Optical rotations were performed on a JASCO P-1020 polarimeter. IR spectra were measured on a Bruker FT-IR Tensor 27 spectrometer with KBr pellets. UV spectra were obtained on Shimadzu UV-2401A spectrometer. 1D-NMR and 2D-NMR spectra were recorded on an AV-600 MHz or a Bruker DRX-400 MHz spectrometer. Coupling constants were expressed in Hz and chemical shifts were given on a ppm scale with tetramethylsilane as internal standard. HRESIMS were recorded on an API QSTAR Pulsar 1 spectrometer. CD spectra were obtained on a JASCO 810 spectrometer. Column chromatography (CC) was performed on silica gel (200–300 mesh, Qingdao Marine Chemical Ltd., Qingdao, People’s Republic of China), Sephadex LH-20 (Pharmacia Fine Chemical Co., Ltd., Sweden), and MCI-gel CHP 20P (75–100 μm, Mitsubishi Chemical Co., Ltd). Thin-layer chromatography (TLC) was carried out on silica gel H-precoated plates (Qingdao Haiyang Chemical Co., Ltd.) with CHCl3/MeOH (9:1, 4:1, v/v) as developing solvents and spots were visualized by Dragendorff’s reagent. High performance liquid chromatography (HPLC) was performed using waters 600 equipment with semi-preparative and preparative C18 columns (150 × 9.4 and 250 × 21.2 mm, respectively).
Av 600 mhz
Manufactured by Bruker
Sourced in Germany, United States
The AV 600 MHz is a high-performance nuclear magnetic resonance (NMR) spectrometer designed for advanced analytical applications in chemistry and materials science. It operates at a proton frequency of 600 MHz, offering high-resolution analysis of molecular structures and compositions.
Automatically generated - may contain errors
Lab products found in correlation
Silica gel, by Qingdao Marine Chemical (2 mentions)
Sephadex lh 20, by GE Healthcare (2 mentions)
Spd m20a, by Shimadzu (2 mentions)
810 spectrometer, by Jasco (1 mentions)
Uv 2401a spectrometer, by Shimadzu (1 mentions)
Drx 400 mhz spectrometer, by Bruker (1 mentions)
P 1020 polarimeter, by Jasco (1 mentions)
Ft ir tensor 27 spectrometer, by Bruker (1 mentions)
Mci gel chp 20p, by Mitsubishi (1 mentions)
Ft ir 8300 spectrophotometer, by Shimadzu (1 mentions)
F 7000 spectrometer, by Hitachi (1 mentions)
Uv 2700 uv vis spectrophotometer, by Shimadzu (1 mentions)
Microtof q 2 mass spectrometer, by Bruker (1 mentions)
J 1500, by Jasco (1 mentions)
1 4 dioxane, by J&K Scientific (1 mentions)
Av 400 mhz, by Bruker (1 mentions)
Waters q tof premier, by Waters Corporation (1 mentions)
1260 6221 tof mass spectrometry, by Agilent Technologies (1 mentions)
Precoated silica gel plates, by Qingdao Marine Chemical (1 mentions)
Uv 2401pc spectrometer, by Shimadzu (1 mentions)
11 protocols using av 600 mhz
1
Comprehensive Spectroscopic Analysis of Compounds
2
Characterization of Chitosan Amino Acid Grafts
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The FTIR and NMR analyses were carried out to demonstrate the grafting of amino acids on chitosan backbone. The FTIR spectra of bare chitosan and modified chitosan polymer were recorded by Shimadzu 8300 FTIR Spectrophotometer over the range 400–4000 cm−1 with resolution of 4 cm−1 and 64 scan acquisition following the method as described previously by Shigemasa et al.52 (link) The dried sample (2 mg) was mixed with KBR powder and pressed into a pellets at 20°C for spectra analysis.
In addition, to further verify the conjugation of amino acids onto chitosan backbone 1HNMR spectra of bare chitosan and Arg-CS-NAcHis was recorded by using a 1H Nuclear Magnetic Resonance Spectrometer (Bruker AV 600 MHz, Germany). Approximately, 5 mg samples solution in DMSO was prepared in 5 mm 1HNMR tube and mixed ultrasonically to dissolve at a final concentration of 5 mg/mL. The 1HNMR spectra was obtained with the following conditions; number of data points 298 K, relaxation delay between scans 1 second; acquisition time 3.75 second with number of scan 80.
In addition, to further verify the conjugation of amino acids onto chitosan backbone 1HNMR spectra of bare chitosan and Arg-CS-NAcHis was recorded by using a 1H Nuclear Magnetic Resonance Spectrometer (Bruker AV 600 MHz, Germany). Approximately, 5 mg samples solution in DMSO was prepared in 5 mm 1HNMR tube and mixed ultrasonically to dissolve at a final concentration of 5 mg/mL. The 1HNMR spectra was obtained with the following conditions; number of data points 298 K, relaxation delay between scans 1 second; acquisition time 3.75 second with number of scan 80.
