Total and extractable contents of metal elements in soil and plant samples were determined using microwave digestion and diethylenetriamine pentaacetate (DTPA) extraction, respectively. Total (strong acid-extractable) Cd and Zn in soil before and after planting was estimated by digesting approximately 1 g of air-dried soil with 4.5 ml of 37% hydrochloric acid (HCl), 1.5 ml of 65% nitric acid, and 1 ml of 30% H 2 O 2 in a microwave digestion system (Milestone ETHOS One, USA). A similar procedure was employed to digest plant materials, but without HCl addition. The amount of DTPA-extractable Cd and Zn in soil was determined using 0.005M DTPA+0.01 M CaCl 2 +0.1M triethanolamine, pH 7.30 at a soil-to-solution ratio (w/v) of 1:2. The metal concentrations in both the digests and extracts were quanti ed using an atomic absorption spectrophotometer (Perkin Elmer AAnalyst 200).
Ethos one
Manufactured by Milestone
Sourced in Italy, United States
The Ethos One is a compact and versatile laboratory equipment designed for a range of applications. It features a microwave power of 1800 watts and a frequency of 2.45 GHz. The equipment is equipped with a rotating carousel and a temperature control system.
Automatically generated - may contain errors
Lab products found in correlation
6530 infinity q tof detector, by Agilent Technologies (2 mentions)
Suprapur, by Merck Group (2 mentions)
Direct q 3 uv, by Merck Group (2 mentions)
Aanalyst 200, by PerkinElmer (1 mentions)
Vista pro, by Agilent Technologies (1 mentions)
Triplus rsh, by Thermo Fisher Scientific (1 mentions)
Methanol, by Merck Group (1 mentions)
Methylene chloride, by Merck Group (1 mentions)
Trace 1310, by Thermo Fisher Scientific (1 mentions)
M xylene, by Merck Group (1 mentions)
Dvb car pdms, by Merck Group (1 mentions)
Isq qd, by Thermo Fisher Scientific (1 mentions)
Quadrupole time of flight tandem, by Agilent Technologies (1 mentions)
Optima 8000, by PerkinElmer (1 mentions)
Tecator cyclotec 1093, by Foss (1 mentions)
Fp 528, by Leco (1 mentions)
Cryodos 50, by Telstar (1 mentions)
Activa m, by Horiba (1 mentions)
Traceselect, by Merck Group (1 mentions)
Aas 5 fl, by Zeiss (1 mentions)
32 protocols using ethos one
1
Quantifying Metal Elements in Soil and Plants
2
Elemental Analysis of Tissue Samples
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Flame atomic absorption spectrophotometer (ZEISS, AAS5, and Germany) was used to measure the contents of copper and silver in muscle and some edible organs such as heart, liver, and spleen tissue homogenate [19 (link)]. Briefly, concentrated nitric acid and 30% H2O2 were added to 0.5 g tissue samples and kept overnight, then heated in a microwave digestion system (ETHOS One; Milestone, Sorisole, Italy) till it became completely digested and colorless. Afterward, the samples were allowed to cool, and the remaining solutions were diluted with 2% nitric acid.
3
Gadolinium Tracing in Rat Brain
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The animals were euthanized by an overdose of sodium pentobarbital anesthesia at the end of the clearance period. The heart was exposed, and cardiac perfusion with 0.9% saline solution was performed to remove excess blood from the brain. The whole brain was carefully isolated and was quickly dissected using the rat brain matrix (DSN-2; Institute of Materia Medica, China). The samples of the DCN, cerebellum, pons, olfactory bulb, frontal cortex, striatum, hippocampus, and thalamus were carefully extracted on ice according to the anatomical atlas of the rat brain [18 ].
The brain samples were weighed and sealed in a quartz tube immersed with 1.5 mL of concentrated nitric acid and were subjected to digestion in a microwave digester for 85 min (ETHOS One; Milestone, Bergamo, Italy). Each sample was then transferred to a polypropylene tube and diluted to 10 mL with ultra-purified water. Subsequently, the accumulation of the 158 Gd isotope in each sample was measured with ICP-MS (7700x; Agilent Technologies, Santa Clara, CA) (with an internal standard of indium 115). A standard curve of inorganic Gd (0.1-50 μg/L) was used to monitor the response of the Gd concentration. The results were expressed in nanomoles (nmol) of Gd per gram of wet tissue weight.
The brain samples were weighed and sealed in a quartz tube immersed with 1.5 mL of concentrated nitric acid and were subjected to digestion in a microwave digester for 85 min (ETHOS One; Milestone, Bergamo, Italy). Each sample was then transferred to a polypropylene tube and diluted to 10 mL with ultra-purified water. Subsequently, the accumulation of the 158 Gd isotope in each sample was measured with ICP-MS (7700x; Agilent Technologies, Santa Clara, CA) (with an internal standard of indium 115). A standard curve of inorganic Gd (0.1-50 μg/L) was used to monitor the response of the Gd concentration. The results were expressed in nanomoles (nmol) of Gd per gram of wet tissue weight.
