Reagents and solvents were acquired from Sigma Aldrich and used without further purification. Reactions were monitored by TLC using 0.2 mm silica plates with UV indicator (UV254). Column chromatography was executed using Sorbent Technologies 60Ȧ silica gel (230–400 mesh) or Merck neutral aluminum oxide (70–230 mesh). Merck TLC silica gel 60 glass plates were use for preparative thin layer chromatography. All 1H NMR and 13C NMR spectra were obtained using a Bruker AV-500, DPX-400, AV-400, or DPX-250 spectrometer (500 MHz, 400 MHz or 250 MHz for 1H, 100 MHz for 13C) with samples dissolved in deuterated chloroform, acetone, or DMSO using trimethylsilane as an internal indicator. Chemical shifts (δ) are conveyed in ppm with CDCl3 (1H: 7.27 ppm; 13C: 77.16 ppm), acetone-d6 (1H: 2.05 ppm; 13C: 29.84 ppm), and DMSO-d6 (1H: 2.50 ppm; 13C: 39.52 ppm) used as references. Coupling constants (J) are stated in Hertz (Hz). High resolution ESI mass spectra were obtained using an Agilent Technologies 6210 ESI-TOF Mass Spectrometer.
6210 esi tof mass spectrometer
Manufactured by Agilent Technologies
Sourced in United States
The 6210 ESI/TOF mass spectrometer is a high-performance instrument designed for accurate mass determination and analysis of a wide range of molecular compounds. It utilizes electrospray ionization (ESI) coupled with time-of-flight (TOF) mass analysis technology to provide precise mass measurements and high-resolution data.
Automatically generated - may contain errors
Lab products found in correlation
V 550 uv vis spectrophotometer, by Jasco (4 mentions)
Av 400 spectrometer, by Bruker (3 mentions)
Tlc silica gel 60 glass plates, by Merck Group (2 mentions)
Ft ir 480 plus ft ir spectrometer, by Jasco (2 mentions)
P 1020 polarimeter, by Jasco (2 mentions)
Sephadex lh 20, by GE Healthcare (2 mentions)
Av 500, by Bruker (1 mentions)
Av 400, by Bruker (1 mentions)
Dpx 250, by Bruker (1 mentions)
Dpx 400, by Bruker (1 mentions)
P 1020 digital polarimeter, by Jasco (1 mentions)
Av 600 spectrometer, by Bruker (1 mentions)
J 810 spectrometer, by Jasco (1 mentions)
G1311c pump, by Agilent Technologies (1 mentions)
Silica gel, by Qingdao Marine Chemical (1 mentions)
Reverse phase c18 silica gel, by Merck Group (1 mentions)
Av 300, by Bruker (1 mentions)
P 1030, by Jasco (1 mentions)
Waters chromatograph, by Waters Corporation (1 mentions)
Nicolet 6700 spectrometer, by Thermo Fisher Scientific (1 mentions)
12 protocols using 6210 esi tof mass spectrometer
1
General Organic Chemistry Protocols
2
Analysis of IMMU-132 Antibody Chains
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Because the interchain disulfides are reduced and the resulting sulfhydryl groups are used for drug conjugation (or blocked), the heavy and light chains resolved during LC-MS analysis without addition of reducing agents, and were analyzed independently. Different lots of IMMU-132 were injected on an Agilent 1200 series HPLC using an Aeris Widepore C4 reverse-phase HPLC column (3.6 μM, 50 × 2.1 mm) and resolved by reverse phase HPLC with a 14-min linear gradient of 30 – 80% acetonitrile in 0.1% formic acid. Electrospray ionization time of flight (ESI-TOF) mass spectrometry was accomplished with an in-line Agilent 6210 ESI-TOF mass spectrometer with Vcap, fragmentor and skimmer set to 5000V, 300V and 80V, respectively. The entire RP-HPLC peak representing all kappa or heavy chain species were used to generate deconvoluted mass spectra.