3
Comprehensive analytical techniques for chemical characterization
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1H and 13C NMR spectra were recorded on a Bruker AV600MHz or AV850MHz spectrometer. High-resolution mass spectra (HRMS) were acquired on a Bruker micro TOF-Q-II mass spectrometer. Circular dichroism (CD) spectra were recorded on Jasco J-1500. Absorption spectra were recorded on a Shimadzu UV-2700 UV-Vis spectrophotometer. Fluorescence spectra were obtained on a Horiba Fluorolog-3 spectrometer or a Hitachi F-7000 spectrometer. ISE assay was conducted by an Orion Dual Star.
4
NMR Spectroscopy of Biological Samples
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The analysis was performed on Bruker AV 600 MHz superconducting Fourier transform nuclear magnetic resonance spectrometer. The plasma and liver samples were tested by relaxation‐edited pulse train (CPMG). TSP was taken as the reference peak of chemical shift, which was set as δ 0 ppm. One dimensional NMR spectra were obtained from the free induction attenuated signals by Fourier transform.
5
NMR Spectroscopy Analysis Protocol
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NMR spectra were obtained on Bruker AV-400
MHz and AV-600 MHz spectrometers. The 1H NMR chemical shifts
were measured relative to CDCl3 or DMSO-d6 as the internal reference (CDCl3: δ
= 7.26 ppm; DMSO-d6: δ = 2.50 ppm).
The 13C NMR chemical shifts were given using CDCl3 as the internal standard (CDCl3: δ = 77.16 ppm;
DMSO-d6: δ = 39.52 ppm). High-resolution
mass spectra (HRMS) were obtained with a Waters-Q-TOF-Premier (ESI).
Unless otherwise noted, all reagents were obtained from commercial
suppliers and used without further purification.
Unless otherwise
noted, all reagents were obtained from commercial suppliers and used
without further purification. PivOD (>95% deuterium incorporation
by 1H NMR analysis)20 (link) and 2-deuterated
benzo[b]thiophene (>95% deuterium incorporation
by 1H NMR analysis)21 (link) were prepared
according to the literature procedures. Ultradry solvents including N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO),
isopropanol (IPA), 1,2-dichloroethane (DCE), and 1,4-dioxane were
purchased from J&K Scientific. Tetrahydrofuran (THF) and methyl tert-butyl ether (MTBE) were dried by refluxing over Na
and freshly distilled prior to use.
MHz and AV-600 MHz spectrometers. The 1H NMR chemical shifts
were measured relative to CDCl3 or DMSO-d6 as the internal reference (CDCl3: δ
= 7.26 ppm; DMSO-d6: δ = 2.50 ppm).
The 13C NMR chemical shifts were given using CDCl3 as the internal standard (CDCl3: δ = 77.16 ppm;
DMSO-d6: δ = 39.52 ppm). High-resolution
mass spectra (HRMS) were obtained with a Waters-Q-TOF-Premier (ESI).
Unless otherwise noted, all reagents were obtained from commercial
suppliers and used without further purification.
Unless otherwise
noted, all reagents were obtained from commercial suppliers and used
without further purification. PivOD (>95% deuterium incorporation
by 1H NMR analysis)20 (link) and 2-deuterated
benzo[b]thiophene (>95% deuterium incorporation
by 1H NMR analysis)21 (link) were prepared
according to the literature procedures. Ultradry solvents including N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO),
isopropanol (IPA), 1,2-dichloroethane (DCE), and 1,4-dioxane were
purchased from J&K Scientific. Tetrahydrofuran (THF) and methyl tert-butyl ether (MTBE) were dried by refluxing over Na
and freshly distilled prior to use.
6
Spectroscopic and Mass Analytical Methods
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The reagents and solvents were commercially purchased and no further purification was required. Reactions were checked by thin-layer chromatography (TLC) on precoated silica gel plates (Qingdao Marine Chemical Factory, GF254). Melting points are determined on a XT4MP apparatus (Taike Corp., Beijing, China) and are not corrected. The purity (relative content) of active compounds was determined by HPLC through area normalisation method. 1H NMR and 13C NMR spectra were recorded on Bruker AV-400 or AV-600 MHz instruments using CDCl3 as solvent. High-resolution mass spectra (HRMS) were obtained on an Agilent 1260-6221 TOF mass spectrometry.
