The degree of functionalization was studied by using 1H NMR according to a previously reported method [21 (link)]. 1H NMR spectra were collected by using an NMR spectrometer (AL300; JEOL, Tokyo, Japan) with a single axis gradient inverse probe at a frequency of 300 MHz. Before the measurement, 30 mg of GelMA and GelMAGMA macromers were respectively dissolved into 1 mL deuterium oxide containing 0.05% (w/v) 3-(trimethylsilyl)propionic-2,2,3,3-d4 acid sodium salt (Sigma-Aldrich, St. Louis, MO, USA) for calibration at 40 °C.
Al300
Manufactured by JEOL
Sourced in Japan
The JEOL AL300 is a compact, high-performance atomic force microscope (AFM) designed for nanoscale imaging and analysis. The AL300 provides precise measurements of surface topography, roughness, and other nanoscale features without the need for complex sample preparation.
Automatically generated - may contain errors
Lab products found in correlation
Nicolet 6700, by Thermo Fisher Scientific (3 mentions)
Al 400, by JEOL (2 mentions)
3 trimethylsilyl propionic 2 2 3 3 d4 acid sodium salt, by Merck Group (1 mentions)
Elix water purification system, by Merck Group (1 mentions)
Vario el 3 microanalyzer, by Elementar (1 mentions)
Hexane, by Merck Group (1 mentions)
Thiosemicarbazide, by Merck Group (1 mentions)
Hplc grade methanol, by Merck Group (1 mentions)
Acetonitrile acn, by Merck Group (1 mentions)
Xevo g2 xs qtof mass spectrometer, by Waters Corporation (1 mentions)
1100 series, by Agilent Technologies (1 mentions)
Gc 2010, by Agilent Technologies (1 mentions)
Activated alumina, by Fujifilm (1 mentions)
Ecx 400p, by JEOL (1 mentions)
Aluminium oxide 60 f254, by Merck Group (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Spd 20av, by Shimadzu (1 mentions)
Lc 20ap pump, by Shimadzu (1 mentions)
Microtof q 3 spectrometer, by Bruker (1 mentions)
Milli q advantage a10 water purification system, by Merck Group (1 mentions)
7 protocols using al300
1
Quantifying Degree of GelMA Functionalization
2
Synthesis and Characterization of HM Compound
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Hexane (95%), thiosemicarbazide (98%) was purchased from Sigma-Aldrich (St. Louis, MO, USA). HM was prepared in the Medicinal and Process Chemistry Division of Central Drug Research Institute, Lucknow, Uttar Pradesh, India. Milli-Q pure water was obtained from a Millipore Elix water purification system (Millipore India Pvt. Ltd., New Delhi, India). high-performance liquid chromatography (HPLC) grade methanol and acetonitrile (ACN) were purchased from Merck Ltd., (Mumbai, India). IR spectra was recorded using potassium bromide (KBr) discs, on a PerkinElmer Spectrum RX1 infrared (IR) spectrophotometer. 1H and 13C nuclear magnetic resonance (NMR) spectra were recorded in dimethyl sulfoxide (DMSO) on Bruker DRX-300 (400 MHz) and JEOL AL300 Fourier transform (FT)-NMR (400 MHz) systems; chemical shift (d) is reported in ppm using tetramethyl silane as an internal reference. Mass spectra were recorded on Agilent 6520 mass spectrometer. Elemental analysis was performed on Elementar's Vario EL III micro-analyzer.
3
Spectroscopic Analysis of Enantioselective Compounds
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Conversion and enantiomeric excess (ee) were determined by GC analysis on a SHIMADZU GC-2010 or by HPLC analysis on an Agilent 1100 Series instrument by comparison with synthesized racemic compounds. NMR spectra were recorded on a JEOL AL-300 (1H NMR 300.40 MHz, 13C NMR 75.45 MHz) spectrometer. 1H NMR chemical shifts were reported in parts per million (ppm) relative to tetramethylsilane (0 ppm) in CDCl3, except for the broad peaks. 13C NMR chemical shifts for were reported in parts per million (ppm) relative to CDCl3 (77.16 ppm) with complete proton decoupling. High-resolution electrospray-ionization mass spectra (HRMS (ESI)) were recorded with on a Waters Xevo G2-XS QTof mass spectrometer.
