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15 protocols using chromasolv

1

Chemical Reagents for Analytical Procedures

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The following chemical reagents were used in this work: acetonitrile (LC-MS grade; Chromasolv, Honeywell International Inc., Charlotte, NC, USA), ammonium hydroxide (LC-MS grade; Fluka, Honeywell International Inc., Charlotte, NC, USA), N,N-dimethylformamide (DMF; Sigma-Aldrich, Merck KGaA, Darmstadt, Germany), formic acid (LC-MS grade; Optima, Fisher Chemical, Thermo Fisher Scientific Inc., Waltham, MA, USA), 2-propanol (LC-MS grade; Chromasolv, Honeywell International Inc., Charlotte, NC, USA), methanol (LC-MS grade; Chromasolv, Honeywell International Inc., Charlotte, NC, USA), PAN (Aldrich, Merck KGaA, Darmstadt, Germany), and water (LC-MS grade; LiChrosolv, Merck KGaA, Darmstadt, Germany).
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2

NMR Spectroscopy of CRAM Proxy Compounds

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NMR spectra for analogues 916 were acquired at 298 K at 600 MHz on a Bruker Avance Neo
spectrometer
with a TCI (CRPHe TR-1H &19F/13C/15N 5 mm-EZ) probe. The samples were dissolved in 0.1
N NaOD in D2O prepared by adding 23 mg of Na (>99.8%
sodium
basis, Sigma-Aldrich, Merck) to 10 mL of D2O (deuteration
degree min 99.9%, MagniSolv, Sigma-Aldrich, Merck) and chemical shifts
referenced to the residual solvent peak at 4.79 ppm in the 1H NMR spectrum, and approximately 5 μL of methanol (min 99.9%,
Chromasolv, Honeywell) was added for referencing purposes in 13C NMR experiments. 13C NMR spectra were recorded
in 0.1 N NaOD in D2O prepared by adding 23 mg of Na (>99.8%
sodium basis, Sigma-Aldrich, Merck) to 10 mL of D2O (deuteration
degree min 99.9%, MagniSolv, Sigma-Aldrich, Merck), and approximately
5 μL of methanol (min 99.9%, Chromasolv, Honeywell) was added,
so that the samples could be referenced to the residual methanol solvent
peak at 49.50 ppm. 1H NMR, 13C NMR, COSY, HSQC,
and HMBC spectra for CRAM proxies 916 are provided in Figures S6–S53.
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3

Targeted LC-MS/MS Analysis of Bioactive Compounds

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All samples were analysed on a Shimadzu LCMS-8060 triple quadrupole system. Samples (8 µL injection volume) were separated on an Agilent InfinityLab Poroshell 120 EC-C18 column (3 × 100 mm, 2.7 µm) with a matching Agilent InfinityLab Poroshell 120 EC-C18 guard column (3 × 5 mm, 2.7 µm), using gradient elution in reversed-phase mode. Column oven temperature was set at 25.0 °C. Phase A consisted of LC-MS grade water (LiChrosolv®, Merck) with 0.1% formic acid (Optima™ LC/MS, Fisher Chemical), and phase B consisted of LC-MS grade acetonitrile (CHROMASOLV™, Honeywell) with 0.1% formic acid (Optima™ LC/MS, Fisher Chemical). Gradient starting conditions were 10% phase B (maintained for 0.5 min), followed by a linear increase of phase B concentration to 100% (for 25.5 min), hold at 100% phase B (for 3 min) and column re-equilibration with 10% phase B (6 min).
Total running time was 35 min per sample. The total flow rate was 300 µL min -1 . Investigated analytes and their respective monitored m/z ratios are listed in Table A2 in ESI A. †
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4

Analytical Standards of Pesticides and Herbicides

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Analytical standards of monuron, diuron, alachlor, acetochlor, 3-(3-chlorophenyl)-1,1-dimethylurea, desethyl-sebuthylazine, desethyl-terbuthylazine, 3-(2,3-dichlorophenyl)-1,1-dimethylurea, 3-(2,4-dichlorophenyl)-1,1-dimethylurea, 3-(2,5-dichlorophenyl)-1,1-dimethylurea, 3-(2,6-dichlorophenyl)-1,1-dimethylurea, and 3-(3,5-dichlorophenyl)-1,1-dimethylurea as well as a standard mixture containing sebuthylazine and terbuthylazine were obtained from Sigma-Aldrich and were of analytical grade or higher.
For the CCS calibration nicotinate, adenine, acetaminophen, pyridoxine, caffeine, atrazine, metolachlor, sulfadimethoxine, and ampicillin were used. The calibrants were all purchased from Sigma-Aldrich and were of analytical grade.
Acetonitrile (CHROMASOLV™ for HPLC, gradient grade,  ≥ 99.9%) and water (Honeywell Riedel-de Haën™, Seelze, Germany) with 0.1% of formic acid (reagent grade, 98–100% from Scharlau, Barcelona, Spain) were used as mobile phase for LC/IMS/HRMS analysis.
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5