7
Spectroscopic Analysis of Natural Products
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NMR spectra were recorded on a Bruker AV-600 MHz (Bruker, Zurich, Switzerland) using TMS as an internal standard for chemical shifts with reference to the TMS resonance. ESIMS and HRTOF-ESIMS were measured on an API QSTAR Pulsar spectrometer. UV spectra were recorded on a Shimadzu UV-2401PC spectrometer. IR was recorded on the Bruker Tensor-27 instrument using KBr pellets. Optical rotations were recorded on a Horiba SEPA-300 polarimeter. CD spectra were measured on a Chirascan instrument. An Agilent 1100 series instrument equipped with an Agilent ZORBAX SB-C18 column (5 μm, 9.6 mm × 250 mm) was used for high-performance liquid chromatography (HPLC) separation.
TLC was performed on precoated TLC plates (200–250 µm thickness, F254 Si gel 60, Qingdao Marine Chemical, Inc., Qingdao, China), with compounds visualized by spraying the dried plates with 10% aqueous H2SO4 followed by heating until they were dry. Silica gel ((200–300) mesh, Qingdao Marine Chemical, Inc.), Lichroprep RP-18 (40–63 μm, Fuji), and Sephadex LH-20 (20–150 μm, Pharmacia) were used for column chromatography. Methanol, chloroform, ethyl acetate, acetone, petroleum ether, n-hexane, and 2-propanol were purchased from Tianjing Chemical Reagents Co. (Tianjing, China). All other materials were of the highest grade available.
TLC was performed on precoated TLC plates (200–250 µm thickness, F254 Si gel 60, Qingdao Marine Chemical, Inc., Qingdao, China), with compounds visualized by spraying the dried plates with 10% aqueous H2SO4 followed by heating until they were dry. Silica gel ((200–300) mesh, Qingdao Marine Chemical, Inc.), Lichroprep RP-18 (40–63 μm, Fuji), and Sephadex LH-20 (20–150 μm, Pharmacia) were used for column chromatography. Methanol, chloroform, ethyl acetate, acetone, petroleum ether, n-hexane, and 2-propanol were purchased from Tianjing Chemical Reagents Co. (Tianjing, China). All other materials were of the highest grade available.
8
Comprehensive Biophysical Characterization
9
Extraction and Purification of Streptomyces Compounds
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Streptomyces sp. FJS31-2 was cultured using 140 × 500 mL shake flasks containing 100 mL of ISP 2 agar medium with 10% natural humus acid water extracts and then incubated for 15 d at 28 °C. The solid culture was mashed and extracted three times with 140 L of ethanol after cultivation. The organic portion was then concentrated in vacuo to remove the solvent. The crude extract was applied to silica gel column chromatography using the CHCl3/MeOH gradient to obtain the crude products. Further purification was conducted using Sephadex LH-20 (GE Healthcare, Tokyo, Japan) (MeOH) column and RP-HPLC (Shimadzu SPD-M20A with Xbridge ODS 10 mm × 150 mm column). Compounds were identified with an HRESI-MS (Waters Xevo G2 QTOF mass spectrometer (Waters corportion, Milford, MA, USA) and NMR (Bruker AV 600 MHz) (Bruker Corporation, Karlsruhe, Germany) analyses.
10
Spectroscopic Characterization of Chitosan Derivatives
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To demonstrate the conjugation of AN and Arg groups to the CS, Fourier transform infrared (FTIR) and 1HNMR spectroscopy methods were used. The FTIR spectra of CS and AN–CS–Arg were recorded on an FTIR Spectrophotometer-430 (Jasco Company, Tokyo, Japan) following the method of Shigemasa et al.61 (link) Approximately 2 mg of the samples was mixed with 100 mg of KBr and made into pellets for spectroscopic analysis at 20°C. All spectra were measured over 400–4,000 cm−1.
1HNMR spectra of CS and AN–CS–Arg were recorded on a 1HNMR Spectrometer (Bruker AV 600 MHz; Bruker Optik GmbH, Ettlingen, Germany) using 5 mm 1HNMR tube at 25°C. Then, 5 mg samples were dissolved in 1 mL D2O solution and ultrasonically mixed to dissolve completely, yielding a final concentration of 5 mg/mL. 1HNMR spectra were measured at 298 K with 80 scans, a spectral width of 4,800 Hz, and a relaxation delay of 1 second between scans and acquisition time of 3.75 seconds.62
1HNMR spectra of CS and AN–CS–Arg were recorded on a 1HNMR Spectrometer (Bruker AV 600 MHz; Bruker Optik GmbH, Ettlingen, Germany) using 5 mm 1HNMR tube at 25°C. Then, 5 mg samples were dissolved in 1 mL D2O solution and ultrasonically mixed to dissolve completely, yielding a final concentration of 5 mg/mL. 1HNMR spectra were measured at 298 K with 80 scans, a spectral width of 4,800 Hz, and a relaxation delay of 1 second between scans and acquisition time of 3.75 seconds.62
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