Dehydroepiandrosterone, NBS, hydrazine hydrate, phloxine B, isocyanate, isothiocyanate substituents and other regents were purchased from Energy Chemical (Shanghai) Co. Ltd. China. All regents and solvent (analytical grade) used without further purification. 1H-NMR (600 MHz) and 13C-NMR (150 MHz) were recorded on a Bruker Avance DRX400 instrument (Bruker, Karlsruhe, Germany), using tetramethylsilane (TMS) as internal standards. Melting points (mp) were determined on an MP120 auto melting point apparatus (Haineng, Jinan, China). Mass spectra (ESI) of all compounds were recorded on Esquire 6000 mass spectrometer (Bruker, Karlsruhe, Germany). Flash chromatography was performed using 400 mesh silica gel.
Esquire 6000 mass spectrometer
Manufactured by Bruker
Sourced in Germany
The Esquire 6000 is a mass spectrometer designed for accurate mass analysis. It utilizes an ion trap technology to capture and analyze ionic species. The Esquire 6000 provides high-sensitivity detection and precise mass measurement capabilities for a variety of analytical applications.
Automatically generated - may contain errors
Lab products found in correlation
Avance drx 400, by Bruker (1 mentions)
Hydrazine hydrate, by Energy Chemical (1 mentions)
Agilent 6230 tof mass spectrometer, by Agilent Technologies (1 mentions)
Smart apex 2 ccd diffractometer, by Bruker (1 mentions)
Av 400 nmr spectrometer, by Bruker (1 mentions)
Sep pak cartridges, by Waters Corporation (1 mentions)
6 protocols using esquire 6000 mass spectrometer
1
Synthesis and Characterization of Novel Compounds
2
Glutathione Redox States Analysis by ESI-MS
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Electron spray ionization (ESI) mass spectra were obtained on an Esquire 6000 mass spectrometer (Bruker). Full mass spectra of the investigated GSH and GSSG were acquired in both negative-ion and positive-ion mode with the spectrometer equipped with an ion-trap analyser. Two samples of 10 μl treated for the same time were pooled and diluted tenfold with acetonitrile-water (50:50) for 200 μl with a final concentration of 1 mg/ml. Instrumental parameters were tuned for each sample with GSH or GSSG. The capillary voltage was set in a range of −22 to 25 V, the spray voltage was between 3.00 and 4.50 kV, and a capillary temperature of 180 ºC was employed. The mass scan range was from m/z 50 to 2000 amu, for 20 s scan time. Spectra were acquired using a direct infusion setup with a flow rate of 5 μl/min with a cone voltage of 20 kV. To determine occurring in-source fragments, which increase the sample complexity without yielding significant additional information, MS/MS spectra of both GSH and GSSG were acquired using the same conditions with a collision energy ramp between 2.00 and 4.00 eV. Spectra were deconvoluted and a background of ten times noise (500 counts in positive and 5 counts in negative mode) was subtracted before peak annotation. All experiments were performed in duplicates.
3
ESI-MS Analysis of Organometallic Compounds
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Electron spray ionization (ESI) mass spectra were obtained on an Esquire 6000 mass spectrometer (Bruker). Full mass spectra of the investigated ferrocenecarboxylic acid, iron(III) acetylacetonate (Fe(acac)3), chloro(protoporphyrinato)iron(III) (hemin), GSH and GSSG were acquired in both negative-ion and positive-ion mode with the spectrometer equipped with an ion-trap analyser. Three samples of 10 μl treated for the same time were pooled and diluted tenfold with acetonitrile for 300 μl with a final concentration of 1 mg/ml. Instrumental parameters were tuned for each sample. The capillary voltage was set in a range of −22 to 25 V, the spray voltage was between 3.00 and 4.50 kV, and a capillary temperature of 180 °C was employed. The mass scan range was from m/z 50 to 2000 amu, for 20 s scan time. Spectra were acquired using a direct infusion setup with a flow rate of 5 μl/min with a cone voltage of 20 kV. To determine occurring in-source fragments, which increase the sample complexity without yielding significant additional information, MS/MS spectra were acquired using the same conditions with a collision energy ramp between 2.00 and 4.00 eV. Spectra were deconvoluted and a background of ten times noise (500 counts in positive and 5 counts in negative mode) was subtracted before peak annotation. All experiments were performed in triplicates.
