In this study, an efficient utilization and valorization of mandarin peel (Citrus unshiu Marc. var. Kuno) was investigated using innovative and green extraction techniques. The first step of this study included the extraction and analysis of the volatile compounds by performing a supercritical CO₂ (SC-CO₂) extraction under different operating pressure conditions (100 and 300 bar). The analysis of volatile compounds of the obtained extracts was conducted by gas chromatography-mass spectrometry (GC-MS), and limonene was found to be the dominant volatile component (13.16% at 100 bar; 30.65% at 300 bar). After SC-CO₂ treatment, the exhausted citrus peel waste enriched with bioactive compounds was subjected to subcritical water extraction (SWE) in a wide temperature range (130–220 °C) using different solvent-solid ratio (10–30 mL/g) in time periods from 5 to 15 min, in order to obtain bioflavonoids. Identification and quantification of present bioflavonoids was conducted by high-performance liquid chromatography with a with a diode array detector (HPLC), and hesperidin (0.16–15.07 mg/g) was determined as the most abundant flavanon in mandarin peel with other polyphenolic compounds that were possible by-products of thermal degradation. At higher temperatures, the presence of 5-hydroxymethylfurfural (5-HMF) and chlorogenic acid were detected. Antiradical activity and total phenolic content in the extracts were determined using spectrophotometric methods, while the process optimization was performed by response surface methodology (RSM).

Natural products are increasingly in demand in dermatology and cosmetology. In the present study, highly valuable supercritical CO₂ (sCO₂) extracts rich in bioactive compounds with antiradical and antibacterial activity were obtained from the inflorescences of industrial hemp. Volatile compounds were analyzed by gas chromatography in tandem with mass spectrometry (GC-MS), while cannabinoids were determined by high performance liquid chromatography (HPLC-DAD). Extraction yields varied from 0.75 to 8.83%, depending on the pressure and temperature applied. The extract obtained at 320 bar and 40 °C with the highest content (305.8 µg mg⁻¹) of cannabidiolic acid (CBDA) showed the best antiradical properties. All tested extract concentrations from 10.42 µg mL⁻¹ to 66.03 µg mL⁻¹ possessed inhibitory activities against E. coli, P. aeruginosa, B. subtilis, and S. aureus. The sCO₂ extract with the highest content of cannabidiol (CBD) and rich in α-pinene, β-pinene, β-myrcene, and limonene was the most effective. The optimal conditions for sCO₂ extraction of cannabinoids and volatile terpenes from industrial hemp were determined. The temperature of 60 °C proved to be optimal for all responses studied, while the pressure showed a different effect depending on the compounds targeted. A low pressure of 131.2 bar was optimal for the extraction of monoterpenes, while extracts rich in sesquiterpenes were obtained at 319.7 bar. A high pressure of 284.78 bar was optimal for the extraction of CBD.

With globalization, growing popularization and changes in dietary habits where more processed food is consumed, a generation of food wastes and by-products has increased. Under-exploitation of by-products and waste leads to finance losses and environmental pollution although most of the waste are a rich source of bioactive compounds. Using spray drying process, extracted bioactive compounds from food wastes and by-products can be transferred into powder form, and returned to the food chain. Spray drying technique showed to be the most convenient, energy efficient and time-saving process, where a liquid is directly transformed into stable powder, which can be stored for a prolonged time or easily incorporated into other products. This review article focuses on the application of processing parameters of spray drying with specific emphasis on the production of dry extracts of food waste and their influence on powder properties. Research gaps and challenges along with possible applications are also discussed.

