•SWE is a suitable friendly technique to extract cacao pod husk pectin.•SW extracts pectin with higher yields and molecular mass than citric acid.•Cacao pod husk pectin structure is not affected by ...SC-CO2 pretreatment.•SWE is a green method for pectin recovery from cacao pod husk after phenols SFE.
Pectin was obtained with citric acid and subcritical water extraction from cacao pod husk with or without a previous step consisting of a supercritical fluid extraction of phenols. By subcritical conditions a higher yield (10.9%) was attained in a time 3-fold shorter than that obtained by conventional extraction (˜8%) and a greater effectiveness in the recovery of pectin with higher molecular weight (750 kDa) was also found. Regarding pectin structure, galacturonic acid and degree of methyl esterification content were similar (˜55 and ˜36%, respectively) in both methods. Moreover, pectin recovered by citric acid presented 2-fold higher amount of impurities as compared to subcritical water extraction. Hardly any effects of a previous supercritical treatment were observed in the structure and composition of pectin, indicating the efficiency of the integrated supercritical carbon dioxide and subcritical water extraction as green processes for the obtainment of phenol and pectin from cacao pod husk.
► Compressed fluids show important advantages for extraction of bioactives. ► SFE, PLE and SWE are fast, reliable and clean methods for extracting bioactives. ► Principles, instrumentation and ...applications of SFE, PLE and SWE are presented.
The improvement of sample-preparation and extraction techniques for determinations of natural bioactive compounds is very important. New concepts relate to not only enhancement of extraction efficiencies but also environmental impact. This evolution towards Green Analytical Chemistry is to new extraction and sample-preparation processes that should be faster, more reproducible and more environmentally friendly.
Compressed fluid-based sample-preparation techniques (e.g., supercritical fluid extraction and pressurized liquid extraction) demonstrate good capabilities. In this review, we update knowledge on the techniques together with the main technical developments and the most notable recent applications for the extraction of bioactive compounds.
This review attempts to provide an updated overview (including works published till June 2006) on the latest applications of compressed fluids as sample preparation techniques for food analysis. ...After a general review of the principles of supercritical fluid extraction (SFE) and pressurized liquid extraction (PLE; also called accelerated solvent extraction, ASE or subcritical water extraction, SWE, when water is employed as extraction solvent), the principal applications of such techniques in the mentioned fields of food and natural products are described, discussing their main advantages and drawbacks.
is an EFSA-approved novel food and dietary supplement with increasing use in nutraceutical production worldwide. This study investigated the neuroprotective potential of bioactive compounds extracted ...from
using green biobased solvents (ethyl acetate, AcOEt, and cyclopentyl methyl ether, CPME) under pressurized liquid extraction (PLE) conditions and supercritical fluid extraction (SFE). Response surface optimization was used to study the effect of temperature and solvent composition on the neuroprotective properties of the PLE extracts, including anticholinergic activity, reactive oxygen/nitrogen species (ROS/RNS) scavenging capacity, and anti-inflammatory activity. Optimized extraction conditions of 40 °C and 34.9% AcOEt in CPME resulted in extracts with high anticholinergic and ROS/RNS scavenging capacity, while operation at 180 °C and 54.1% AcOEt in CPME yielded extracts with potent anti-inflammatory properties using only 20 min. Chemical characterization revealed the presence of carotenoids (neoxanthin, violaxanthin, zeaxanthin, α- and β-carotene) known for their anti-cholinesterase, antioxidant, and anti-inflammatory potential. The extracts also exhibited high levels of omega-3 polyunsaturated fatty acids (PUFAs) with a favorable ω-3/ω-6 ratio (>7), contributing to their neuroprotective and anti-inflammatory effects. Furthermore, the extracts were found to be safe to use, as cytotoxicity assays showed no observed toxicity in HK-2 and THP-1 cell lines at or below a concentration of 40 μg mL
. These results highlight the neuroprotective potential of
extracts, making them valuable in the field of nutraceutical production and emphasize the interest of studying new green solvents as alternatives to conventional toxic solvents.