4
Digestion and Analysis of Plant and Soil Cd and Zn
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Dried plant material was ground to a fine powder with a mortar machine (IKA; A11 Basic, Japan), sieved through a 2-mm nylon mesh sieve, and weighed. Plant tissue and rhizosphere soil (0.5 g each) were digested in a microwave digestion apparatus (ETHOS One; Milestone Inc.). Extractable Cd and Zn were recovered from soil using 0.005 M diethylenetriamine pentaacetic acid (DTPA) adjusted to pH 5.3 with 0.1 M HCl and 0.01 M CaCl 2 . Cadmium and Zn concentrations were determined using FAAS. Plant and soil standard reference materials (NIST SRM ® 1515 apple leaves and NIST SRM ® 2710a Montana soil, respectively) and a blank method were used to evaluate the accuracy and precision of analytical data. Percent recovery for Cd and Zn in plant and soil samples ranged from 90-110%.
5
Quantifying Cadmium in Organ Tissues
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Tissue samples of liver and kidneys (about 50 mg) were digested in Teflon vessels with 1 mL of concentrated nitric acid using a closed microwave digestion system (Ethos One; Milestone, Germany). After decomposition at 180°C for 10 min, Milli-Q water was added to the samples until the volume reached 10 mL. The concentrations of Cd in these samples were determined by ICP-MS (Agilent 7700x Japan). Indium ( 115 In) was used as an internal standard for analyzing 111 Cd. The detection limit of 111 Cd was 0.1 μg/L.
6
Microwave-Assisted Elemental Analysis
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The samples were digested by microwave-assisted digestion using an Ethos One microwave system (Milestone, Chicago, USA), equipped with programmable power control (maximum power 1600 W) and segmented rotor HPR 1000/10 s (operating pressure up to 35 bar maximum; operating temperature 260 °C maximum) with 10 reaction vessels. Measurements were carried out with a Vista Pro (Varian, Australia) optical emission spectrometer with inductively coupled plasma and axial viewing configuration, equipped with a solid-state detector, Sturman-Masters mist chamber, and V-groove nebulizer. Selected emission wavelengths for the analysis were chosen according to previous interference studies (Larrea-Marín, Pomares-Alfonso, Gómez-Juaristi, Sánchez-Muniz, & de la Rocha, 2010). The lines that exhibited low interference, high analytical signal and background ratios were selected.
7
Determination of VOCs in Calypogeia azurea
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The following solvents were used during the research: n-hexane, puriss. p.a., ≥99% (GC), ethyl acetate, puriss. p.a., 99.9% (GC), methanol for GC, Sigma-Aldrich (Steinheim, Germany) and m-xylene, diethyl ether, puriss. ≥99.9% (GC), methylene chloride >99.9%, POCH (Gliwice, Poland). Saturated n-alkanes of C7-C40 standard Supelco (Bellefonte, PA, USA) were used to determine the Kovats retention indices.
Fused silica fibers coated with divinylbenzene/carboxy/polydimethylsiloxane (DVB/CAR/PDMS) (Supelco, Bellefonte, PA, USA) stationary phases were used for the SPME analysis.
Trace 1310 (Thermo Scientific, Waltham, MA, USA) coupled with a mass spectrometer ISQ QD (Thermo Scientific, Waltham, MA, USA) with a 007-5MS column (30 m, 0.25 mm, 0.25 μm) (Quadrex, Woodbridge, CT, USA) were used to analyze the VOC compounds present in the cells of the Calypogeia azurea species.
The TriPlus RSH (Thermo Scientific, Waltham, MA, USA) automatic sample injector was used to ensure that the samples were dispensed with sufficient reproducibility.
HD was carried out using a Deryng apparatus consisting of a 500 mL round-bottom flask, a condenser, and a heating bowl (Lab-szkło, Kraków, Poland), recommended by the VI edition of the Polish Pharmacopoeia of 2002. The Ethos one (Milestone, Sorisole, Italy) was used for MAE.
Fused silica fibers coated with divinylbenzene/carboxy/polydimethylsiloxane (DVB/CAR/PDMS) (Supelco, Bellefonte, PA, USA) stationary phases were used for the SPME analysis.
Trace 1310 (Thermo Scientific, Waltham, MA, USA) coupled with a mass spectrometer ISQ QD (Thermo Scientific, Waltham, MA, USA) with a 007-5MS column (30 m, 0.25 mm, 0.25 μm) (Quadrex, Woodbridge, CT, USA) were used to analyze the VOC compounds present in the cells of the Calypogeia azurea species.
