All commercial reagents and solvents were used as received without further purification unless otherwise indicated. Synthetic compounds 3a –d and 4a –l were directly used for reaction without further purification and characterization. Melting points were recorded on an SGW X-4 microscope melting point apparatus (Shanghai Tech Instrument Co., Ltd., Shanghai, China). Infrared spectra (IR) were performed on NICOLET iS10 sepectrometer (Shimazu Co., Ltd., Kyoto, Japan). NMR spectra were recorded on a Bruker Avance 500MHz spectrometer (Bruker Co., Ltd., Zurich, Switzerland) at room temperature with tetramethylsilane (TMS) as an internal standard and CDCl3 or DMSO-d6 as solvents. Mass spectra (MS) were obtained by LCMS-IT-TOF spectrometer (Shimadzu Co., Ltd., Kyoto, Japan) or TSQ Quantum Ultra (Thermo Scientific Co., Ltd., Madison, WI, USA). Elemental analysis for C, H, O, and N were carried out with Elementar VarioMICRO Cube analyzer (Elementar, Frankfurt, Germany).
Lcms it tof spectrometer
Manufactured by Shimadzu
Sourced in Japan
The LCMS-IT-TOF spectrometer is a hybrid mass spectrometry instrument that combines liquid chromatography (LC) with ion trap time-of-flight (IT-TOF) mass analysis. The core function of this system is to provide high-resolution, accurate mass measurement capabilities for the identification and quantification of a wide range of chemical compounds.
Automatically generated - may contain errors
Lab products found in correlation
Silica gel, by Qingdao Haiyang Chemical (2 mentions)
Lc 20at, by Shimadzu (2 mentions)
Drx 400 spectrometer, by Bruker (2 mentions)
Rp 18 f254s plates, by Merck Group (2 mentions)
Avance 500 mhz spectrometer, by Bruker (1 mentions)
Tsq quantum ultra, by Thermo Fisher Scientific (1 mentions)
Vario micro cube analyzer, by Elementar (1 mentions)
Uv 2450 spectrophotometer, by Shimadzu (1 mentions)
Tensor 37 infrared spectrophotometer, by Bruker (1 mentions)
Pack ods a column, by YMC (1 mentions)
Lux cellulose 2 chiral column, by Phenomenex (1 mentions)
Eca 500ii, by JEOL (1 mentions)
V 550 uv vis spectrometer, by Jasco (1 mentions)
Fluorolog 3 spectrofluorometer, by Horiba (1 mentions)
Optima 8000, by PerkinElmer (1 mentions)
Acetonitrile, by Merck Group (1 mentions)
Streptozotocin (stz), by Merck Group (1 mentions)
Metformin, by Merck Group (1 mentions)
Acarbose, by Merck Group (1 mentions)
Avance 400 mhz, by Brucker (1 mentions)
14 protocols using lcms it tof spectrometer
1
Synthesis and Characterization of Novel Compounds
2
Detailed Analytical Techniques for Chemical Characterization
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Optical rotations were measured on a Perkin-Elmer 341 polarimeter (Perkin-Elmer, Waltham, MA, USA). UV spectra were recorded on a Shimadzu UV-2450 spectrophotometer (Shimadzu, Kyoto, Japan). IR spectra were determined on a Bruker Tensor 37 infrared spectrophotometer (Bruker, Bremerhaven, Germany) with KBr disks. NMR spectra were measured on a Bruker AM-400/500 spectrometer (Bruker, Bremerhaven, Germany) at 25 °C. HRESIMS analyses were carried out on a Shimadzu LCMS-IT-TOF spectrometer (Shimadzu, Kyoto, Japan). A Shimadzu LC-20AT (Shimadzu, Kyoto, Japan) equipped with an SPD-M20A PDA detector was used for the HPLC analysis, and a YMC-pack ODS-A column (250 × 10 mm, S-5 μm, 12 nm) (YMC, Kyoto, Japan) or Phenomenex Lux cellulose-2 chiral column (250 × 10 mm, 5 μm, 12 nm) (Phenomenex, Los Angeles, CA, USA) was used for semipreparative HPLC separation. Silica gel (100–200, 300–400 mesh, Qingdao Haiyang Chemical Co. Ltd., Qingdao, China) and Sephadex LH-20 gel (GE Amersham Biosciences, Boston, MA, USA) were used for the column chromatography (CC). All solvents were of analytical grade (Guangzhou Chemical Reagents Company, Ltd., Guangzhou, China) while acetonitrile (MeCN) was of HPLC grade (Grace Chemical Technology Co. Ltd., Qingdao, China).
