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Lc it tof

Manufactured by Shimadzu
Sourced in Japan

The LC-IT-TOF is a liquid chromatography-ion trap-time-of-flight mass spectrometer, designed for high-performance analytical applications. It combines the separation capabilities of liquid chromatography with the high mass accuracy and resolving power of time-of-flight mass analysis.

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4 protocols using lc it tof

1

Mass Spectrometric Analysis of Biomolecules

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Mass spectrometric measurements (MS and MS/MS) were performed on an ESI-FT-ICR Apex-Qe 7T instrument (Bruker). The potential between the spray needle and the orifice was set to 4.5 kV. MS and MS/MS spectra an acetonitrile/water/formic acid (50:50:0.1) mixture or methanol were used. For fragmentation, the collision-induced dissociation (CID) technique was used with argon as the collision gas. The MS was calibrated with a Tunemix mixture (Bruker Daltonics).
MS and MS/MS experiment was also performed on a Shimadzu LC-IT-TOF instrument. CID fragmentation (with Argon) was used in the instrument, and the potential between the spray needle and the orifice was set to 4.5 kV. The LC systems were operated with the following mobile phases: A = 0.1% HCOOH in H2O and B = 0.1% HCOOH in MeCN. MS spectra were recorded without the LC column installation.
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2

Analytical Techniques for Compound Identification

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The NMR data were recorded on a Bruker 500 and 600 MHz spectrometer (Bruker, Germany). IR spectra were recorded with KBr disks by a Bruker vertex-70 spectrometer (Bruker, Germany). A high-resolution mass spectrum was acquired via Shimadzu LC-IT-TOF (Shimadzu, Japan). MPLC separation was performed on a Büchi sepacore (Buchi Labortechnik AG, Flawil, Swizerland) with YMC gel ODS C18 column (45–60 μm, YMC Co., Ltd., Kyoto, Japan). Column chromatography (CC) was carried out using silica gel (200–300 mesh, Qingdao Marine Chemical Co., Ltd., Qingdao, China) and Sephadex LH-20 (GE Healthcare Bio-Sciences AB, Uppsala, Sweden). Thin-layer chromatography (TLC) was undertaken on HSGF254 plates (Qingdao Marine Chemical Co., Ltd., China). Semi-preparative HPLC was conducted on an LC-3000 semi-preparation gradient HPLC system (Chuangxintongheng, Beijing, China), equipped with a UV–vis detector and a semipreparative RP-HPLC column (Shiseido CAPCELL PAK C18 column, 250 × 20 mm, 5 μm, Japan). ACN (HPLC grade) (CINC High Purity Solvents, Shanghai, China). Methanol, acetone, petroleum ether (60–90), ethyl acetate (AR) (Sinopharm Co., Ltd., Shanghai, China), ultrapure water was produced by a Milli-Q water purification system (Milford, MA, USA).
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3

Characterization of Organic Compounds

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All reagents were used as purchased from commercial sources (Sigma-Aldrich, Acros Organics, Vetec or Fluka). Progress of the reactions was followed by thin-layer chromatography (silica gel 60 F 254 in aluminum foil). Chemical identity was confirmed by NMR and IR spectroscopy and accurate mass. IR was determined in KBr pellets. For NMR, we used a Varian Unity Plus 400 MHz (400 MHz for 1 H and 100 MHz for 13 C) and Bruker AMX-300 MHz (300 MHz for 1 H and 75.5 MHz for 13 C) instruments. DMSO-d 6 and CDCl 3 -d 6 were purchased from CIL or Sigma-Aldrich. Chemical shifts are reported by ppm and multiplicities are given as: s (singlet), d (doublet), t (triplet),q (quartet), m (multiplet) integration, and coupling constants (J) in hertz. Structural assignments corroborated by DEPT experiments. Mass spectrometry experiments were performed on a Q-TOF spectrometer (nanoUPLC-Xevo G2 Tof, Waters) or LC-IT-TOF (Shimadzu). When otherwise specified, ESI was carried out in the positive ion mode. Typical conditions were: capillary voltage of 3 kV and cone voltage of 30 V, and peak scan between 50 and 1000 m/z.
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4

Characterization of Organic Compounds via NMR and MS

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All reagents were used as purchased from commercial sources (Sigma-Aldrich, Acros Organics, Vetec or Fluka). Progress of the reactions was followed by thin-layer chromatography (silica gel 60 F254 in aluminum foil). IR was determined in KBr pellets. For NMR, it was used a Bruker AMX-300 MHz (300 MHz for 1 H and 75.5 MHz for 13 C) instrument. DMSOd 6 was purchased from CIL. Chemical shifts are reported in ppm, and multiplicities are given as s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet) and dd (doublet of doublets) and coupling constants (J) in hertz. NH signals were localized in each spectrum after the addition of a few drops of D 2 O. Structural assignments were corroborated by DEPT analysis. Mass spectrometry experiments were performed on a Q-TOF spectrometer LC-IT-TOF (Shimadzu). When otherwise specified, ESI was carried out in the positive ion mode. Reactions in an ultrasound bath were carried out under frequency of 40 kHz (180 W) and without external heating.
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