A Network of Processes for Biorefining Burdock Seeds and Roots.

In this work, a novel sustainable approach was proposed for the integral valorisation of Arctium lappa (burdock) seeds and roots. Firstly, a preliminary recovery of bioactive compounds, including unsaturated fatty acids, was performed. Then, simple sugars (i.e., fructose and sucrose) and phenolic compounds were extracted by using compressed fluids (supercritical CO2 and propane). Consequently, a complete characterisation of raw biomass and extraction residues was carried out to determine the starting chemical composition in terms of residual lipids, proteins, hemicellulose, cellulose, lignin, and ash content. Subsequently, three alternative ways to utilise extraction residues were proposed and successfully tested: (i) enzymatic hydrolysis operated by Cellulases (Thricoderma resei) of raw and residual biomass to glucose, (ii) direct ethanolysis to produce ethyl levulinate; and (iii) pyrolysis to obtain biochar to be used as supports for the synthesis of sulfonated magnetic iron-carbon catalysts (Fe-SMCC) to be applied in the dehydration of fructose for the synthesis of 5-hydroxymethylfurfural (5-HMF). The development of these advanced approaches enabled the full utilisation of this resource through the production of fine chemicals and value-added compounds in line with the principles of the circular economy.

Brewer's Spent Grain, Coffee Grounds, Burdock, and Willow-Four Examples of Biowaste and Biomass Valorization through Advanced Green Extraction Technologies.

This paper explores the transformation of biowastes from food industry and agriculture into high-value products through four examples. The objective is to provide insight into the principles of green transition and a circular economy. The first two case studies focus on the waste generated from the production of widely consumed food items, such as beer and coffee, while the other two examine the potential of underutilized plants, such as burdock and willow, as sources of valuable compounds. Phenolic compounds are the main target in the case of brewer's spent grain, with p-coumaric acid and ferulic acid being the most common. Lipids are a possible target in the case of spent coffee grounds with palmitic (C16:0) and linoleic (C18:2) acid being the major fatty acids among those recovered. In the case of burdock, different targets are reported based on which part of the plant is used. Extracts rich in linoleic and oleic acids are expected from the seeds, while the roots extracts are rich in sugars, phenolic acids such as chlorogenic, caffeic, o-coumaric, syringic, cinnamic, gentisitic, etc. acids, and, interestingly, the high-value compound epicatechin gallate. Willow is well known for being rich in salicin, but picein, (+)-catechin, triandrin, glucose, and fructose are also obtained from the extracts. The study thoroughly analyzes different extraction methods, with a particular emphasis on cutting-edge green technologies. The goal is to promote the sustainable utilization of biowaste and support the green transition to a more environmentally conscious economy.

Sustainable Transformation of Two Algal Species of Different Genera to High-Value Chemicals and Bioproducts.

This study investigates the potential of two algae species from different genera, namely the recently isolated Scenedesmus obliquus BGP and Porphyridium cruentum, from the perspective of their integral sustainable transformation to valuable substances. Conventional Soxhlet and environmentally friendly supercritical fluid extraction were applied to recover oils from the species. The extracts were characterized through analytical techniques, such as GC-Fid and LC-MS/MS, which allowed their qualitative and quantitative differentiation. Thus, P. cruentum oils contained up to 43% C20:4 and C20:5 fatty acids, while those of S. obliquus BGP had only residual amounts. The LC-MS/MS analysis of phenolic compounds in the S. obliquus BGP and P. cruentum extracts showed higher content of 3-OH-4-methoxybenzoic acid and kaempferol 3-O-glycoside in the former and higher amounts of ferulic acid in the latter. Total phenolic content and antioxidant activity of the oils were also determined and compared. The compositional analysis of the oil extracts revealed significant differences and varying potentialities based on their genera and method of extraction. To the best of our knowledge our work is unique in providing such detailed information about the transformation prospects of the two algae species to high-value chemicals and bioproducts.

