For NMR observations, 30 mg of each powdered sample was extracted with 1000 mL of deuterated methanol (99.8%, Cambridge Isotope Laboratories Inc., MA, USA) with 1 mM sodium 2,2-dimethyl-2-silapentane-5-sulfonate (DSS) internal standard at 55 °C for 15 min. After centrifugation at 25 °C for 5 min, the extracted supernatant was transferred to a 5 mm NMR tube. Two dimensional J-resolved (2DJ) spectra were acquired at 298 K using a Bruker AVANCE II 700 spectrometer equipped with a 1H inverse triple-resonance cryogenically cooled probe with Z-axis gradients (Bruker BioSpin GmbH, Rheinstetten, Germany).
Deuterated methanol
Manufactured by Cambridge Isotopes
Sourced in United States
Deuterated methanol is a stable isotope of methanol where the hydrogen atoms have been replaced with deuterium. It is a clear, colorless liquid with a characteristic alcoholic odor. Deuterated methanol is commonly used as a solvent and labeled compound in various analytical and research applications.
Automatically generated - may contain errors
Lab products found in correlation
2 2 diphenyl 1 picrylhydrazyl (dpph), by Merck Group (3 mentions)
Rutin, by Merck Group (3 mentions)
Gallic acid, by Merck Group (3 mentions)
Sephadex lh 20, by Merck Group (2 mentions)
Avance 3 400 mhz, by Bruker (2 mentions)
Sodium hydroxide (naoh), by Merck Group (2 mentions)
Sodium nitrite, by Merck Group (2 mentions)
2 2 azinobis 3 ethylbenzothiazoline 6 sulfonic acid (abts), by Merck Group (2 mentions)
Si 60 f254, by Merck Group (2 mentions)
Folin ciocalteu, by Merck Group (2 mentions)
Polyamide 6, by Merck Group (2 mentions)
Chloroform, by Cambridge Isotopes (2 mentions)
Ascorbic acid, by Merck Group (2 mentions)
Formic acid, by Merck Group (2 mentions)
Deuterium oxide, by Cambridge Isotopes (2 mentions)
Z axis gradient, by Bruker (1 mentions)
Avance 2 700 spectrometer, by Bruker (1 mentions)
Catechin, by Merck Group (1 mentions)
Hydrochloric acid (hcl), by Merck Group (1 mentions)
Sodium carbonate, by Merck Group (1 mentions)
14 protocols using deuterated methanol
1
NMR Metabolite Extraction Protocol
2
Chromatographic Analysis of Natural Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Silica gel 60 (particle size 0.063–0.2 mm, 70–230 mesh) (Fluka, St. Louis, MO, USA), Polyamide-6 and Sephadex LH-20 (Sigma-Aldrich, Taufkirchen, Germany) were utilized for column chromatography. TLC plates (Si 60 F254, Merck, Darmstadt, Germany) and analytical-grade solvents were used in the study. Visualization of the spots was carried out using p-anisaldehyde spray reagent [37 ].
The UV investigation was carried out in methanol utilizing a Shimadzu UV1, 601PC UV–visible scanning spectrophotometer (Shimadzu Corp., Tokyo, Japan). Optical rotation was measured using a 341 Perkin Elmer polarimeter (Darmstadt, Germany). HRESIMS was executed on Agilent LC/Q-TOF, 6530 (Santa Clara, CA, USA). All 1D and 2D NMR spectra were recorded on a Bruker Avance III 400 MHz (Bruker AG, Fällanden, Switzerland) and analysed using Topspin 3.1 software (Bruker AG, Fällanden, Switzerland). Deuterated methanol and chloroform (Cambridge Isotopes, Andover, MA, USA) were used.
Aluminium trichloride (AlCl3.6H2O), anhydrous sodium carbonate (Na2CO3), ascorbic acid, DPPH, ABTS (Sigma, PN: A3219, St. Louis, MO, USA), Folin–Ciocalteu, gallic acid, rutin, sodium hydroxide (NaOH), and sodium nitrite (NaNO2) were purchased from Merck (Rahway, NJ, USA) and Sigma-Aldrich (St. Louis, MO, USA).
The UV investigation was carried out in methanol utilizing a Shimadzu UV1, 601PC UV–visible scanning spectrophotometer (Shimadzu Corp., Tokyo, Japan). Optical rotation was measured using a 341 Perkin Elmer polarimeter (Darmstadt, Germany). HRESIMS was executed on Agilent LC/Q-TOF, 6530 (Santa Clara, CA, USA). All 1D and 2D NMR spectra were recorded on a Bruker Avance III 400 MHz (Bruker AG, Fällanden, Switzerland) and analysed using Topspin 3.1 software (Bruker AG, Fällanden, Switzerland). Deuterated methanol and chloroform (Cambridge Isotopes, Andover, MA, USA) were used.
