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Vnmrs 500 nmr spectrometer

Manufactured by Agilent Technologies
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The VNMRS 500 NMR spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for analytical and research applications. It provides a 500 MHz magnetic field for the acquisition of NMR spectra, enabling the analysis of molecular structures and compositions.

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12 protocols using vnmrs 500 nmr spectrometer

1

High-Resolution Mass Spectrometry and NMR Analysis

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For high-resolution of the determination of the exact mass of different peaks, HR-QTOF ESI/MS was performed in positive ion mode using an ACQUITY (UPLC, Waters Corp., Milford, MA, USA) coupled with an SYNAPT G2-Si column (Waters Corp., Milford, MA, USA). The obtained mass data were subsequently analyzed by MassLynx version 4.1. NMR spectra were measured using a VNMRS 500 NMR spectrometer (Agilent Technology, Santa Clara, CA, USA) and residual solvent peaks (chloroform-d6 = δH 2.50) of deuterated NMR solvents (Sigma-Aldrich, St. Louis, MO, USA) were used as reference peaks.
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2

Analytical Techniques for Chemical Characterization

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Optical rotations and the UV spectrum were measured on a Model 343 polarimeter (PerkinElmer, Waltham, MA, USA) and a Lambda 35 UV/vis spectrophotometer (PerkinElmer, Waltham, MA, USA), respectively. 1H, 13C and 2D NMR spectral data were obtained in CDCl3 on a VNMRS 500 NMR spectrometer (Agilent Technologies, Santa Clara, CA, USA). Low-resolution ESI-MS were measured on an Agilent 1100 LC/MS system (Agilent Technologies, Santa Clara, CA, USA) with a Luna C18(2) 5-μm column (4.6 mm × 150 mm, flow rate 0.7 mL/min) (Phenomenex, Torrance, CA, USA). High-resolution mass spectral data were acquired on a JMS-AX505WA mass spectrometer (JEOL Ltd., Akishima-shi, Tokyo, Japan). A Lichroprep RP-18 (Merck, Darmstadt, Germany) was used for the flash column chromatography. Semipreparative HPLC separations were performed using a 321 HPLC system (Gilson Inc., Middleton, WI, USA) with a Luna C18(2) 10-μm column (10 × 250 mm) at a flow rate of 4 mL/min. A 1525 HPLC-PDA system (Waters, Milford, MA, USA) with a Luna C18(2) 5-μm column (4.6 mm × 150 mm) was used for the routine analysis of extracts and fractions. HPLC-grade solvents were used for all chromatographic analyses.
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3

High-Resolution Mass Spectrometry and NMR Analysis

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High-resolution quadrupole-time-of-flight electrospray ionization–mass spectrometry (HR-QTOF ESI/MS) analysis was performed in positive ion mode using an ACQUITY UPLC system coupled with a SYNAPT G2-Si column (Waters Corporation, Milford, MA, USA). NMR spectra were measured using a VNMRS 500 NMR spectrometer (Agilent Technology, Santa Clara, CA, USA), and residual solvent peaks (DMSO-d6 = δH 2.50) of deuterated NMR solvents (Sigma-Aldrich, St. Louis, MA, USA) were used as reference peaks.
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4

Synthesis of N-(6-methoxy-1,5-naphthyridin-4-yl)-4-piperidinecarboxamide

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Starting materials were purchased and used as received. Solvents were of reagent grade and distilled before use. N-(6-methoxy-1,5-naphthyridin-4-yl)-4-piperidinecarboxamide was prepared according to the literature (45 , 46 ). The melting point (uncorrected) was determined on a Boetius melting-point apparatus (VEB Kombinat NAGEMA, Dresden, GDR). 1H and 13C nuclear magnetic resonance (NMR) spectra were recorded at room temperature on an Agilent Technologies VNMRS 500 NMR spectrometer. The residual solvent signals of methanol-d41H = 3.31 ppm; δ13C = 49.00 ppm) were used to reference the spectra (abbreviations, s = singlet, d = doublet, t = triplet, q = quartet, td = triplet of doublets, m = multiplet). The mass spectrum was recorded on a Q Exactive Plus Orbitrap mass spectrometer (Thermo Scientific, Bremen, Germany) using methanol as solvent.
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5