•In-depth response surface analysis was done for scCO2 extraction of H. pluvialis.•Ethanol cosolvent affected extract’ antioxidant activity more than pressure or temperature.•We investigated a ...further increase in ethanol up to the region of gas-expanded liquids.•Astaxanthin recovery was larger in CO2-expanded ethanol (CXE) than scCO2 extractions.•CXE extracts high-value compounds from microalgae to unprecedented levels.
Microalgae represent diverse branch of microorganism that can produce a wide range of unique functional ingredients that can be used in food, cosmetics, pharmaceuticals, and energy. Among them, Haematococcus pluvialis is known for accumulating the highest levels of a potent natural antioxidant, astaxanthin, which has demonstrated positive health effects. Therefore, the aim of numerous studies has been to develop novel and efficient extraction techniques to produce high-quality (purity and antioxidant activity) extracts, while complying with the Green Chemistry Principles. Supercritical CO2 (scCO2) emerges as an alternative to organic solvents because of its high selectivity and bioactivity-preserving qualities. Nevertheless, astaxanthin is a large molecule with low solubility in scCO2 that usually requires long extractions at high pressures. Ethanol has been used as co-solvent to increase astaxanthin solubility in scCO2. In this work, a Box–Behnken experimental design was used to study the effects of operating pressure (20–35MPa), temperature (40–70°C), and ethanol content in scCO2 (0–13%, w/w) on the yield, astaxanthin content, and antioxidant activity of H. pluvialis extract. Results showed that ethanol content in CO2 has a more significant effect on all responses than pressure and temperature. These results lead us to investigate the effect of a further increase in ethanol content, up to the region of gas-expanded liquids. We studied the effects of temperature (30–60°C) and ethanol content (50–70%, w/w) at a fixed pressure (7MPa) on the same response variables using CO2-expanded ethanol (CXE). Results showed that temperature and ethanol content had a significant influence on astaxanthin yield and antioxidant activity. Also, the overall responses of CXE surpassed scCO2 extractions to match conventional extraction with acetone, maintaining high quality extracts, thus validating the use of this new type of green technology for extraction of high-value compounds.
In the present review, we have tried to highlight foodomics' goals with regards to green chemistry principles providing an update (from mid-2013 up to 2017) on the novelties and new approaches that ...can be employed to make foodomics greener. Although Foodomics covers different fields of research included in food science approached using advanced -omics technologies and associated to sustainability, in the present work only those directly related to green analytical chemistry (GAC) and novel foods development are discussed. Aspects treated in the present work deal with new trends in production of functional food ingredients (through the use of alternative solvents and design of biorefinery processes) and with green alternatives mainly for metabolomics and proteomics. Moreover, different methodologies to quantify the greenness of the processes are presented.
•Updated review (2013–2017) about strategies used to make Foodomics studies greener.•Green solvents and pressurized fluids are good approaches to obtain bioactives.•Green Analytical Chemistry approaches to make -omics platforms greener are discussed.•Several techniques to quantify “greeness” in Foodomics are evaluated.
This work presents a green, downstream process, from extraction to phytochemical characterization and bioactivity testing, to obtain and evaluate the functional properties of phenolic compounds from ...cowpea (Vigna unguiculata (L.) Walp.) seeds and pods. Phenolic-rich extracts were obtained by pressurized liquid extraction (PLE). The main factors affecting the extraction conditions (temperature and solvent) were optimized in order to attain extracts with the highest extraction yield, antioxidant capacity, and total phenolic content. The optimal extraction conditions were 1:1 ethanol:water at 170 °C with one extraction cycle for seeds and three extraction cycles for pods. Phenolic compounds of optimal extract were analyzed by UHPLC-q-TOF-MS/MS (quadrupole-time of flight tandem MS). The obtained PLE-extracts exhibited higher phenolic content and antioxidant activity compared to conventional extraction procedures. The in vitro anti-neurodegenerative potential of extracts was measured through Acetylcholinesterase (AChE) inhibition assay. The results revealed the higher bioactivity observed in cowpea pod samples compared to seed extracts, which might be related to higher levels of quercetin and quercetin glycosides, kaempferol diglucoside, and other tetrahydroxylated flavones and flavonols identified in these samples. These results also provide an added-value benefit to the cultivation of this legume, considering the high potential of cowpea phenolic extracts as nutraceutical and functional ingredients in food formulations.