Aluminium trichloride (AlCl3.6H2O), anhydrous sodium carbonate (Na2CO3), ascorbic acid, DPPH, ABTS (Sigma, PN: A3219, St. Louis, MO, USA), Folin–Ciocalteu, gallic acid, rutin, sodium hydroxide (NaOH), and sodium nitrite (NaNO2) were purchased from Merck (Rahway, NJ, USA) and Sigma-Aldrich (St. Louis, MO, USA).
3
Characterization of Deuterated Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Deuterated Methanol (99.8 atom % deuterium) and deuterium oxide (99.9 atom % deuterium) were obtained from Cambridge Isotope Laboratories, Inc. (Andover, MA, USA). 3-(trimethylsilyl)propionic-2,2,3,3-d4 acid (TSP), Folin-Ciocalteu’s phenol reagent, sodium carbonate, diethylene glycol, gallic acid, rutin, catechin, 2,2-diphenyl-1-picrylhydrazyl (DPPH), L-ascorbic acid, formic acid and hydrochloric acid were obtained from Sigma-Aldrich (St. Louis, MO, USA), and sodium hydroxide was purchased from Junsei Chemical (Tokyo, Japan). Methanol, water, and acetonitrile were of the highest commercial grade and obtained from Honeywell (St. Muskegon, MI, USA). All chemicals were of analytical grade.
4
Solvent Procurement for Chemical Analysis
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
All solvents were purchased from Merck KGaA, Fisher Scientific Ltd. and VWR International LLC, except of deuterated methanol which was purchased from Cambridge Isotope Laboratories Inc.
5
Synthesis of DDMAT-DMAC Copolymer
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
2-(Dodecylthiocarbonothioylthio)-2-methylpropionic
acid (DDMAT), N,N-dimethylacrylamide (DMAC), and 2,2′-azobis(2-methylpropionitrile)
(AIBN) were purchased from Sigma-Aldrich and used as received. Diacetone
acrylamide (DAAM), adipic acid dihydrazide (ADH), and 4,4′-azobis(4-cyanovaleric
acid) (ACVA) were purchased from Alfa Aesar and were used as received.
Deuterated methanol was purchased from Cambridge Isotope Laboratories.
Dioxane was purchased from Sigma-Aldrich UK, and diethyl ether was
purchased from Fisher Scientific. All solvents were HPLC grade.
acid (DDMAT), N,N-dimethylacrylamide (DMAC), and 2,2′-azobis(2-methylpropionitrile)
(AIBN) were purchased from Sigma-Aldrich and used as received. Diacetone
acrylamide (DAAM), adipic acid dihydrazide (ADH), and 4,4′-azobis(4-cyanovaleric
acid) (ACVA) were purchased from Alfa Aesar and were used as received.
Deuterated methanol was purchased from Cambridge Isotope Laboratories.
Dioxane was purchased from Sigma-Aldrich UK, and diethyl ether was
purchased from Fisher Scientific. All solvents were HPLC grade.
6
Chromatographic Analysis of Natural Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Silica gel 60 (particle size 0.063–0.2 mm, 70–230 mesh) (Fluka, St. Louis, MO, USA), Polyamide-6 and Sephadex LH-20 (Sigma-Aldrich, Taufkirchen, Germany) were utilized for column chromatography. TLC plates (Si 60 F254, Merck, Darmstadt, Germany) and analytical-grade solvents were used in the study. Visualization of the spots was carried out using p-anisaldehyde spray reagent [37 ].
The UV investigation was carried out in methanol utilizing a Shimadzu UV1, 601PC UV–visible scanning spectrophotometer (Shimadzu Corp., Tokyo, Japan). Optical rotation was measured using a 341 Perkin Elmer polarimeter (Darmstadt, Germany). HRESIMS was executed on Agilent LC/Q-TOF, 6530 (Santa Clara, CA, USA). All 1D and 2D NMR spectra were recorded on a Bruker Avance III 400 MHz (Bruker AG, Fällanden, Switzerland) and analysed using Topspin 3.1 software (Bruker AG, Fällanden, Switzerland). Deuterated methanol and chloroform (Cambridge Isotopes, Andover, MA, USA) were used.
Aluminium trichloride (AlCl3.6H2O), anhydrous sodium carbonate (Na2CO3), ascorbic acid, DPPH, ABTS (Sigma, PN: A3219, St. Louis, MO, USA), Folin–Ciocalteu, gallic acid, rutin, sodium hydroxide (NaOH), and sodium nitrite (NaNO2) were purchased from Merck (Rahway, NJ, USA) and Sigma-Aldrich (St. Louis, MO, USA).
The UV investigation was carried out in methanol utilizing a Shimadzu UV1, 601PC UV–visible scanning spectrophotometer (Shimadzu Corp., Tokyo, Japan). Optical rotation was measured using a 341 Perkin Elmer polarimeter (Darmstadt, Germany). HRESIMS was executed on Agilent LC/Q-TOF, 6530 (Santa Clara, CA, USA). All 1D and 2D NMR spectra were recorded on a Bruker Avance III 400 MHz (Bruker AG, Fällanden, Switzerland) and analysed using Topspin 3.1 software (Bruker AG, Fällanden, Switzerland). Deuterated methanol and chloroform (Cambridge Isotopes, Andover, MA, USA) were used.