The endemic brown macroalga Fucus virsoides J. Agardh from the Adriatic Sea was in the focus of the present research. The volatiles of fresh (FrFv) and air-dried (DrFv) samples of F. virsoides obtained by headspace solid-phase microextraction (HS-SPME) and hydrodistillation (HD) were analyzed by gas chromatography equipped with flame ionization detector and mass spectrometry (GC-FID/MS). The major HS-FrFv compound was pentadecane (61.90–71.55%) followed by pentadec-1-ene (11.00–7.98%). In HS-DrFv, pentadec-1-ene was not present, and few lower aliphatic compounds appeared, as well as benzaldehyde and benzyl alcohol. In HD-FrFv, particularly abundant were alkenes (such as pentadec-1-ene (19.32%), or (E)-pentadec-7-ene (8.35%)). In HD-DrFv, more oxidation products were present (e.g., carbonyl compounds such as tridecanal (18.51%)). The fatty acids profile of freeze-dried sample (FdFv) after conversion to methyl esters was determined by GC-FID, and oleic acid was dominant (42.28%), followed by arachidonic acid (15.00%). High-performance liquid chromatography-high-resolution mass spectrometry with electrospray ionization (HPLC-ESI-HRMS) was used for the screening of less polar fractions (F3 and F4) of F. virsoides. Mono- and diglycerides of stearic, palmitic, oleic, and arachidonic acids were found. Terpenoids and steroids comprised the compounds C₂₀H₃₀₍₃₂₎O₂ and C₂₉H₄₈O₍₂₎. Among carotenoids, fucoxanthin was identified. Chlorophyll derivatives were also found (C₅₅H₇₄₍₇₂₎N₄O_(5-7)), dominated by pheophytin a. The antioxidant activity of the fractions was investigated by in vitro assays (oxygen radical absorbance capacity (ORAC), reduction of radical cation (ABTS•⁺), 2,2-diphenyl-1-picryl-hydrazyl-hydrate (DPPH) assay, and ferric reducing antioxidant power (FRAP)) and by in vivo zebrafish model (along with fish embryotoxicity). In vitro experiments proved good radical scavenging abilities of F3 and F4 fractions, which were additionally supported by the protective effect against hydrogen peroxide-induced oxidative stress in zebrafish embryos.

Saffron (Crocus sativus) floral by-products are a source of phenolic compounds that can be recovered and used in the nutraceutical, pharmaceutical, or cosmetic industries. This study aimed to evaluate the phenolic compounds’ extraction using green extraction techniques (GETs) in saffron floral by-products and to explore the influence of selected extraction techniques on the phytochemical composition of the extracts. Specifically, ultrasound-assisted extraction (UAE), subcritical water extraction (SWE), and deep eutectic solvents extraction (DESE) were used. Phenolic compounds were identified with (HR) LC-ESI-QTOF MS/MS analysis, and the quantitative analysis was performed with HPLC-PDA. Concerning the extraction techniques, UAE showed the highest amount for both anthocyanins and flavonoids with 50:50% v/v ethanol/water as solvent (93.43 ± 4.67 mg/g of dry plant, dp). Among SWE, extraction with 96% ethanol and t = 125 °C gave the best quantitative results. The 16 different solvent mixtures used for the DESE showed the highest amount of flavonoids (110.95 ± 5.55–73.25 ± 3.66 mg/g dp), while anthocyanins were better extracted with choline chloride:butane-1,4-diol (16.0 ± 0.80 mg/g dp). Consequently, GETs can be employed to extract the bioactive compounds from saffron floral by-products, implementing recycling and reduction of waste and fitting into the broader circular economy discussion.

This work reports the preparation of amino acid-functionalized CQDs from citric acid by facile hydrothermal synthesis. The prepared N-doped CQDs exhibited excellent optical, physical, and chemical properties, and the differences were observed among the six different amino acids used as nitrogen dopants (Leu, Trp, Lys, Arg, Ala, His). Compared to the blank sample (without the addition of amino acids), N-doped CQDs have shown significantly higher quantum yield, also demonstrating the potential in metal ion sensing. The highest quantum yield of 36.45%, with a peak excitation/emission of 340/406 nm, was achieved using citric acid and amino acid Leu (CQD@Leu), treated at temperature of 180 °C during 9 h. The prepared samples were investigated toward metal ion selectivity (Ca²⁺, Cu²⁺, Fe³⁺, K⁺, Hg²⁺, Mg²⁺, Al³⁺, Mn²⁺, and Na⁺), and the CQD@Leu showed a selective and sensitive response upon the addition of Fe³⁺ ions. Therefore, CQD@Leu was selected for further investigation in Fe³⁺ detection in the model system and real well water samples. A developed model was described by a logistic function with a good coefficient of determination of R² = 0.9982, while the linear range was determined in the concentration range from 0.3 mol dm⁻³ to 30 mol dm⁻³, with a determined limit of detection of LOD = 1.77 ± 0.01 mol dm⁻³ and limit of quantification of LOQ = 5.89 ± 0.04 mol dm⁻³. Furthermore, the results of the in vitro cytotoxicity test (MTT) with normal and tumor cell lines (MRC-5, HeLa, NCI-H358, and CaCo-2) clearly demonstrate the excellent biocompatibility of CQD@Leu.