Anticancer Drug Compound Preparation

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Formic acid was purchased from Fisher Chemical (Loughborough, UK). Methanol, acetonitrile, deionized water, and LC-MS CHROMASOLV were obtained from Honeywell (Wunstorfer Strasse, Seelze, Germany). U87 and U373 cells were purchased from the Radiobiology and Experimental Radio Oncology Lab, University Cancer Center Hamburg, Hamburg, Germany. Etoposide was purchased from Sigma-Aldrich (St. Louis, MO, USA). Paclitaxel was purchased from Merck (Darmstadt, Germany). Fetal bovine serum, penicillin, and streptomycin were purchased from Sigma Aldrich (St. Louis, MO, USA).
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6

Analytical Standards for Pesticide Quantification

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Analytical standards of thiacloprid (C17451000) and flupyradifurone (37,050) were obtained from Dr. Ehrenstorfer (Dr. Ehrenstorfer GmbH, Augsburg, Germany) and Sigma-Aldrich (Sigma-Aldrich Chemie GmbH, Taufkirchen, Germany), respectively. Acetonitrile (ACN), CHROMASOLV™ for high liquid pressure chromatography (HPLC) with gradient grade (34851, Honeywell Riedel-de Haën™, Seelze, Germany) and bidest. ultra-pure water from a Milli-Q system (Merck KGaA, Darmstadt, Germany) were used for sample preparation as well as for LC–MS analysis. Formic acid puriss. (27,001) was purchased from Honeywell (Honeywell Riedel-de Haën™, Seelze, Germany) and sodium chloride, (≥99%, Ph. Eur., USP P029.3) was bought from Carl Roth (Carl Roth GmbH + Co. KG, Karlsruhe, Germany). Anhydrous magnesium sulfate (M7506) was also obtained from Sigma-Aldrich (Sigma-Aldrich Chemie GmbH, Taufkirchen, Germany). The used solid phase extraction (SPE) material and the grinding media were obtained in a dispersive 2 mL (universal kit 5982-0028CH, Agilent Technologies Sales & Services GmbH & Co. KG, Waldbronn, Germany).
Note: Availability of standard laboratory and chromatographically equipment is assumed.
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7

Organic Micropollutant Sample Prep

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For the sample preparation of organic micropollutants, three solvents—dichloromethane (≥99.8%, Ultra Resi—analyzed®, J.T. Baker (Mallinckrodt Baker, Inc, Phillipsburg, NJ, USA)), n-hexane (95.0%, Ultra Resi—analyzed®, J.T. Baker (Mallinckrodt Baker, Inc, Phillipsburg, NJ, USA)) and methanol (≥99.8%, for HPLC, Chromasolv®, (Honeywell, Charlotte, NC, USA)) were used.
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8

Lignin Content Analysis by UV-Vis

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100 μL of each sample was diluted 1 : 10 in 50% methanol : water (Honeywell, Chromasolv™) and analysed spectrophotometrically at 280 nm in a 96-well UVStar® plate (Greiner Bio-One) and compared to a standard curve of Sigma Kraft Lignin (Sigma Aldrich, 471003), Fig. S1, to determine the overall aromatic content. Concentrated samples were filtered using a 0.2 μm PTFE filter (VWR) and diluted in 50% methanol : water to obtain a final concentration of 150–175 μg mL−1 lignin.
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9

Organic Field-Effect Transistor Fabrication

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Imidazole >98% and 1,4,5,8-naphthalenetetracarboxylic dianhydride (>95%) were purchased from TCI Europe N.V. Toluene, hydrochloric acid, 96% ethanol, and methanol were obtained from Avantor Performance Materials Poland. Chloroform-D (CDCl3), n-aliphatic amines, n-heptane, Toluene (CHROMASOLV® (Honeywell, Charlotte, NC, USA), for HPLC, 99.9%), 1,2-dichlorobenzene (for HPLC, 99%), and chloroform (CHROMASOLV®Plus, (Honeywell, Charlotte, NC, USA), for HPLC, >99.9%) were supplied by Sigma-Aldrich, Darmstadt, Germany. All reagents and solvents were used as received. The OFETs were prepared using silicon substrates with 230 nm silicon dioxide gate dielectric with prepatterned Au/ITO (20 nm/10 nm) electrodes (Fraunhofer Gen. 4 OFET substrates (Fraunhofer IPMS, Dresden, Germany)). The OFET channel width (W) and the length were 10 mm and 10 μm, respectively.
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10

Analytical Reagents for Spectroscopic Assays

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Analytical reagent-grade chemicals and bi-distilled water were used throughout this experiment. Methanol used was of HPLC-grade, ≥99.9%, CHROMASOLV™ (Honeywell Riedel-de Haën™); KNO3, acetone (Multisolvent® HPLC grade), NaOH, and H2SO4 were purchased from Merck KGaA, Darmstadt, Germany. Methyl viologen, oxalic acid anhydrous 99%, salicylic acid acs 99%, sodium carbonate (Na2CO3), glucose solution, anthrone 97%, l-ascorbic acid, Folin–Ciocâlteu reagent, DPPH radical reagent, Trolox, and gallic acid were purchased from Merck KGaA, Darmstadt, Germany. Standard solutions were prepared with bi-distilled water.
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