3
Mass Spectrometry and NMR Analysis
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HRMS (ESI) data were obtained in the positive and negative modes on a SHIMADZU LC–MS-IT-TOF spectrometer. NMR spectra were recorded on ECA500II and ECX400P spectrometers (JEOL). Compounds 1a –f were dissolved in dimethyl sulfoxide-d6 (DMSO-d6) and 2a –f , 3a –f , and 4a –f in chloroform-d (CDCl3), and their spectra are expressed in ppm) based on the residuals of these solvents at 2.49 and 7.26 for 1H NMR and 39.5 and 77.0 for 13C NMR.
4
Characterization of 3CLpro Inhibitor
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Ultraviolet (UV) spectra were recorded using a JASCO V-550 UV/VIS spectrometer (Jasco, Japan). 1H (400 MHz) and 13C (100 MHz) nuclear magnetic resonance (NMR) spectra were obtained using a Bruker DRX-400 spectrometer (Bruker, Ettlingen, Germany) with tetramethylsilane as the internal standard. Electrospray ionization-mass spectrometry (ESI-MS) was performed on a Shimadzu LCMS-IT-TOF spectrometer (Shimadzu Co., Kyoto, Japan). Thin-layer chromatography (TLC) analysis was performed on silica gel 60 F254 and RP-18 F254S plates (0.25 mm layer thickness; Merck, Darmstadt, Germany). Column chromatography was performed using silica gel (60 A, 70–230, or 230–400 mesh ASTM; Merck, Darmstadt, Germany) and reversed-phase silica gel (ODS-A 12 nm S-150, S-75 μm; YMC Co., Kyoto, Japan). Spots were detected with UV light (254 nm) and sprayed with 10% H2SO4, followed by heating. 3CLpro was purchased from Sigma Aldrich (St. Louis, MO, USA). 3Clpro Substrate was synthesized with Anygen (Gwangju, Republic of Korea).
5
Actinide and Lanthanide Extraction Protocol
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The reagents mentioned were
purchased from Aladdin (Shanghai Aladdin Biochemical Technology Co.
Ltd, China) and were of analytical or chromatographic grade. CH2Cl2 and THF were distilled from CaH2. The reactions were conducted under N2 unless otherwise
stated. 241Am and 152,154Eu, provided by the
China Institute of Atomic Energy, were used as radioactive tracers
in solvent extraction.
The NMR spectra were recorded on a Varian
Inova NMR spectrometer (Bruker Inc., Switzerland). Electrospray ionization
mass spectrometry (ESI-MS) data were obtained by an LCMS-IT-TOF spectrometer
(Shimadzu, Japan). The concentration of Eu was determined using an
inductively coupled plasma optical emission spectrometer (ICP-OES,
Optima8000, PerkinElmer).
The activities of 241Am
and 152,154Eu were
measured by a NaI (TI) scintillation counter. Luminescence spectroscopic
titration was obtained on a fluorescence spectrophotometer (F96pro,
China). The Transient Fluorescence spectra was measured on a Fluorolog-3
spectrofluorometer (JobinYvon, Horiba).
purchased from Aladdin (Shanghai Aladdin Biochemical Technology Co.
Ltd, China) and were of analytical or chromatographic grade. CH2Cl2 and THF were distilled from CaH2. The reactions were conducted under N2 unless otherwise
stated. 241Am and 152,154Eu, provided by the
China Institute of Atomic Energy, were used as radioactive tracers
in solvent extraction.
The NMR spectra were recorded on a Varian
Inova NMR spectrometer (Bruker Inc., Switzerland). Electrospray ionization
mass spectrometry (ESI-MS) data were obtained by an LCMS-IT-TOF spectrometer
(Shimadzu, Japan). The concentration of Eu was determined using an
inductively coupled plasma optical emission spectrometer (ICP-OES,
Optima8000, PerkinElmer).
The activities of 241Am
and 152,154Eu were
measured by a NaI (TI) scintillation counter. Luminescence spectroscopic
titration was obtained on a fluorescence spectrophotometer (F96pro,
China). The Transient Fluorescence spectra was measured on a Fluorolog-3
spectrofluorometer (JobinYvon, Horiba).
6
Enzymatic Assay for Antidiabetic Evaluation
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Streptozotocin (STZ), acarbose, metformin (MF), p-nitophenylglucopyranoside, α- glucosidase (Saccharomyces cerevisiae), porcine pancreatic α-amylase were purchased from Sigma-Aldrich, St’ Louis, MO, USA. Folin-Ciocalteu reagent was purchased from Loba chemie, Mombai, India. External standards for HPLC analysis were either isolated from the plant or supplied by National Organization of Drug Control and Research (NODCAR), Egypt. All solvents were of analytical grade and purchased from Adwic company, Egypt. Acetonitrile and trifluoracetic acid were of HPLC grade and purchased from Sigma-Aldrich (MO, USA). Stationary phases for chromatographic separations were purchased from Merck (Darmstadt, Germany). NMR spectra were acquired using Brucker, Avance, 400 MHz. (MA, USA). MS data were recorded on Shimadzu LCMS-IT-TOF spectrometer (Kyoto, Japan).
