Optical rotations were determined with a JASCO P1020 digital polarimeter. IR spectra were taken on a JASCO FT/IR-4100 spectrometer. The NMR spectra were recorded on a Varian 400MR FT-NMR instrument at 400 MHz for 1H and 100 MHz for 13C, and on a Varian Unity INOVA 500 FT-NMR spectrometer at 500 MHz for 1H and 125 MHz for 13C in CDCl3. LR- and HR-ESIMS were measured with a Bruker APEX II mass spectrometer. Silica gel 60 (230–400 mesh, Merck, Darmstadt, Germany) and SiliaBond C18 silica gel (40–63 µm, 60 Å, 17% carbon loading, SiliCycle, Québec, QC, Canada) were used for column chromatography. Precoated silica gel plates (Kieselgel 60 F254, Merck, Darmstadt, Germany) and precoated silica gel RP-18 plates (Kieselgel 60 F254S, Merck, Darmstadt, Germany) were used for TLC analysis.
Kieselgel 60 f254
Manufactured by Merck Group
Sourced in Germany, United States, Japan
Kieselgel 60 F254 is a type of silica gel used in thin-layer chromatography (TLC). It is a chemically inert, porous material with a high surface area that is commonly used as a stationary phase in TLC to separate and analyze a wide range of organic compounds. The material contains a fluorescent indicator, F254, which allows for the visualization of separated compounds under ultraviolet light.
Automatically generated - may contain errors
Lab products found in correlation
Silica gel 60, by Merck Group (26 mentions)
Rp 18 f254, by Merck Group (24 mentions)
Kieselgel 60, by Merck Group (20 mentions)
P 1010 polarimeter, by Jasco (6 mentions)
Silica gel, by Merck Group (6 mentions)
Avance 400, by Bruker (5 mentions)
Sephadex lh 20, by GE Healthcare (5 mentions)
Maxis impact spectrometer, by Bruker (5 mentions)
Drx 400, by Bruker (5 mentions)
Ac 400 spectrometer, by Bruker (5 mentions)
Jms 700, by JEOL (5 mentions)
P 2000 digital polarimeter, by Jasco (4 mentions)
Ultra shield 700, by Bruker (4 mentions)
Microtof q 2 mass spectrometer, by Bruker (4 mentions)
P 2000 polarimeter, by Jasco (4 mentions)
Silica gel 60 m, by Merck Group (4 mentions)
Avance 3 500 spectrometer, by Bruker (4 mentions)
Lichroprep rp 18, by Merck Group (4 mentions)
Jnm ecp 400 spectrometer, by JEOL (4 mentions)
Siliabond c18 silica gel, by Silicycle (3 mentions)
259 protocols using kieselgel 60 f254
1
Analytical Techniques for Compound Characterization
2
Spectroscopic Characterization of Natural Compounds
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NMR spectra, including
2D NMR (1H-1H COSY, HSQC, and HMBC), were obtained
using a Bruker Avance Neo 600 (Bruker, Germany) spectrometer at 600
MHz at the Central Laboratory of Kangwon National University (Chuncheon,
Korea). Column chromatography procedures were performed on silica
gel Kieselgel 60 (40–60 μm, 230–400 mesh, Merck,
Germany) and Sephadex LH-20 gel (18–111 μm, GE Healthcare,
Sweden). Thin-layer chromatography (TLC) was performed on precoated
silica gel plates (Kieselgel 60 F254 Merck, Germany) and
RP-C18 plates (Kieselgel 60 F254s, Merck, Germany).
Spots were detected by TLC using UV light or H2SO4-EtOH (v/v) spray followed by heating. Multiple preparative HPLC
was performed on a LC-Forte/R system equipped with a YMC UV/Vis detector
(YMC, Shimogyo-ku, Japan) using a YMC-Actus Triart C18 column
(s-5 μm, 12 nm, 20 × 250 mm2) at a flow rate
of 50 mL/min and monitored at 210 nm. Extra high purity solvents were
purchased from DaeJung (Sicheung, Korea) for extraction, fractionation,
and separation.
2D NMR (1H-1H COSY, HSQC, and HMBC), were obtained
using a Bruker Avance Neo 600 (Bruker, Germany) spectrometer at 600
MHz at the Central Laboratory of Kangwon National University (Chuncheon,
Korea). Column chromatography procedures were performed on silica
gel Kieselgel 60 (40–60 μm, 230–400 mesh, Merck,
Germany) and Sephadex LH-20 gel (18–111 μm, GE Healthcare,
Sweden). Thin-layer chromatography (TLC) was performed on precoated
silica gel plates (Kieselgel 60 F254 Merck, Germany) and
RP-C18 plates (Kieselgel 60 F254s, Merck, Germany).