4
NMR and Spectroscopy Characterization Protocol
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1H and 13C{1H} NMR spectra were recorded using a JEOL AL300 (300 MHz for 1H, 75.5 MHz for 13C) and JEOL ECX-400P (400 MHz for 1H, 99.6 MHz for 13C) spectrometer with CDCl3, CD2Cl2, CD3OD, and THF-d8, and the chemical shifts were noted in δ ppm with reference to the internal tetramethylsilane peak (Si(CH3)4, 0.00 ppm) and internal residual solvent peak (7.27 ppm for CHCl3, 5.30 ppm for CH2Cl2, 3.33 ppm for CH3OH, and 1.72 and 3.58 ppm for THF). Silica gel column chromatography was performed using Silica Gel 60 spherical, neutrality (Nacalai tesque inc.). Alumina column chromatography was carried out using activated alumina (300 mesh, Wako). Thin layer chromatography (TLC) was conducted on aluminium plates coated with silica gel 60 F254 (Merck) or aluminium oxide 60 F254 (Merck). Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectra were taken using the golden gate diamond anvil ATR accessory (NICOLET 6700, Thermo scientific), using typically 64 scans at a resolution of 2 cm–1. High-resolution mass spectra (HRMS) were measured using a JEOL JMS-HX110A spectrometer. All reactions were performed under argon.
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1H and 13C{1H} NMR spectra were recorded using a JEOL AL300 (300 MHz for 1H, 75.5 MHz for 13C) and JEOL ECX-400P (400 MHz for 1H, 99.6 MHz for 13C) spectrometer with CDCl3, CD2Cl2, CD3OD, and THF-d8, and the chemical shifts were noted in δ ppm with reference to the internal tetramethylsilane peak (Si(CH3)4, 0.00 ppm) and internal residual solvent peak (7.27 ppm for CHCl3, 5.30 ppm for CH2Cl2, 3.33 ppm for CH3OH, and 1.72 and 3.58 ppm for THF). Silica gel column chromatography was performed using Silica Gel 60 spherical, neutrality (Nacalai tesque inc.). Alumina column chromatography was carried out using activated alumina (300 mesh, Wako). Thin layer chromatography (TLC) was conducted on aluminium plates coated with silica gel 60 F254 (Merck) or aluminium oxide 60 F254 (Merck). Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectra were taken using the golden gate diamond anvil ATR accessory (NICOLET 6700, Thermo scientific), using typically 64 scans at a resolution of 2 cm–1. High-resolution mass spectra (HRMS) were measured using a JEOL JMS-HX110A spectrometer. All reactions were performed under argon.
5
Characterization of Hydrophobically Modified PVAs
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The chemical
structures of the hm-PVAs were analyzed by nuclear magnetic resonance
(1H NMR) spectroscopy (AL300; JEOL Ltd., Tokyo, Japan)
using a 0.5% (w/v) hm-PVA/DMSO-d6 solution
at 25 °C. Each sample was scanned eight times. Fourier transform
infrared spectroscopy (FT-IR; 8400S, Shimadzu Corp., Kyoto, Japan)
was conducted to confirm the presence of acetal groups in the hm-PVAs.
The scan range was 700–4000 cm–1, and each
sample was scanned 64 times. The hydrophobic group modification ratios
of the hm-PVAs were determined by 1H NMR spectroscopy.
The modification ratios were calculated as follows where the integral area (αCH proton)
is the area of the peak at 3.87 ppm, corresponding to the αCH
proton in the PVA and hm-PVA backbones, and the integral area (CH3 proton) is the area of the peak at 0.85 ppm assigned to the
CH3 proton in the hydrophobic groups of the hm-PVAs.
structures of the hm-PVAs were analyzed by nuclear magnetic resonance
(1H NMR) spectroscopy (AL300; JEOL Ltd., Tokyo, Japan)
using a 0.5% (w/v) hm-PVA/DMSO-d6 solution
at 25 °C. Each sample was scanned eight times. Fourier transform
infrared spectroscopy (FT-IR; 8400S, Shimadzu Corp., Kyoto, Japan)
was conducted to confirm the presence of acetal groups in the hm-PVAs.
