The PLE method was employed to extract polyphenols from olive leaves. This was achieved by utilizing different solvent mixtures, including water–glycerol (from 0% to 30% w/w) and water–ethanol (from 0% to 30% w/w) combined with varying temperatures of extraction (50 °C and 70 °C). The solvent levels and process parameters were selected by prior research [31 (link),32 (link)]. Then, an extraction cell was used to load ~10 g of dried olive leaves and 40 g of neutral quartz sand, which were mixed previously. For extraction, a pressurized liquid system (ASE 150, Dionex, Thermo Fisher, San Jose, CA, USA) was used combined with the following parameters: 10 MPa pressure, a single extraction cycle, 150% wash volume, 250 s of nitrogen purge time, and a static extraction duration of 5 min. The obtained extracts were filtered and stored at −20 °C.
Ase 150
Manufactured by Thermo Fisher Scientific
Sourced in United States
The ASE 150 is a laboratory instrument designed for automated solid-phase extraction (SPE) of samples. It is capable of performing various sample preparation steps, including conditioning, loading, washing, and elution, in a fully automated manner. The ASE 150 is a versatile and efficient tool for sample preparation in analytical laboratories.
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Lab products found in correlation
2707 autosampler, by Waters Corporation (1 mentions)
Photodiode array detect or 2998, by Waters Corporation (1 mentions)
1525 binary hplc pump, by Waters Corporation (1 mentions)
Hplc system, by Waters Corporation (1 mentions)
Ethanol, by Merck Group (1 mentions)
Methanol, by Merck Group (1 mentions)
Cellulose filter, by Cytiva (1 mentions)
Centrifugal concentrator, by Eppendorf (1 mentions)
Hydromatrix, by Agilent Technologies (1 mentions)
13 protocols using ase 150
1
Polyphenol Extraction from Olive Leaves
2
Accelerated Solvent Extraction and HPLC Analysis
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An ASE-150 (Accelerated Solvent Extraction, Thermo Fisher®, Sunnyvale, CA, USA) apparatus with 100 mL stainless steel cells was used for extractions. A Waters HPLC system, photodiode array detector 2998, autosampler 2707 and binary HPLC pump 1525 (Waters, Milford, MA, USA) were used for analysis and method validation. Chromatographic separation was performed using a Kinetex Biphenyl TMS end-capped column, 4.6 × 150 mm with 5 μm particle size (Phenomenex®, Torrance, CA, USA). The mobile phase contained 0.2% formic acid in water (phase A) or acetonitrile (phase B). The total run time was 21 min: gradient elution started with 40% phase B reaching 45% in 1 min, continued until 9 min when the phase reached 80%. Phase B was subsequently raised by 5% over 4 min (85%) and maintained for 3 min. After one more min, B reached 100%, before returning to the initial phase in 1 min, where it was maintained for 3 min. The 10 μL sample was injected at 1 mL/min.
3
Extraction and Isolation of Campomanesia Leaves and Roots
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C. adamantium O. Berg leaves and roots were collected following the identification of the plant and authorization of the SISBIO (Sistema de Autorização e Informação em Biodiversidade, permit number 54470).
Leaves and roots of C. adamantium O. Berg were collected in Dourados, in the state of Mato Grosso do Sul, Brazil (coordinates: 22° 02′ 47.9 S′ and 055° 08′ 14.3′ W). The samples were cleaned, dried in a convection oven at 45°C, and ground using a Croton knife mill. An exsiccated sample was deposited in the Herbarium of the Federal University of Grande Dourados, Mato Grosso do Sul, Brazil, with registration number 4108.
Extracts were prepared from the powdered material using an accelerated solvent extractor (ASE®-150, Dionex), as described by Espindola et al. (2016 (link)). The samples were placed in a cell of 100 mL and extracted with distilled water at temperature of 125°C through two 5 min static cycles, with an 80% flush volume and a 60 s purge. The extracts were lyophilized to obtain the dry extract. Thus, the aqueous extracts of Campomanesia leaves (AECL) and roots (AECR) were obtained with a yield of 13 and 6%, respectively.
Leaves and roots of C. adamantium O. Berg were collected in Dourados, in the state of Mato Grosso do Sul, Brazil (coordinates: 22° 02′ 47.9 S′ and 055° 08′ 14.3′ W). The samples were cleaned, dried in a convection oven at 45°C, and ground using a Croton knife mill. An exsiccated sample was deposited in the Herbarium of the Federal University of Grande Dourados, Mato Grosso do Sul, Brazil, with registration number 4108.
Extracts were prepared from the powdered material using an accelerated solvent extractor (ASE®-150, Dionex), as described by Espindola et al. (2016 (link)). The samples were placed in a cell of 100 mL and extracted with distilled water at temperature of 125°C through two 5 min static cycles, with an 80% flush volume and a 60 s purge. The extracts were lyophilized to obtain the dry extract. Thus, the aqueous extracts of Campomanesia leaves (AECL) and roots (AECR) were obtained with a yield of 13 and 6%, respectively.