4
Synthesis of Amino Acid-DBE Substrates
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Amino acid-DBE substrates
(3,5-dinitrobenzyl esters of amino acids) were synthesized as reported
previously19 (link) with the following modification. N-Boc-protected amino acid DBE-esters were deprotected in
2 mL of neat TFA for 10 min, followed by washing with 10 mL of 3×
diethyl ether. Products were obtained as TFA salts. TFA salts were
dissolved in 100% DMSO to a final concentration of 25 mM and used
in reactions directly. 1H NMR spectra were recorded using
a 400 MHz NMR spectrometer (Varian INOVA) operating at 400 MHz. Low-resolution
mass spectrometry was performed by directly injecting 10 μL
of a 2 mg/mL solution in 1:1 acetonitrile/water mixture on an Esquire
6000 mass spectrometer (Bruker Daltonics). High-resolution mass spectrometry
was performed by injecting 500 pmol of material dissolved in water
on an Agilent 1200 HPLC instrument coupled to an Agilent 6230 TOF
mass spectrometer.
(3,5-dinitrobenzyl esters of amino acids) were synthesized as reported
previously19 (link) with the following modification. N-Boc-protected amino acid DBE-esters were deprotected in
2 mL of neat TFA for 10 min, followed by washing with 10 mL of 3×
diethyl ether. Products were obtained as TFA salts. TFA salts were
dissolved in 100% DMSO to a final concentration of 25 mM and used
in reactions directly. 1H NMR spectra were recorded using
a 400 MHz NMR spectrometer (Varian INOVA) operating at 400 MHz. Low-resolution
mass spectrometry was performed by directly injecting 10 μL
of a 2 mg/mL solution in 1:1 acetonitrile/water mixture on an Esquire
6000 mass spectrometer (Bruker Daltonics). High-resolution mass spectrometry
was performed by injecting 500 pmol of material dissolved in water
on an Agilent 1200 HPLC instrument coupled to an Agilent 6230 TOF
mass spectrometer.
5
Synthetic and Analytical Methods for Metal Complex
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Solvents and starting materials for syntheses were purchased commercially and used as received. Elemental analyses were carried out on an Elemental Vario EL analyzer. 1H NMR spectra are recorded on a Bruker AV400 NMR spectrometer in DMSO-d6 solution. The UV spectra were recorded on a Purkinje General TU-1800 spectrophotometer. Fluorescence spectra were determined on a Varian CARY Eclipse spectrophotometer. ESI-MS spectra were obtained on a Bruker Daltonics Esquire 6000 mass spectrometer. Fluorescent images were taken on a Zeiss Leica inverted epifluorescence/reflectance laser scanning confocal microscope. The X-ray diffraction measurement for 1·0.5H2O was performed on a Bruker SMART APEX II CCD diffractometer equipped with a graphite monochromatized MoKα radiation (λ = 0.71073 Å) by using ϕ-ω scan mode. Semi-empirical absorption correction was applied to the intensity data using the SADABS program.31 The structure was solved by direct methods and refined by full matrix least-square on F2 using the SHELXTL-97 program.32 All non-hydrogen atoms were refined anisotropically. All H atoms were positioned geometrically and refined using a riding model.
6
HPLC-MS Analysis of Tanacetum parthenium Extracts
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The aqueous extract was analyzed by Aligent Technologies 1200 Series HPLC, utilizing a Millennium Chromatography Manager (464) system, with an Ultraviolet (UV) Detector of Diode (DAD) rearrangement (Waters 2996). Reverse-phase separation was conducted at room temperature, employing a Synergi Polar-RP 80A 150×2.00 mm I.D., with a 4 -µm particle size. The column was eluted at a flow-rate of 0.2 mL/min, in gradient mode, with mixtures of MeOH/H 2 O (3:97; 5 min), MeOH/H 2 O (80:20; 40 min), and H 2 O (5 min), for a total runtime of 50 min. Elution was monitored at 220 and 254 nm. HPLC was coupled to a Bruker Daltonics Esquire 6000 mass spectrometer.
An aliquot of the aqueous extract was filtered through C18 Waters Sep-Pak ® cartridges. Three fractions were obtained and injected into the HPLC system. Santin [1] and santamarin [2] were previously isolated from organic extracts of Tanacetum parthenium and served as standards. HPLC peaks were not corrected for response factors and are reported as relative percentage of the area (Estrada-Reyes et al., 2010) . The identity and purity of the standards were confirmed by their physical and chemical properties and their spectral data ( 1 H and 13 C Nuclear Magnetic Resonance [NMR] and MS), by means of comparison with results described in the literature.
An aliquot of the aqueous extract was filtered through C18 Waters Sep-Pak ® cartridges. Three fractions were obtained and injected into the HPLC system. Santin [1] and santamarin [2] were previously isolated from organic extracts of Tanacetum parthenium and served as standards. HPLC peaks were not corrected for response factors and are reported as relative percentage of the area (Estrada-Reyes et al., 2010) . The identity and purity of the standards were confirmed by their physical and chemical properties and their spectral data ( 1 H and 13 C Nuclear Magnetic Resonance [NMR] and MS), by means of comparison with results described in the literature.
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