Spots were detected by TLC using UV light or H2SO4-EtOH (v/v) spray followed by heating. Multiple preparative HPLC
was performed on a LC-Forte/R system equipped with a YMC UV/Vis detector
(YMC, Shimogyo-ku, Japan) using a YMC-Actus Triart C18 column
(s-5 μm, 12 nm, 20 × 250 mm2) at a flow rate
of 50 mL/min and monitored at 210 nm. Extra high purity solvents were
purchased from DaeJung (Sicheung, Korea) for extraction, fractionation,
and separation.
3
Liquid Chromatography-Mass Spectrometry Workflow
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Liquid chromatography-mass spectrometry (LC-MS) spectra were recorded on an Agilent 1100/ZQMSD (Santa Clara, CA, USA) instrument equipped with UV (220 nm and 254 nm) and MSAP+ and PL-ELS detectors. TLC was carried out using Kieselgel 60 F254 (Merck 1.05554.0001, Merck KGaA, Darmstadt, Germany). The analytical samples for NMR and HRMS studies were purified by preparative TLC using Kieselgel 60 F254 (Merck 1.07748.1000, Merck KGaA, Darmstadt, Germany) coated glass plates.
4
Spectroscopic Analysis of Organic Compounds
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Optical rotations were determined with a JASCO DIP-370 digital polarimeter. UV spectra were obtained in CH3CN using a JASCO V-530 spectrophotometer, and IR spectra were evaluated on a Hitachi 260-30 spectrophotometer. The 1H-NMR (500 MHz, using CDCl3 as solvent for determination), 13C-NNR (125 MHz), DEPT, HETCOR, COSY, NOESY, and HMBC spectra were obtained on a Varian (Unity Plus, CA, USA) NMR spectrometer. The low-resolution electrospray ionization mass spectrometry (ESI-MS) spectra were obtained on an API 3000 (Applied Biosystems, CA, USA). Silica gel 60 (Merck, 70–230 mesh, 230–400 mesh) was used for column chromatography. Precoated silica gel plates (Merck, Darmstadt, Germany, Kieselgel 60 F254, 0.50 mm, 0.20 mm) were used for analytical thin-layer chromatography (TLC), and precoated silica gel plates (Merck, Kieselgel 60 F-254, 0.50 mm) were used for preparative TLC. Spots were detected by spraying the plates with 50% H2SO4 and then heating them on a hot plate [25 (link),26 ].
5
Column Chromatography and Spectroscopic Analysis
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Column chromatography was performed in a glass column using Silica gel 60 (40–63 µm, Merck, Darmstadt, Germany) and SiliaBond C18 silica gel (40–63 µm, 60 Å, 17% carbon loading, Silicycle, Quebec, Canada), and the fractions were pooled according to the TLC analysis using precoated silica gel plates (Kieselgel 60 F254, 0.25 mm, Merck, Darmstadt, Germany) and silica gel RP-18 plates (Kieselgel 60 F254S, Merck, Darmstadt, Germany). UV and IR spectra were recorded on a PerkinElmer Lambda-265 UV-Vis and a PerkinElmer Spectrum Two FT-IR spectrometers (PerkinElmer Inc., Waltham, MA, USA), respectively. Optical rotations were determined at 25 °C with a JASCO P2000 digital polarimeter (JASCO Co., Tokyo, Japan). The NMR spectra, including the 2D NMR experiments, were performed on Bruker Avance-400 and -500 spectrometers (Bruker BioSpin, Rheinstetten, Germany) with chemical shifts reported in ppm referenced to δC 77.0/δH 7.26 ppm (CDCl3) and δC 135.5/δH 7.58 ppm (pyridine-d5).
6
Spectroscopic Characterization of Organic Compounds
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IR spectra were recorded on a PerkinElmer FT-IR Spectrum Two spectrophotometer. 1H-NMR (400 MHz) and 13C-NMR (100 MHz) spectra were measured in CDCl3 or C6D6 by using JEOL-JNM-ECS-400 spectrometer. ESI-MS were obtained on a Hitachi High-Technologies Corporation NanoFrontier eLD spectrometer. Optical rotations were measured on a HORIBA SEPA-500 polarimeter. UV-Vis spectra were recorded on a JASCO V-650 spectrophotometer. Silica gel (Merck, Kieselgel 60, 70-230 mesh) were used for column chromatography (CC). Silica gel plate (Merck, Kieselgel 60 F254S) was used for preparative thin-layer chromatography (TLC).
7
TLC Analysis of Carbohydrate Samples
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Carbohydrate samples were spotted in 1 cm lines on TLC sheets (Merck Kieselgel 60 F254, 20 × 20 cm), which were developed with 1-butanol: acetic acid: water = 2:1:1 (v/v/v). Bands were visualized by orcinol/sulfuric acid staining (10 min for 100°C).