4
Polyphenol Extraction from Carménère Pomace
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Approximately 5 g dw Carménère pomace was mixed with 110 g quartz sand. The mixture was then placed in an HPLE device (ASE 150, Dionex, Sunnyvale, CA, USA), which was used to obtain the polyphenol extracts from the Carménère pomace using pure water, water-glycerol (15%), and water-ethanol (15%) mixtures at 90, 120, and 150 °C. Both the temperature and co-solvent levels were defined based on previous research [21 (link),22 (link)]. The extraction conditions were 10 MPa, one extraction cycle, 150% washing volume, 250 s nitrogen purge time, and 5 min static extraction time to obtain a matrix/extractant ratio of 1:10. The collected extracts were transferred to amber vials and stored at −20 °C until the chemical analysis.
5
Carménère Pomace Extraction Optimization
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This process was developed according to the methodology of Mariotti-Celis et al. [35 (link)] with some modifications. Carménère pomace samples of 5 g (dry weight) were extracted at 90, 120 and 150 °C using different amounts of ethanol (15%, 32.5% and 50%) as co-solvents in an accelerated solvent extraction device (ASE 150, Dionex) applying pressurized nitrogen (~10.2 atm). Raw extracts were frozen (−20 °C) in amber vials until the chemical analysis.
6
Pressurized Liquid Extraction of Marine Sponge
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The lyophilized samples were extracted using the following pressurized liquid extraction process. PLE experiments were performed using an accelerated solvent extractor system (ASE 150, Dionex Corporation, Sunnyvale, CA, USA). The following solvents were used: methylene chloride, ethanol, and methanol (Sigma-Aldrich, Saint-Quentin Fallavier, France).
A mixture of 8 g of freeze-dried powder of sponge and 8 g of sand of Fontainebleau was poured into a 34 mL stainless steel extraction cell, fitted with glass fiber filters at its ends. The extraction was performed with a mixture of CH2Cl2/MeOH (50/50) at 45 °C under 100 bar during 5 static cycles of 5 min. A second extraction was performed with the same parameters after the cell was turned upside down, rinsed with solvents, and flushed with nitrogen. The combined organic extracts were filtered on glass wool before being concentrated under reduced pressure. The dry extract was desalted using absolute EtOH via resuspension, centrifugation, and collection of the supernatant, 3 times successively. The combined supernatants were concentrated under reduced pressure to provide the dry crude extract which was finally stored at 4 °C, prior to analysis and bioassay.
A mixture of 8 g of freeze-dried powder of sponge and 8 g of sand of Fontainebleau was poured into a 34 mL stainless steel extraction cell, fitted with glass fiber filters at its ends. The extraction was performed with a mixture of CH2Cl2/MeOH (50/50) at 45 °C under 100 bar during 5 static cycles of 5 min. A second extraction was performed with the same parameters after the cell was turned upside down, rinsed with solvents, and flushed with nitrogen. The combined organic extracts were filtered on glass wool before being concentrated under reduced pressure. The dry extract was desalted using absolute EtOH via resuspension, centrifugation, and collection of the supernatant, 3 times successively. The combined supernatants were concentrated under reduced pressure to provide the dry crude extract which was finally stored at 4 °C, prior to analysis and bioassay.
7
Extraction of Campomanesia adamantium Roots
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Campomanesia adamantium O. Berg roots were collected in Dourados, MS, under coordinates S 22°02′47.9′′ W 055°08′14.3′′. They were sanitized, dried in an oven with air circulation at 45°C, and ground in a Willy-type knife mill. A voucher specimen was deposited in the herbarium DDMS/UFGD number 4108.
The extract was prepared by repeat extractions of the pulverized material using accelerated solvent extractor (ASE® 150-Dionex). The samples were placed in a cell of 100 mL and extracted with distilled water at a temperature of 125°C in static two cycles of 5 min each time, with 80% of the volume of washing and 60-second purge. The extracts were combined in an aqueous medium and then lyophilized to obtain the dry extract, yield 6%.
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Campomanesia adamantium O. Berg roots were collected in Dourados, MS, under coordinates S 22°02′47.9′′ W 055°08′14.3′′. They were sanitized, dried in an oven with air circulation at 45°C, and ground in a Willy-type knife mill. A voucher specimen was deposited in the herbarium DDMS/UFGD number 4108.
The extract was prepared by repeat extractions of the pulverized material using accelerated solvent extractor (ASE® 150-Dionex). The samples were placed in a cell of 100 mL and extracted with distilled water at a temperature of 125°C in static two cycles of 5 min each time, with 80% of the volume of washing and 60-second purge. The extracts were combined in an aqueous medium and then lyophilized to obtain the dry extract, yield 6%.