The scan range was 700–4000 cm–1, and each
sample was scanned 64 times. The hydrophobic group modification ratios
of the hm-PVAs were determined by 1H NMR spectroscopy.
The modification ratios were calculated as follows where the integral area (αCH proton)
is the area of the peak at 3.87 ppm, corresponding to the αCH
proton in the PVA and hm-PVA backbones, and the integral area (CH3 proton) is the area of the peak at 0.85 ppm assigned to the
CH3 proton in the hydrophobic groups of the hm-PVAs.
6
Analytical Techniques for Chemical Characterization
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Nuclear magnetic resonance (NMR) analyses for 1H and 13C NMR spectra were measured on either a JEOL AL300 (300 MHz) or an AL400 (400 MHz) instrument. High-resolution mass spectroscopy (HRMS) was carried out on a Bruker MicrOTOF-QIII spectrometer by electrospray ionization time-of-flight (ESI-TOF). Matrix-assisted laser desorption ionization (MALDI-TOF) mass spectrometry analysis was obtained on a Bruker autoflex spectrometer using 2,5-dihydroxybenzoic acid as a matrix. Reversed-phase high-performance liquid chromatography (HPLC) was performed using a Shimadzu system (Kyoto, Japan), consisting of two LC-20AP pumps and a SPD-20AV photodiode array detector. The used column was a preparative 20 × 250–mm Cosmosil 5C18-AR-300 from Waters Corporation (MA, USA). Ultrapure water used for all experiments described in this paper was obtained from the Milli-Q Advantage A10 Water Purification System sold by Merck Millipore (Burlington, USA).
7
Characterization of Trinuclear Complexes
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General procedures
1 H NMR spectra were recorded using a JEOL AL400 (400 MHz)
or an AL300 (300 MHz) instrument with the analyte dissolved in acetone-d 6 , MeCN-d 3 , or CDCl 3 . 31 P NMR spectra were recorded using a JEOL ECX400 (400 MHz) instrument with the analyte dissolved in acetone-d 6 . IR spectra were recorded using a JASCO FT/IR-610 spectrometer with a resolution of 1 cm 860-CO oven. The eluent was a 1 : 1 (v/v) mixture of methanol and MeCN containing 0.5 M CH 3 COONH 4 , and the flow rate was 0.2 mL min -1 . Separation of the trinuclear complexes was achieved using SEC with a pair of Shodex PROTEIN KW-2002.5 columns (300 mm long, 20.0 mm i.d.) with a KW-LG guard column (50 mm long, 8.0 mm i.d.) and a recycling preparative HPLC apparatus with a JASCO 870-UV detector. The eluent was a 1 : 1 (v/v) mixture of methanol and MeCN containing 0.15 M CH 3 COONH 4 , and the flow rate was 6.0 mL min -1 . UV-vis absorption spectra were recorded using a JASCO V-670 instrument.
1 H NMR spectra were recorded using a JEOL AL400 (400 MHz)
or an AL300 (300 MHz) instrument with the analyte dissolved in acetone-d 6 , MeCN-d 3 , or CDCl 3 . 31 P NMR spectra were recorded using a JEOL ECX400 (400 MHz) instrument with the analyte dissolved in acetone-d 6 . IR spectra were recorded using a JASCO FT/IR-610 spectrometer with a resolution of 1 cm 860-CO oven. The eluent was a 1 : 1 (v/v) mixture of methanol and MeCN containing 0.5 M CH 3 COONH 4 , and the flow rate was 0.2 mL min -1 . Separation of the trinuclear complexes was achieved using SEC with a pair of Shodex PROTEIN KW-2002.5 columns (300 mm long, 20.0 mm i.d.) with a KW-LG guard column (50 mm long, 8.0 mm i.d.) and a recycling preparative HPLC apparatus with a JASCO 870-UV detector. The eluent was a 1 : 1 (v/v) mixture of methanol and MeCN containing 0.15 M CH 3 COONH 4 , and the flow rate was 6.0 mL min -1 . UV-vis absorption spectra were recorded using a JASCO V-670 instrument.
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