8
Spectroscopic Characterization of Compounds
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1H and 13C NMR spectra were collected on a Bruker AVANCE III spectrometer (Germany) at 500 and 125 MHz, respectively, and chemical shifts are given in δ (ppm) using CDCl3, CD3OD, (CD3)2CO, or (CD3)2SO as solvent. High-resolution mass spectrometry (HRMS) analysis was performed using a Bruker MicroTOF-QII-system with an ESI-source. Melting point was determined using a Bibby Stuart Melting point SMB3 (UK). UV spectra were measured in ethanol on a T92+ Spectrophotometer (PG instrument, UK). Merck precoated silica gel plates (Kieselgel 60 F254, Germany) were used for analytical thin-layer chromatography (TLC). Merck preparative layer chromatography plates (PLC silica gel 60 F254, 2 mm thickness) and Scharlau silica gel 60 (0.06-0.2 mm) (Spain) were used for isolation and purification.
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1H and 13C NMR spectra were collected on a Bruker AVANCE III spectrometer (Germany) at 500 and 125 MHz, respectively, and chemical shifts are given in δ (ppm) using CDCl3, CD3OD, (CD3)2CO, or (CD3)2SO as solvent. High-resolution mass spectrometry (HRMS) analysis was performed using a Bruker MicroTOF-QII-system with an ESI-source. Melting point was determined using a Bibby Stuart Melting point SMB3 (UK). UV spectra were measured in ethanol on a T92+ Spectrophotometer (PG instrument, UK). Merck precoated silica gel plates (Kieselgel 60 F254, Germany) were used for analytical thin-layer chromatography (TLC). Merck preparative layer chromatography plates (PLC silica gel 60 F254, 2 mm thickness) and Scharlau silica gel 60 (0.06-0.2 mm) (Spain) were used for isolation and purification.
9
Dextran-based Celecoxib Conjugate Synthesis
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1,1′-Carbonyldiimidazole (CDI), dextranase (Penicillium sp.), and 3,5-dinitrosalicylic acid (DNS) were purchased from Sigma Chemical Co. (St Louis, MO, USA). Succinic anhydride and 5-benzyl N-(Boc)-glutamate were purchased from Tokyo Chemical Industry (Tokyo, Japan). Dextran (molecular weight: 15–20 kDa) was purchased from Fluka (Sigma Chemical Co.). Celecoxib was ether-extracted from Celebrex capsules (Pfizer, Inc., New York, NY, USA). All other chemicals were reagent grade, commercially available products. Buffer solutions (pH 1.2 and 6.8) were prepared as described in USP XXIII. Thin layer chromatographys (TLCs) were performed on Merck Kieselgel 60 F254. The high-performance liquid chromatography (HPLC) system consisted of a Model 306 pump, a Model 117 UV detector, a Model 234 autoinjector, and a Model 805 manometric module from Gilson (Middleton, WI, USA). A symmetry column C18 (Waters, Milford, MA, USA) (250×4.6 mm) with a guard column (Waters, 3.9×20 mm) was used. Six-week-old male Sprague Dawley rats (Samtako Bio Korea, Kyeong-gi-do, South Korea) were housed in the university animal facility with controlled temperature, humidity, and dark/light cycle. The animal protocol used in this study has been reviewed and approved by the Pusan National University-Institutional Animal Care and Use Committee (PNU-IACUC) on their ethical procedures and scientific care.
10
Nuclear Magnetic Resonance Spectroscopy Protocol
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All of the spectral
data including proton (1H-) and carbon (13C-)
NMR spectra were measured using dimethyl sulfoxide-d6 (DMSO-d6) or methanol-d3 (MeOH-d3) as the
solvent by a JNM ECP-400 spectrometer (JEOL, Tokyo, Japan) at 600
MHz for 1H NMR and 150 MHz for 13C NMR. Chemical
shift values were referenced versus appropriate residual solvent peaks
(2.50 ppm for 1H NMR and 39.52 ppm for 13C NMR).
Silica (Si) gel 60 (70-230 mesh, Merck, Darmstadt, Germany) was used
to perform column chromatography. Thin-layer chromatography was employed
on precoated Merck Kieselgel 60 F254 plates (20 ×
20 cm2, 0.25 mm, Merck, Darmstadt, Germany) sprayed with
50% H2SO4. All solvents used for column chromatography
were of reagent grade and were acquired from commercial sources (E.
Merck, Fluka and Sigma-Aldrich Co).
data including proton (1H-) and carbon (13C-)
NMR spectra were measured using dimethyl sulfoxide-d6 (DMSO-d6) or methanol-d3 (MeOH-d3) as the
solvent by a JNM ECP-400 spectrometer (JEOL, Tokyo, Japan) at 600
MHz for 1H NMR and 150 MHz for 13C NMR. Chemical
shift values were referenced versus appropriate residual solvent peaks
(2.50 ppm for 1H NMR and 39.52 ppm for 13C NMR).
Silica (Si) gel 60 (70-230 mesh, Merck, Darmstadt, Germany) was used
to perform column chromatography. Thin-layer chromatography was employed
on precoated Merck Kieselgel 60 F254 plates (20 ×
20 cm2, 0.25 mm, Merck, Darmstadt, Germany) sprayed with
50% H2SO4. All solvents used for column chromatography
were of reagent grade and were acquired from commercial sources (E.
Merck, Fluka and Sigma-Aldrich Co).
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