The TriPlus RSH (Thermo Scientific, Waltham, MA, USA) automatic sample injector was used to ensure that the samples were dispensed with sufficient reproducibility.
HD was carried out using a Deryng apparatus consisting of a 500 mL round-bottom flask, a condenser, and a heating bowl (Lab-szkło, Kraków, Poland), recommended by the VI edition of the Polish Pharmacopoeia of 2002. The Ethos one (Milestone, Sorisole, Italy) was used for MAE.
8
Trace Element Analysis of Teeth Samples
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All teeth samples were washed with water and then dried in an oven at 65°C. All the samples weighed between 0.2 g and 0.5 g (according to precise measurement in a Teflon vessel) prior to being digested with 6 mL of concentrated ultrapure nitric acid (65%) and 2 mL of ultrapure hydrogen peroxide (30%). The acid digestion of the teeth samples was performed using a commercial high-pressure laboratory microwave oven (Ethos One; Milestone Srl – Via Fatebenefratelli 1/5, 24010 Sorisole (BG), Italy). For each sample, a one-step microwave program was used, increasing for 15 minutes to 200°C at 1,000 W and maintenance at 200°C and 1,000 W for 10 minutes. Any undissolved material was removed with filtered 25 mm polyethylene syringes.
9
Mineral Analysis of Coprinus comatus
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Coprinus comatus dry powder preparation samples were digested using concentrated HNO3 and H2O2 and Ethos One, Milestone microwave (Sorisole, Italy) with an internal temperature sensor. The operational conditions and the heating programme were carried out according to the manufacturers’ recommendations. Digests were diluted with ultrapure deionized water to 25 ml in a glass flask and transferred to a previously acid-cleaned polypropylene vessel for further analysis. A Varian SpectrAA 10 (Varian Techtron Pty Limited, Mulgrave, Australia) model atomic absorption spectrometer (AAS) with deuterium background correction was used for determination of mineral element (Mg), trace element (Fe, Cu, Zn, Se) and toxic heavy metal (Pb, Cd, Hg, As) contents. The assembly was operated from an interfaced computer running SpectrAA software. The samples were analysed according to the procedures and conditions described in our previous publication [4 (link)]. Coprinus comatus samples were analysed in triplicate (n = 3), and blank samples were included to control for possible contamination.
10
HPLC-MS Analysis of Derivatized Carboxylic Acids
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For the HPLC analysis, ~0.1 mg of each sample was subjected to extraction assisted by microwaves in a microwave oven Ethos One (Milestone, U.S.A.) (power 600 W), with 300 µL of a chloroform-hexane (3:2) mixture at 80 °C for 25 min.
Carboxylic acids were derivatised using 2,2′-dipyridyl disulphide (DPDS) and triphenylphosphine (TPP), and 2-hydrazinoquinoline (HQ) to form hydrazides. For the derivatisation reaction, 20 μL of the extraction solutions were dried under nitrogen flow in the insert of a 2 mL auto-sampler vial, dissolved with 60 µL of acetonitrile to which was added 20 µL of HQ, DPDS, and TPP containing solutions. The sample were heated for 60 °C for 6 hours32 (link). All the analyses were carried out on a 1200 Infinity HPLC coupled by a Jet Stream ESI interface with a Quadrupole-Time of Flight tandem mass spectrometer 6530 Infinity Q-ToF detector (Agilent Technologies, USA). The separation and mass spectrometric experiments were performed according to the conditions reported in21 (link),33 (link)–36 (link). The fatty acid quantification was based on calibration curves reporting the integrated areas of the [M + H]+ ions of the HQ derivatives as detected by the “Find by Formula” algorithm. The interpretation of the acyl glyceride species was performed by comparison with the literature21 (link),33 (link)–37 (link).
Carboxylic acids were derivatised using 2,2′-dipyridyl disulphide (DPDS) and triphenylphosphine (TPP), and 2-hydrazinoquinoline (HQ) to form hydrazides. For the derivatisation reaction, 20 μL of the extraction solutions were dried under nitrogen flow in the insert of a 2 mL auto-sampler vial, dissolved with 60 µL of acetonitrile to which was added 20 µL of HQ, DPDS, and TPP containing solutions. The sample were heated for 60 °C for 6 hours32 (link). All the analyses were carried out on a 1200 Infinity HPLC coupled by a Jet Stream ESI interface with a Quadrupole-Time of Flight tandem mass spectrometer 6530 Infinity Q-ToF detector (Agilent Technologies, USA). The separation and mass spectrometric experiments were performed according to the conditions reported in21 (link),33 (link)–36 (link). The fatty acid quantification was based on calibration curves reporting the integrated areas of the [M + H]+ ions of the HQ derivatives as detected by the “Find by Formula” algorithm. The interpretation of the acyl glyceride species was performed by comparison with the literature21 (link),33 (link)–37 (link).
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