7
Spectroscopic Characterization of Compounds
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Optical
rotations were measured on a JASCO P2100 polarimeter (Japan). Mass
spectral data were carried out on a SHIMADZU LCMS-IT-TOF spectrometer.
The NMR experiments for all of the isolated compounds were done using
a Bruker AscendTM 400/R NMR spectrometer with the following frequencies: 1H NMR (400 MHz) and 13C NMR (100 MHz). Deuterated
methanol (CD3OD) was selected as the solvent of choice
for the NMR experiments with TMS as internal standard, and chemical
shifts were detected in δ ppm values.
rotations were measured on a JASCO P2100 polarimeter (Japan). Mass
spectral data were carried out on a SHIMADZU LCMS-IT-TOF spectrometer.
The NMR experiments for all of the isolated compounds were done using
a Bruker AscendTM 400/R NMR spectrometer with the following frequencies: 1H NMR (400 MHz) and 13C NMR (100 MHz). Deuterated
methanol (CD3OD) was selected as the solvent of choice
for the NMR experiments with TMS as internal standard, and chemical
shifts were detected in δ ppm values.
8
Characterization and Purification Methods
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All reagents were purchased from Sigma-Aldrich, Strem, TCI, and Alfa Aesar chemical companies and used without further purification. Analytical thin-layer chromatography (TLC) was performed using silica gel 60 F254 precoated plates (0.25 mm thickness) with a fluorescent indicator. Visualisation of the TLC plates was performed by means of UV light or either KMnO4 or I2 stains. NMR spectra were recorded on Bruker Avance 500 MHz spectrometers; chemical shifts were reported in ppm and calibrated to residual solvent peaks at 7.27 ppm and 77.00 ppm for 1H and 13C in CDCl3 or internal reference compounds. The following abbreviations are used in reporting the NMR data: s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet), and br (broad). Coupling constants (J) are expressed in Hz. Spectra are reported as follows: chemical shift (δ, ppm), multiplicity, integration, and coupling constants (Hz). The products were purified by flash chromatography on silica gel 60 (230–400 mesh) using a BUCHI chromatograph. MS spectra were recorded on a Shimadzu LCMS IT-TOF spectrometer.
9
Ruthenium-Catalyzed Organic Synthesis
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Commercially available chemicals were used as received. Ruthenium catalysts were obtained from Apeiron Catalysts. Scavenger III was prepared according to a procedure reported in the literature.55 Merck silica gel 60 (230–400 mesh) was used for filtration through silica gel. NMR (1H and 13C) spectra were recorded on Agilent Mercury 400 MHz spectrometers, with CDCl3 as the solvent. Chemical shifts (δ) are given in ppm, with the solvent signal of CDCl3 used as a point of reference. Coupling constants (J) are reported in Hertz (Hz). IR spectra were recorded on a Thermo Scientific Nicolet iS 50 FT-IR spectrometer; wavenumbers ( ) are given in cm−1. MS measuremens were recorded on a Shimadzu LCMS-IT-TOF spectrometer. GC measurements were performed on a PerkinElmer Clarus 580 instrument with an InertCap 5MS-Sil column. Elemental analyses were performed by the Institute of Organic Chemistry, PAS, Warsaw. The determination of ruthenium content was performed by the Certified Chemical Laboratory of Multielemental Analyses, Wrocław University of Technology.
10
Synthetic Characterization and Purification
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All commercial reagents and solvents were purchased from commercial suppliers and used without further purification. 1H- and 13C-NMR spectra were recorded using TMS as the internal standard in CDCl3 or DMSO-d6 with a Bruker BioSpin GmbH spectrometer (Billerica, MA, USA) at 400 MHz and 101 MHz, respectively. High resolution mass spectra (HRMS) were recorded using Shimadzu LCMS-IT-TOF spectrometer (Shimadzu, Kyoto, Japan). Melting points (mp) were obtained using a SRS-OptiMelt automated melting point instrument (Sunnyvale, CA, USA) without correction. The purities of synthesized compounds were confirmed to be higher than 95% by analytical HPLC performed with a dual pump Shimadzu LC-20AB (Shimadzu) system equipped with a Ultimate XB-C18 column and eluted with methanol-water (60:40–70:30) containing 0.1% TFA at a flow rate of 0.3 mL/min. Flash column chromatography was performed with silica gel (200–300 mesh) purchased from Qingdao Haiyang Chemical Co. Ltd. (Qingdao, China). All the reactions were monitored by thin layer chromatography using silica gel.
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