Assessment of Gnaphalium viscosum (Kunth) Valorization Prospects: Sustainable Recovery of Antioxidants by Different Techniques.

This work investigates the prospects for exploitation of Gnaphalium viscosum (Kunth) abundant but with limited applications till present biomass. The feasibility of traditional techniques (two-phase solvent, and the benchmark Soxhlet extraction) and supercritical extraction without/with a cosolvent at T = 40-60 °C and p = 30-50 MPa was examined to explore the possibility of recovering phytochemicals from G. viscosum leaves, flowers and stems. The efficiency of the techniques was assessed and compared based on yield, influence of solvents used, total phenolic content and antioxidant activity of the extracts. Phenolics of different complexities were identified and quantified by applying LC (LC-MS/MS, and LC-HRAM), while the fatty acid profile was determined by GC-FID. The results of this extensive study demonstrated the huge valorization potential and prospects of G. viscosum, since highly potent antioxidants such as kaempferol, kaempferol-3-O-ß-d-glucoside (astragalin), and chlorogenic acid were ascertained in considerable amounts. Furthermore, for the first time, the presence of leontopodic acid, a greatly substituted derivative of glucaric acid, was detected in the species.

Microwave-Assisted Extraction of Phenolic Compounds from Spent Coffee Grounds. Process Optimization Applying Design of Experiments.

In this study, sustainable technology microwave-assisted extraction (MAE) in association with green solvents was applied to recover phenolic compounds from spent coffee grounds (SCGs). A design of experiments (DOE) was used for process optimization. Initially, a 24-1 two level Fractional Factorial Design was used and ratios "solvent to solute" and "ethanol to water" were identified as the significant experimental factors. Consequently, Central Composite Design (CCD) was applied to analyze the effects of the significant variables on the response yield, total polyphenols content (TPC), and antioxidant activity (AA) by the DPPH assay method, and quadratic surfaces to optimize those responses were generated. The values of the significant factors of 16.7 (solvent/solute) and 68.9% (ethanol/water) were optimized simultaneously the yield (%) at 6.98 ± 0.27, TPC (mg GAE/g) at 117.7 ± 6.1, and AA (µmol TE/g) at 143.8 ± 8.6 and were in excellent agreement with those predicted from the CCD model. The variations of the compositions of the lipids, caffeine, pentacyclic diterpenes, and FAME as a function of the dominant factor % ethanol in the solvent mixture were analyzed by applying NMR and GC-FID, and the results obtained confirmed their determinative significance.

Extraction of thymol from different varieties of thyme plants using green solvents.

BACKGROUND: Thymol (2-isopropyl-5-methylphenol) is the main monoterpene phenol found in thyme essential oil. This compound has revealed several biological properties, including antibacterial, anti-inflammatory and antioxidant activities. In this work, a comparison was made between the performance of different green solvents (ethanol, limonene and ethyl lactate), by pressurized liquid extraction (PLE) and supercritical fluid extraction (SFE) at different conditions, to extract thymol from three different varieties of thyme (Thymus vulgaris, Thymus zygis and Thymus citriodorus). Additionally, new solubility data of thymol in limonene and ethanol at ambient pressure and temperatures in the range 30-43 °C are reported. RESULTS: The highest thymol recoveries were attained with T. vulgaris (7-11 mg g(-1)). No thymol could be quantified in the PLE samples of T. citriodorus. The highest concentrations of thymol in the extracts were obtained with limonene. Thymol is very soluble in both solvents, particularly in ethanol (∼900 mg g(-1) at ∼40 °C), and is the main compound (in terms of peak area) present in the essential oil extracts obtained. CONCLUSION: The three solvents show good capacity to extract thymol from T. vulgaris and T. zygis by PLE. Although PLE proved to be a suitable technology to extract thymol from thyme plants, the highest concentrations of thymol were obtained by SFE with supercritical CO2 .