3
Preparative HPLC Characterization of Compounds
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Preparative HPLC was performed using a COSMOSIL C18 preparative column (5 μm, 20 × 250 mm). HRESIMS data were acquired using an Agilent 6210 ESI/TOF mass spectrometer (NYSE: A, MA, USA). Optical rotations were measured using a JASCO P-1020 digital polarimeter (JASCO, Tokyo, Japan). UV spectra were measured using a JASCO V-550 UV/vis spectrophotometer (JASCO, Tokyo, Japan). A JASCO FT/IR-480 plus FT-IR spectrometer was used for scanning the IR spectra with KBr pellets (JASCO, Tokyo, Japan). The 1D and 2D NMR spectra were obtained on a Bruker AV-600 spectrometer with TMS as internal standard. All chemical reagents were purchased from Tianjin Damao Chemical Company (Tianjin, China).
4
Isolation and Characterization of Natural Products
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Optical rotations were obtained on a JASCO P-1020 polarimeter. UV spectra were recorded using a JASCO V-550 UV/VIS spectrophotometer. CD spectra were measured on a JASCO J-810 spectrometer. 1D and 2D NMR spectra were recorded on Bruker AV-500 NMR spectrometers with TMS as an internal standard. HRESIMS analyses were recorded on an Agilent 6210 ESI/TOF mass spectrometer. Column chromatography (CC) was performed with Silica gel (Qingdao Marine Chemical Plant, Qingdao, P. R. China), ODS (50 μm, YMC, Kyoto, Japan) and Sephadex LH-20 (Pharmacia Biotech, Uppsala, Sweden). Preparative HPLC was conducted on a Cosmosil C18 preparative column (5 μm, 20 × 250 mm) equipped with a G1311C pump and a G1315D photodiode array detector (Agilent Technologies, CA, USA). All chemical reagents were purchased from Tianjin Damao Chemical Company (Tianjin, P. R. China).
5
Spectroscopic Characterization of Compounds
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Ultraviolet (UV) spectra were determined in CH3Cl3 on a Jasco V-550 UV/vis spectrophotometer. ESI-MS spectra were carried out on a Finnigan LCQ Advantage Max ion trap mass spectrometer. HR-ESI-MS data were obtained on an Agilent 6210 ESI/TOF mass spectrometer. Optical rotation was recorded in CH3Cl3 on Jasco P-1020 polarimeter at room temperature. Infrared (IR) spectra were measured on a Jasco FT/IR-480 plus Fourier Transform infrared spectrometer using KBr pellet. Nuclear magnetic resonance (NMR) spectra were measured on Bruker AV-300 or AV-400 spectrometers. Thin-layer chromatography (TLC) analyses were carried out using pre-coated silica gel GF254 plates (Qingdao Marine Chemical Plant, P.R. China). Column chromatographies were performed on silica gel (200–400 mesh, Qingdao Marine Chemical Plant, P.R. China), reverse-phase C18 silica gel (Merck, Germany) and Sephadex LH-20 (Pharmacia Biotec AB, Sweden). The solvents used in column chromatography and high-performance liquid chromatography (HPLC) were of analytical (Shanghai, P.R. China) grade and chromatographic grade (Fisher Scientific, USA), respectively.
6
Spectroscopic Analysis of Novel Compounds
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Optical rotations were recorded on a JASCO P-1030 automatic digital polarimeter, and UV spectra were recorded with a JASCO V-550 UV/VIS spectrophotometer. IR spectra were determined using a JASCO FT/IR-480 plus FT-IR spectrometer. HRESIMS data were determined by an Agilent 6210 ESI/TOF mass spectrometer. NMR spectra were obtained by a Bruker AV-400 spectrometer with TMS as an internal standard. Preparative HPLC was performed using a Varian chromatograph equipped with a C18 reversed-phase column (Cosmosil, 5 µm, 10 mm × 250 mm). Analytical HPLC was performed using a Waters chromatograph equipped with a C18 reversed phase column (Cosmosil, 5 µm, 4.6 mm × 250 mm). Silica gel (200–300 mesh; Qingdao Marine Chemical, Inc.), ODS silica gel (50 µm; YMC), and Sephadex LH-20 (Pharmacia) were used for column chromatography experiments. Silica gel GF254 plates (Yantai Chemical Industry Research Institute, Yantai, China) were used for thin-layer chromatography (TLC).