8
Comprehensive Cannabis Extraction Protocols
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The hexane extract (HExt) was obtained from 0.6 g of the inflorescences using a model ASE-150 (Dionex) accelerated solvent extraction system with a 5 mL capacity cell using a hexane solvent at 130°C for a static extraction time of 4 minutes across 5 cycles with a 150% rinse. The ethanolic extract (EExt, 70% ethanol) was prepared using the same parameters sequentially from the same sample. The HExt was partitioned into a separatory funnel with hexane and 70% ethanol to obtain two phases: a hexane phase (HExt-HP) and ethanolic phase (HExt-EP). The trichome extract (TExt) was obtained using the method described by Schorr et al. [12 (link)]. The infusion extraction (IExt) involved pouring boiling water over the drug plant in a proportion of 2% for five minutes and then lyophilizing. All chemicals were analytical grade purchased from Vetec, Rio de Janeiro, Brazil.
9
Optimized Extraction and Fractionation of Plant Bioactives
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The dried leaves (430 g) were pulverized and percolated (ethanol:water 7:3) at 20
drops/min for 96 h. The percolate was concentrated to obtain 190.06 g (44.2% yield)
of the crude extract.
The dried roots (31 g) were extracted using a pressurized fluid extractor (ASE 150,
Dionex) using ethanol:H2O (7:3) as the extraction solvent. The program
consisted of 5 min of static time, a temperature of 100 °C, a washing volume of 60%
and a purging time of 100 s in two cycles on the 100 mL extraction cell. The extract
was concentrated to obtain 7.21 g (yield 23.25%) of the crude extract.
The crude extracts from the leaves and roots were fractionated using the ASE
extractor. The plant extract was adsorbed on 21 g of silica gel (70-230 mesh, Sigma,
St. Louis, MO, USA), and a chromatographic column was prepared on the 100-mL
extraction cell, with silica gel (22 g) in the bottom half and the adsorbed extract
in the upper half. The solvent gradient used was hexane, chloroform, ethyl acetate,
ethanol and ethanol:H2O (7:3). In the fractionation process, a 5-min
static program was used, with a temperature of 100 °C, a wash volume of 60% and a
purge time of 100 s in two cycles. The fractions were concentrated and the yields
calculated (Table 1 ).
drops/min for 96 h. The percolate was concentrated to obtain 190.06 g (44.2% yield)
of the crude extract.
The dried roots (31 g) were extracted using a pressurized fluid extractor (ASE 150,
Dionex) using ethanol:H2O (7:3) as the extraction solvent. The program
consisted of 5 min of static time, a temperature of 100 °C, a washing volume of 60%
and a purging time of 100 s in two cycles on the 100 mL extraction cell. The extract
was concentrated to obtain 7.21 g (yield 23.25%) of the crude extract.
The crude extracts from the leaves and roots were fractionated using the ASE
extractor. The plant extract was adsorbed on 21 g of silica gel (70-230 mesh, Sigma,
St. Louis, MO, USA), and a chromatographic column was prepared on the 100-mL
extraction cell, with silica gel (22 g) in the bottom half and the adsorbed extract
in the upper half. The solvent gradient used was hexane, chloroform, ethyl acetate,
ethanol and ethanol:H2O (7:3). In the fractionation process, a 5-min
static program was used, with a temperature of 100 °C, a wash volume of 60% and a
purge time of 100 s in two cycles. The fractions were concentrated and the yields
calculated (
10
Accelerated Solvent Extraction of Malt Rootlets
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PLE was carried out using an accelerated solvent extractor system (ASE 150, Dionex, Sunnyvale, CA, USA). Sample was prepared by mixing 1.5 g of milled malt rootlets and 9 g of sand (used as dispersive agent) which was displayed in a stainless-steel extraction cell (10 mL). A cellulose filter (2.5 cm diameter, Whatman) was fixed at the cell bottom to avoid particles filtration. Initial equipment conditioning involved preheating at 1500 psi for 6 min followed by 100 s of nitrogen purge. Solvents were previously degassed in an ultrasonic bath for 30 min. Optimization of extraction conditions (extraction time, percentage of EtOH, and extraction temperature) was performed by a Box-Behnken incomplete factorial experimental design using the protein content as response variable and fitting the data to a quadratic equation similar to the previously shown for the optimization of UAE variables. As previously, the fitting of the regression model was assessed by ANOVA and the determination of R2.
All extracts were evaporated in a centrifugal concentrator (Eppendorf AG, Hamburg, Germany) and stored at −20 °C until use. Before use, solid samples were solubilized in a 5 mM phosphate buffer (pH 8).
All extracts were evaporated in a centrifugal concentrator (Eppendorf AG, Hamburg, Germany) and stored at −20 °C until use. Before use, solid samples were solubilized in a 5 mM phosphate buffer (pH 8).
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