The fractionation of algae biomass in several high-value compounds that can be used as ingredients in other applications sets the basis of the algae biorefinery approach. The present study aimed at ...the extraction and fractionation of bioactive compounds from the microalga Scenedesmus obliquus, by means of applying a sequential process without the manipulation of the biomass in the extraction cell. This integrated platform of compressed fluid extraction technologies of low-environmental impact was designed in order to produce increases of solvent polarity using non-toxic solvents. The process involved the following steps:(1) supercritical fluid extraction (SFE) using supercritical carbon dioxide (ScCO2); (2) gas expanded liquids (GXL) using 75% ethanol and 25% ScCO2 (v/v) and; (3) pressurized liquid extraction (PLE) using water. Extraction conditions were optimized using response surface methodology (RSM) and kinetic studies. Extraction yield, antioxidant activity as well as contents of total phenols, carotenoids, proteins and sugars were the studied response variables. High performance liquid chromatography coupled to evaporative light-scattering detector (HPLC-ELSD) analyses of the fractions revealed that triacylglycerols were mainly extracted by SFE. Lutein and β-carotene were the main pigments identified in the extracts by HPLC coupled to diode array and mass spectrometry detectors (HPLC-DAD-MS/MS), which were preferentially extracted in the GXL step. Polar compounds such as proteins and sugars remained predominantly in the residue. Therefore, the green downstream platform developed in this study for valorization of the microalgae biomass, is able to produce different fractions with potential application in the food, pharmaceutical and cosmetic industries.
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•Green downstream processing platform for extraction of bioactives from S. obliquus.•Extraction process selective according to the polarity of the solvents used.•ScCO2 extracts were rich in triacylglycerides.•GXL extracts enriched in carotenoids and polar lipids.•Proteins and sugars remained preferentially in the residue.
The Opuntia Stricta var. Dillenii's prickly pears are an underutilized fruits, which provide a great source of betalains (mainly, betacyanins) and phenolic compounds (phenolic acids and flavonoids) ...that could play an important role in health-promotion. This study focuses on the optimization of process for the green extraction of betalains and phenolic compounds from Opuntia stricta var. Dillenii's whole fruits by Pressurized liquid extraction (PLE), using a response surface methodology (RSM) by a central composite design (CCD) in order to obtain rich extracts in betalains and phenolic compounds with the similar profile of the original one found in O. dillenii fruits (avoiding any degradation of these compounds during the extraction process) with proven biological activities. For PLE optimization, the ethanol volume in water (0–100%, v/v) and the temperature (25–65°C) were selected as independent variables. The identification and quantification of the individual bioactive compounds of the obtained green extracts were done by HPLC-DAD-ESI/MS and HPLC-DAD-ESI/QTOF and their biological activities were determined by in vitro tests, as: the antioxidant activity by the ORAC method and the anti-inflammatory activity by the hyaluronidase inhibition method. Ethanol volume in water (%, v/v) was the variable with most significant (p ≤ 0.05) effect in the target responses (bioactive content and biological activities). The best results were obtained at 50% ethanol in water (v/v) and 25°C temperature (run 10) obtaining extracts with betalains as 2.34 ± 0.18 mg of betanin/g dry weight, 2.51 ± 0.04 mg of 5′´-O-E-sinapoyl-2′-apyosil-phyllocactin/g dry weight, 2.32 ± 0.19 mg of neobetanin/g dry weight and phenolic compounds, 2.08 ± 0.07 mg of piscicid acid/g dry weight and 0.25 ± 0.02 mg of isorhamnetin glucoxyl-rhamnosyl-pentoside (IG2) /g dry weight. The betalain and phenolic profile of the PLE extracts was quite similar to the profile from the conventional extraction, but PLE extraction process enhanced the extraction of some bioactives as neobetanin (39%) andpiscidic acid (124%). All employed PLE process CCD combinations significantly upgrade the in vitro biological activities (antioxidant and anti-inflammatory) of the Opuntia stricta var. Dillenii's PLE green extracts.
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