7
NMR, IR, and Spectroscopic Analysis of Pyrazolone Derivatives
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1H and 13C{1H} NMR spectra were recorded on a Bruker 400 MHz NMR
spectrometer with CDCl3 as the solvent and TMS as the internal
standard. IR spectra were recorded on a Thermo fisher Nicolet 6700
spectrometer. HRMS spectra were obtained using the Agilent 6210 ESI/TOF
mass spectrometer. Determination of copper content was performed using
atomic absorption spectroscopy (Agilent 240FS AA). TLC was performed
using commercially available 100–400 mesh silica gel plates
(GF254), and visualization was effected at 254 nm. Column
chromatography was carried out on silica gel (200–300 mesh).
All commercially available reagents were used as received. Pyrazolone1b–1v were synthesized by literature procedures.5b ,7a ,8b
spectrometer with CDCl3 as the solvent and TMS as the internal
standard. IR spectra were recorded on a Thermo fisher Nicolet 6700
spectrometer. HRMS spectra were obtained using the Agilent 6210 ESI/TOF
mass spectrometer. Determination of copper content was performed using
atomic absorption spectroscopy (Agilent 240FS AA). TLC was performed
using commercially available 100–400 mesh silica gel plates
(GF254), and visualization was effected at 254 nm. Column
chromatography was carried out on silica gel (200–300 mesh).
All commercially available reagents were used as received. Pyrazolone
8
Spectroscopic Characterization of Natural Products
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NMR spectra were scanned using a Bruker AV-500 spectrometer with TMS as the internal standard. HRESIMS data were determined using an Agilent 6210 ESI/TOF mass spectrometer. For column chromatography (CC), ODS (50 μm, YMC, Kyoto, Japan), silica gel (200–300 mesh, Qingdao Marine Chemical Plant, Qingdao, P. R. China), and Sephadex LH-20 (Pharmacia Biotech, Uppsala, Sweden) were used. Thin-layer chromatography (TLC) was carried out by using silica gel GF254 plates (Yantai Chemical Industry Research Institute, Yantai, China). Analytical HPLC was performed with A Waters system (e2695 Separations Module, 2998 Photodiode Array Detector) and a Cosmosil C18 analytical column (5 μm, 4.6 × 250 mm). An Agilent 1100 LC series with a diode array detector (DAD) using a preparative Cosmosil C18 column (20 × 250 mm, 5 μm) was applied for preparative HPLC. HPLC separations were performed using a COSMOSIL C18 preparative column (5 μm, 20 × 250 mm). All chemical reagents were purchased from Tianjin Damao Chemical Company (Tianjin, P. R. China).
9
Synthesis and Characterization of BODIPY Derivatives
10
Spectroscopic Analysis of Organic Compounds
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UV and IR spectra were obtained on a JASCO V-550 spectrophotometer and a JASCO FI/IR-480 Plus Fourier transform infrared spectrometer, respectively. CD spectra were recorded on a Chirascan spectropolarimeter. Optical rotations were determined with a JASCO P-1020 Automatic Polarimeter. HR-ESI-MS data were obtained using an Agilent 6210 ESI/TOF mass spectrometer. NMR experiments were performed on Bruker AV-600 and AV-400 spectrometers. HPLC was carried out on an Agilent 1260 chromatograph and a semi-preparative chromatograph with a DAD detector.
Column chromatography (CC) was performed on silica gel (60–80 mesh, 200–300 mesh, Qingdao Marine Chemical Inc., Qingdao, China), Sephadex LH-20 (Pharmacia Biotech AB), and YMC-Pack ODS (Merck). TLC was carried out on glass precoated silica gel GF254 plates. Waters X-bridge C18 column (250 × 4.6 mm, 5 μm; 250 × 10 mm, 5 μm) was used to analyze and isolate the compounds.
Column chromatography (CC) was performed on silica gel (60–80 mesh, 200–300 mesh, Qingdao Marine Chemical Inc., Qingdao, China), Sephadex LH-20 (Pharmacia Biotech AB), and YMC-Pack ODS (Merck). TLC was carried out on glass precoated silica gel GF254 plates. Waters X-bridge C18 column (250 × 4.6 mm, 5 μm; 250 × 10 mm, 5 μm) was used to analyze and isolate the compounds.
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