Supercritical CO₂ extraction is a green method that combines economic and environmental benefits. Microalgae, on the other hand, is a biomass in abundance, capable of providing a vast variety of valuable compounds, finding applications in the food industry, cosmetics, pharmaceuticals and biofuels. An extensive study on the existing literature concerning supercritical fluid extraction (SFE) of microalgae has been carried out focusing on carotenoids, chlorophylls, lipids and fatty acids recovery, as well as the bioactivity of the extracts. Moreover, kinetic models used to describe SFE process and experimental design are included. Finally, biomass pretreatment processes applied prior to SFE are mentioned, and other extraction methods used as benchmarks are also presented.

Macroalgae Ulva lactuca, has been employed as a natural source for the production of extracts with potent bioactivity. The biochemical characterization showed that the macroalgae biomass contains a remarkable amount of the polysaccharide Ulvan (49.9 wt%) which is a valuable chemical compound well known for its benefits in human health. Four nontoxic solvents, water, ethyl acetate, ethanol, and an ethanol/water mixture (70:30 v/v) were examined for their recovery efficiency of total carotenoid and phenolic contents. Experimental results showed that the aqueous mixture of ethanol was the most efficient solvent in the recovery of bioactive compounds with extraction yield of 10–15% dw. The effect of extraction parameters, namely time, temperature, and the ratio of biomass to solvent, on the carotenoid and phenolic compounds’ content, antioxidant activity, and extraction yield, was investigated, using the ethanol/water mixture as a solvent. The extract obtained under 60 °C, 3 h of extraction time and 1:10 biomass to solvent mass ratio showed the highest antioxidant activity. This extract maintained its antioxidant capacity almost stable for five days of storage under cool and dark conditions. Finally, specific phenolic and carotenoid compounds in the U. lactuca extracts were identified using the High-Performance Liquid Chromatography (HPLC) technique.

The production of bioactive products from microalgae biomass with efficient and environmentally friendly technologies is a field of great research interest. The present work focuses on the recovery of high-added value bioactive components from Chlorella vulgaris through microwave-assisted extraction (MAE) with aq. ethanol 90% v/v. The effect of extraction temperature (40–60 °C), duration (5–25 min), solvent-to-biomass ratio (20–90 mL_solv/g_biom), and microwave power (300–800 watts) was investigated regarding the extraction yield, extract’s chlorophyll, carotenoid and phenolic content, and antioxidant activity. MAE optimization at 60 °C, 300 watts, 14 min, and 22 mL_solv/g_biom led to 11.14% w/w yield, 63.36 mg/g_extr total chlorophylls, 7.06 mg/g_extr selected carotenoids of astaxanthin, lutein and β-carotene, 24.88 mg/g_extr total carotenoids, 9.34 mg_GA/g_extr total phenolics, and 40.49 mg_extr/mg_DPPH IC₅₀ (antioxidant activity indicator). Moreover, the conventional solid-liquid extraction (SLE) with aq. ethanol 90% v/v, the supercritical fluid extraction (SFE) with CO₂, as well as SFE with cosolvent addition (10% w/w ethanol), were also performed for comparison purposes. The results revealed that SLE presented the highest yield. However, the non-conventional methods of MAE and SFE led to extracts of competitive or even better quality under significantly shorter extraction duration.

C. vulgaris microalgae biomass was employed for the extraction of valuable bioactive compounds with deep eutectic-based solvents (DESs). Particularly, the Choline Chloride (ChCl) based DESs, ChCl:1,2 butanediol (1:4), ChCl:ethylene glycol (1:2), and ChCl:glycerol (1:2) mixed with water at 70/30 w/w ratio were used for that purpose. The extracts’ total carotenoid (TCC) and phenolic contents (TPC), as well as their antioxidant activity (IC50), were determined within the process of identification of the most efficient solvent. This screening procedure revealed ChCl:1,2 butanediol (1:4)/H₂O 70/30 w/w as the most compelling solvent; thus, it was employed thereafter for the extraction process optimization. Three extraction parameters, i.e., solvent-to-biomass ratio, temperature, and time were studied regarding their impact on the extract’s TCC, TPC, and IC50. For the experimental design and process optimization, the statistical tool Response Surface Methodology was used. The resulting models’ predictive capacity was confirmed experimentally by carrying out two additional extractions under conditions different from the experimental design.

Harvesting of microalgae is a crucial step in microalgae-based mass production of different high value-added products. In the present work, magnetic harvesting of Chlorella vulgaris was investigated using microwave-synthesized naked magnetite (Fe₃O₄) particles with an average crystallite diameter of 20 nm. Optimization of the most important parameters of the magnetic harvesting process, namely pH, mass ratio (m_r) of magnetite particles to biomass (g/g), and agitation speed (rpm) of the C. vulgaris biomass–Fe₃O₄ particles mixture, was performed using the response surface methodology (RSM) statistical tool. Harvesting efficiencies higher than 99% were obtained for pH 3.0 and mixing speed greater or equal to 350 rpm. Recovery of magnetic particles via detachment was shown to be feasible and the recovery particles could be reused at least five times with high harvesting efficiency. Consequently, the described harvesting approach of C. vulgaris cells leads to an efficient, simple, and quick process, that does not impair the quality of the harvested biomass.

The recovery of phenolic compounds from olive leaves (Olea europaea L.) has received special attention due to their significant potential for applications in food, nutraceuticals, cosmetics, and pharmaceuticals. In this work, the extraction of the phenolic compounds from olive leaves was examined by means of conventional extraction and microwave-assisted extraction (MAE) using nontoxic common solvents such as ethanol and water as well as using promising environmentally friendly, Deep Eutectic Solvents (DESs) and their mixtures with ethanol or water. The effects of the various parameters that likely govern the extractability of the bioactive compounds of olive leaves (OL), such as the solvent type, temperature, and biomass to solvent mass ratio, were studied and evaluated with regard to the oleuropein and hydroxytyrosol content, antioxidant activity, and total phenolic content of the extracts. The study also explores the effects of the microwave-assisted extraction parameters, namely irradiation power and time, on the total phenolic content and antioxidant activity of the extracts. The findings of this work suggest that among the solvents studied, the solvent mixture consisting of the DES choline chloride:acetic acid with a molar ratio of 1:2 and ethanol (80:20 w/w) is highly effective in recovering extracts rich in phenolic compounds and with significant antioxidant activity. Moreover, it is demonstrated that the MAE method allows for the recovery of bioactive compounds in a very short processing time.