.25 (48 MPa/EtOH) mg/kg pdw. Limonene was the major monoterpene hydrocarbon; (3E)-hexenol and heneicosanol dominated among alcohols and phenols; dihydroactinidiolide and 4,8,12,16-tetramethyl heptadecan-4-olide were the most abundant lactones; heptanal, nonanal, (2E,4E)-decadienal and octadecanal were the most abundant aldehydes. The most important prenol lipids were triterpenoid squalene, from 0.86 ± 0.10 (24 MPa) to 7.73 ± 0.18 (48 MPa/EtOH) mg/kg pdw and D-α-tocopherol, from 1.20 ± 0.04 (12 MPa) to 15.39 ± 0.31 (48 MPa/EtOH) mg/kg pdw. Aliphatic hydrocarbons (waxes) constituted the main part (41.47 to 54.93%) in the extracts; while in case of a 5% EtOH the percentage of alkanes was the lowest. The fraction of waxes may be removed for the separation of higher value fragrance materials. In general, the results obtained are promising for a wider application of SFE-CO2 for the recovery of fragrance substances from N. poeticus flowers.

Pressurized Solvent Extraction of Paulownia Bark Phenolics

Paulownia bark is mostly utilized jointly with wood, but the possibility of a separate valorization through the pressurized extraction of bark bioactives has been assessed. Subcritical water extraction and supercritical CO2 extraction are green technologies allowing shorter times than conventional solvent extraction under atmospheric shaken conditions. Subcritical water extraction was carried out at temperatures ranging from 140 to 240 °C and supercritical CO2 extraction was performed at different pressures (10, 20 and 30 MPa), temperatures (35, 45 and 55 °C) and ethanol concentrations (0, 10 and 15% (w/w)). Subcritical water extraction under a non-isothermal operation during heating up to 160 °C (19 min) provided extraction yields up to 30%, and the extracts contained up to 7% total phenolics with an ABTS (2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid)) radical scavenging capacity equivalent to 35% the activity of Trolox, whereas at 240 °C, the yield decreased to 20%, but the phenolic content reached 21%, and the antiradical activity was equivalent to 85% of Trolox. Supercritical CO2 extraction at 30 MPa, 45 °C and 30 min reached a global yield of 2% after 180 min of extraction, but the product showed very low antiradical capacity. Gallic acid, vanillic acid, vanillin and apigenin were the major phenolic compounds found in the extracts.

Enzymatic and Microwave Pretreatments and Supercritical CO2 Extraction for Improving Extraction Efficiency and Quality of Origanum Vulgare L. spp. hirtum Extracts

The goal of the study was to establish a procedure for improving the efficiency of supercritical carbon dioxide (scCO2) extraction of Origanum vulgare L. spp. hirtum (Greek oregano) and enhancing the quality of obtained extracts. Microwave and enzymatic pretreatments of the plant material were applied prior to the scCO2 extraction. It was determined that the microwave pretreatment with irradiation power 360 W during 2 min accelerated the extraction of lipophilic compounds and provided a twofold higher extraction yield compared to the control. Moreover, this pretreatment also led to an increase in oxygenated monoterpenes content and the most dominant component carvacrol, as well as the extracts’ antioxidant activity. The enzymatic pretreatment caused a significant increase in the extraction yield and the attainment of the extract with the most potent antioxidant properties. Coupling the pretreatments with scCO2 extraction improves the process of obtaining high value lipophilic products of oregano in terms of utilization of the plant material, acceleration of the extraction with the possibility to adjust its selectivity and quality of extracts, and enhancement of biological activity.

Utilization of Industrial Rosa damascena Mill. By-products and Cocoa Pod Husks as Natural Preservatives in Muffins

Cocoa Pod Husks (CPH) and by-product from supercritical CO2 extracted Rosa damascena Mill. (RDCO2) were used as biopreservatives in muffins. Both by-products were rich source of polyphenols: 28.3 ± 0.6 mg/g Dry Weight (DW) and 17.9 ± 0.7 mg/g DW RDCO2 and CPH, respectively, and exhibited potent antioxidant capacity: 449.1 ± 8.5 µmol Trolox Equivalents (TE)/g DW (by ORAC method) and 58.9 ± 2.1 µmol Gallic Acid Equivalents (GAE)/g DW (by HORAC method) for the RDCO2, and 373.8 ± 9.0 µmol TE/g DW (by ORAC) and 36.8 ± 3.8 µmol GAE/g DW (by HORAC) for the CPH. RDCO2 extracts successfully inhibited development of several important pathogenic and saprophytic microorganisms causing microbial spoilage of food systems. The control muffins were good for consumption up to the 17th day, while the products supplemented with RDCO2 and CPH: until 20th day of storage at 22 ± 0.5 °C. The amount of dietary fibers in muffins supplemented with both by-products increased 3 times (8.57 ± 0.12 %) compared to control (2.91 ± 0.12 %) and the polyphenolic compounds increased 2.5 times (from 50.0 ± 0.3 for the control to 185.9 ± 0.6 mg/g DW). For the first time by-product of supercritical CO2 extraction of Rosa damascena Mill. was characterized and used as natural and cheap biopreservative.

COMBINED MOBILE SUPER CRITICAL CO2 EXTRACTION PLANT

A detailed description of an experimental mobile installation of a new generation, its complete set and the possibilities of supercritical CO2-extraction for processing plant raw materials are presented. New engineering solutions in the operation of a mechanical system were demonstrated, including an improved design of a high gas pressure throttle valve installed in storage tanks and innovations in the system for loading and unloading raw materials using removable nozzles. The operating parameters of the functional elements and their resource are indicated.