Aluminium trichloride (AlCl3.6H2O), anhydrous sodium carbonate (Na2CO3), ascorbic acid, DPPH, ABTS (Sigma, PN: A3219, St. Louis, MO, USA), Folin–Ciocalteu, gallic acid, rutin, sodium hydroxide (NaOH), and sodium nitrite (NaNO2) were purchased from Merck (Rahway, NJ, USA) and Sigma-Aldrich (St. Louis, MO, USA).
7
Oxidation and Cyclization of Levoglucosenone
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Levoglucosenone was graciously provided by the Circa Group. Potassium carbonate 99% (Acros), hydrogen peroxide 30% (Fischer), diethyl succinate 98% (Alpha Aesar), malonyl chloride 97% (Sigma Aldrich), succinyl chloride 95% (Sigma Aldrich), adipoyl chloride 98% (Sigma Aldrich), glutaryl chloride 97% (Sigma Aldrich), terephthaloyl chloride >99% flakes (Sigma Aldrich) were used without further purification unless mentioned. NMR solvents including deuterated chloroform, deuterated methanol, and deuterated dimethyl sulfoxide were purchased from Cambridge Isotopes Laboratories.
8
Pharmaceutical Compound Procurement Protocol
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Griseofulvin was purchased from Alfa Aesar, UK and propofol from Sigma Aldrich, UK. DOX was purchased from LC Laboratories (Woburn, USA). Deuterated methanol was purchased from Cambridge Isotope Laboratories Inc., USA. All other chemicals were purchased from Sigma Aldrich, UK and reagents from Fisher Scientific, UK. Dialysis tubing was purchased from Medicell International Ltd, UK. Syringe filters were purchased from Whatman, UK.
9
Saponin Compound Analysis Protocol
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Deuterated methanol containing 0.03% v/v tetramethylsilane (TMS) (CD3OD, 99.8% D) was purchased from Cambridge Isotope Laboratories, Inc. (Tewksbury, Massachusetts, USA); dimethyl terephthalate (DMT, Lot No. BCBF6171V) was purchased from Sigma-Aldrich (Darmstadt, Germany); standard substances Ginsenoside Rb1 (Lot No. 200725), Ginsenoside Rg1 (Lot No. 200709), Ginsenoside Re (Lot No. 200603), Panaxoside R1 (Lot No. 190813), Panaxoside Fe (Lot No. 190803), Gynostemma saponin XLIX (Lot No. 210826), Gynostemma saponin XVII (Lot No. 210903), and Gynostemma saponin XLVI (Lot No. 210730) were purchased from Shanghai Winherb Medical Technology Co., Ltd. (Shanghai, China); Shenmai Injection was provided by Chiatai Qingchunbao Pharmaceutical Co., Ltd. (China); Xuesaitong Injection was provided by Heilongjiang ZBD Pharmaceutical Group Co., Ltd. (Hangzhou, China); and gynostemma column chromatography eluting intermediate was provided by Wanbangde Pharmaceutical Group Co., Ltd. (Taizhou, China).
10
NMR analysis of HPLC-MS extract
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
The MeOH extracts remaining after HPLC-MS analysis was dried using a vacuum-centrifuge and dissolved in a mixture of deuterium oxide (D2O, D 99.8%, 250 μl) and deuterated methanol (CD3OD, D 99.8%, 750 μl) (Cambridge Isotope Laboratories, Andover, MA, USA). A 700 µl aliquot of the particulate-free extract was transferred into a 5 mm Norell 509-UP-7 NMR tube (Norell Inc., Landisville, NJ, USA) and analysed immediately by 1H NMR.
1H NMR spectra were recorded on a Bruker Avance 600 MHz NMR spectrometer with TXI 5 mm probe and quantification performed using the ERETIC method (Tapiolas et al., 2013 (link)). This technique generates an internal electronic reference signal, calibrated using stock solutions of DMSP.
1H NMR spectra were recorded on a Bruker Avance 600 MHz NMR spectrometer with TXI 5 mm probe and quantification performed using the ERETIC method (Tapiolas et al., 2013 (link)). This technique generates an internal electronic reference signal, calibrated using stock solutions of DMSP.
About PubCompare
Our mission is to provide scientists with the largest repository of trustworthy protocols and intelligent analytical tools, thereby offering them extensive information to design robust protocols aimed at minimizing the risk of failures.
We believe that the most crucial aspect is to grant scientists access to a wide range of reliable sources and new useful tools that surpass human capabilities.
However, we trust in allowing scientists to determine how to construct their own protocols based on this information, as they are the experts in their field.
Ready to get started?
Sign up for free.
Registration takes 20 seconds.
Available from any computer
No download required
Revolutionizing how scientists
search and build protocols!