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Ltq orbitrap xl hybrid ion trap orbitrap

Manufactured by Thermo Fisher Scientific
Sourced in United States

The LTQ Orbitrap XL Hybrid Ion Trap-Orbitrap is a high-resolution, high-mass accuracy mass spectrometer that combines a linear ion trap and an Orbitrap mass analyzer. It provides accurate mass measurements and high-resolution data acquisition capabilities for a wide range of analytical applications.

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6 protocols using ltq orbitrap xl hybrid ion trap orbitrap

1

Spectroscopic Analysis and Chiral HPLC Characterization

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1H NMR and 13C NMR were recorded on a Bruker-400
MHz spectrometer (1H NMR: 400 MHz; 13C NMR:
100 MHz) using TMS as an internal
reference. The chemical shifts (δ) and coupling constants (J) were expressed in ppm and Hz, respectively. UV–Vis
spectrophotometry was carried out on a Shimadzu UV-3000. HPLC analysis
was carried out on an Agilent 1100 series HPLC with a multiple wavelength
detector. Chiralpak AS-H, AD-H, and OD-H columns were purchased from
Daicel Chemical Industries, Ltd. Optical rotations were measured on
a PerkinElmer polarimeter (model 343). HRMS (ESI) was recorded on
Waters Q-TOF Premier and Thermo Scientific LTQ Orbitrap XL Hybrid
Ion Trap-Orbitrap mass spectrometers. Commercially available compounds
were used without further purification. Solvents were purified according
to the standard procedures, unless otherwise noted. Commercial pyrrole
should be distilled for the use of the reactions. Ligands9d ,10b and various 2-enoyl-pyridine N-oxides 2(11 (link)) were prepared according to literature
procedures.
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2

Phosphorylated Sugar Synthesis by MS

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The aqueous solution of sugar and phosphoric acid was injected by a mechanical syringe pump through a hypodermic needle to the fused silica capillary directing toward an MS inlet. A coaxial sheath gas (dry N2 at 120 psi) flow around the capillary results in nebulization, and also helps to direct the spray emerging from the capillary tip toward the MS inlet (the flow rate of 5 μL/min through silica tubing). Two different voltages of 0 and +5 kV were applied to the hypodermic needle. At an MS inlet, the reactants, intermediates, and products are released from droplets by Coulomb fission and enter into the MS through a heated capillary. The capillary temperature was maintained at 275 °C and capillary voltage at 44 V. To confirm the identities of synthesized phosphorylated sugars, tandem mass spectrometry was conducted by CID. The spray distance (the distance from spray tip to the entrance of the heated capillary) was varied from 2 to 25 mm for monitoring the progression of reaction. For all other mass spectrometric analyses, the spray distance was kept at 25 mm. Mass spectra were detected by a high-resolution MS (LTQ Orbitrap XL Hybrid Ion Trap-Orbitrap; Thermo Scientific). All of the necessary chemicals were purchased from Sigma-Aldrich. HPLC-grade solvents were purchased from Fisher Scientific.
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3

Radiotracer Labeling of DTPA-Conjugated Sulfonamide

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For preparation of diethylene triamine pentaacetic acid (DTPA) labeled-sulfonamide (ATS-DTPA), ATS and DTPA dianhydride (w/w 1:50) was incubated at 25°C with bicarbonate buffer (pH 8.5) for 4 hours. Then, the conjugated-compounds were purified by high pressure liquid chromatography with G-10 column. For molecular weight assay, liquid chromatography-mass spectrometry (LTQ Orbitrap XL™ Hybrid Ion Trap-Orbitrap, Thermo Scientific, USA) was performed for ATS analysis. And matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (UltraflexIII TOF/TOF, Bruker Daltonics GmbH, Germany) was performed for DTPA and ATS-DTPA detection. Briefly, the compounds were crystallized with an equal volume of freshly prepared α-cyano-4-hydroxycinnamic acid matrix (10 mg/ml in 50% acetonitrile/0.5% TFA) for mass spectrometry analysis. The calibration standards were used as external calibrator with mass accuracy within 100 ppm. The spectra were processed using FlexAnalysis™ 3.0 software (Bruker, Germany). The ATS-DTPA conjugation efficiency with indium-111 was evaluated from the radiolabeling yields of ATS-DTPA-111In determined by instant thin layer chromatography (ITLC) (AR-2000 radio-TLC Imaging Scanner, Bioscan, France) on silica gel impregnated glass fiber sheets (PALL corporation, USA) using PBS buffer, pH 7.4, as the mobile phase.
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4

Mass Spectrometry of Ribonucleoside Synthesis

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The aqueous solution of 15 mM d-ribose, 15 mM phosphoric acid, and 5 mM nucleobases was injected with 3 mM magnesium sulfate by a mechanical syringe pump through a hypodermic needle to the fused silica capillary directing toward a mass spectrometer inlet. A coaxial sheath gas (dry N2 at 120 psi) flow around the capillary results in nebulization and also helps to direct the spray emerging from the capillary tip toward the mass spectrometer inlet (the flow rate of 5 μL/min through silica tubing). A positive voltage, +5 kV, was applied to the hypodermic needle. At a mass spectrometer inlet, the reactants, intermediates, and products are released from droplets by Coulomb fission and enter into the mass spectrometer through a heated capillary. The capillary temperature was maintained at 275 °C and the capillary voltage at 44 V. To confirm the identities of synthesized ribonucleosides, tandem MS was conducted by CID. For all mass spectrometric analyses, the spray distance (the distance from spray tip to the entrance of the heated capillary) was kept at 5 mm. Mass spectra were detected by high-resolution MS (Thermo Scientific LTQ Orbitrap XL Hybrid Ion Trap-Orbitrap). All of the necessary chemicals were purchased from Sigma-Aldrich. HPLC-grade solvents were purchased from Fisher Scientific.
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5

Chlorophyll Identification via Mass Spectrometry

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Stock solutions of chlorophyll a and b were prepared at 1 mM in methanol. Working solutions of chlorophylls at 40 μM were prepared by diluting the stock solution in methanol. HCl solution prepared at 70 mM concentration in water was mixed with the chlorophyll solutions at 1:1 (v/v) ratio with the final HCl concentration of 35 mM. The mixed solutions were gently stirred and incubated at room temperature for 20 min. Mass spectrometric analyses of the mixed solutions were carried out to determine the identities of the species present using an Orbitrap mass spectrometer (Thermo Scientific LTQ Orbitrap XL Hybrid Ion Trap-Orbitrap; Thermo Scientific, MA, USA).
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6

Chlorophyll Identification via Mass Spectrometry

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Stock solutions of chlorophyll a and b were prepared at 1 mM in methanol. Working solutions of chlorophylls at 40 μM were prepared by diluting the stock solution in methanol. HCl solution prepared at 70 mM concentration in water was mixed with the chlorophyll solutions at 1:1 (v/v) ratio with the final HCl concentration of 35 mM. The mixed solutions were gently stirred and incubated at room temperature for 20 min. Mass spectrometric analyses of the mixed solutions were carried out to determine the identities of the species present using an Orbitrap mass spectrometer (Thermo Scientific LTQ Orbitrap XL Hybrid Ion Trap-Orbitrap; Thermo Scientific, MA, USA).
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