LC-MS Analysis of Lipid Transport Proteins

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LC/MS analysis of LTP was confirmed in positive ion mode using Agilent 1260 Infinity II (Agilent, Santa Clara, CA, USA). Luna® C18(2) (2 mm × 100 mm, 3 μm particle size) columns were used for the analysis. 5 μL of LT and LTP were injected into the C18 column and eluted at a flow rate of 300 μL/min. The mobile phase was composed of solvent A (0.1% v/v formic acid in water) and B (acetonitrile) and increased from 10/90 to 5/95 over 12 min. The column temperature was maintained at 40 °C. The wavelength was measured at 254 nm. The spectrum used for NMR analysis was prepared from a VNMRS 500 NMR spectrometer (Agilent Technology, Santa Clara, CA, USA), and residual solvent peaks (DMSO-d6 = δH 2.50) of deuterated NMR solvent (Sigma-Aldrich, St. Louis, MO, USA) were used as a reference peak.
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6

Phorbas sp. Metabolite Isolation and Characterization

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A specimen of Phorbas sp. (voucher number 07G-26) was collected by hand from Gageo Island, South Korea, in 2007. Optical rotations were measured on a JASCO P-1010 polarimeter (Jasco, Easton, MD, USA). IR spectra were recorded using a JASCO FT/IR 4100 spectrometer (Jasco, Easton, MD, USA), and ultraviolet (UV) spectra using a Varian Cary 50 UV-Visible spectrophotometer (Agilent, Santa Clara, CA, USA). High-resolution (HR)-electrospray ionization (ESI) mass spectra were obtained using a SCIEX X500R mass spectrometer (Sciex, Framingham, MA, USA). The NMR spectra were recorded on a Varian VNMRS 500 NMR spectrometer (Varian, Palo Alto, CA, USA) operating at 500 (1H) or 125 MHz (13C), respectively, with chemical shifts given in ppm using a methanol-d4 solution concerning residual solvent peaks at 3.30 and 49.0 ppm. Semi-preparative liquid chromatography was performed using an Agilent 1200 pump (Agilent, Santa Clara, CA, USA) and an RI detector. Vacuum column chromatography was performed using RP-18 silica gel 60 (Merck, Darmstadt, Germany).
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7

Lanthanide Complex Synthesis and Characterization

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All air- and water sensitive procedures were carried out using standard Schlenk techniques. Deuterated NMR solvents were purchased from Cambridge Isotope Laboratories (MA) and used as received. Hexahydrates of GdCl3, YCl3, and EuCl3 were obtained from Alfa Aesar (REacton, Ward Hill, MA). Cyclen and DOTA were purchased from Strem Chemicals (Newburyport, MA). All other organic solvents and bulk inorganic reagents were purchased from EM Science (Gibbstown, NJ) and used as received, except where indicated. Distilled water was purchased from Arrowhead (Louisville, KY). Dionized water was generated from a PURELAB Ultra Mk2 water purifier (Elga). 1H T1 measurements were acquired on a Varian 400MR NMR Spectrometer at 9.4 T, or on a Bruker mq 60 NMR Analyzer at 1.4 T. 19F-NMR spectra were acquired on a Varian VNMRS 500 NMR Spectrometer at 11.7 T. Chemical shifts were referenced to residual solvent (1H) or C6F6 (19F).
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8

NMR Characterization of Chloroformic Extracts

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The 1H and 13C NMR analysis was performed by dissolving 10 mg of CLE in 0.7 mL of deuterated chloroform. The NMR spectra were acquired at 25 °C by a Varian VNMRS 500 NMR spectrometer (11.74 T) operating at 500 MHz for proton and 125 MHz for carbon, using 256 scans for proton and 16000 scans for carbon, interleaved by 7.7 s for proton and 2.05 s for carbon, with 45° pulses, employing a spectral width of 8012.8 Hz for proton and 31250 Hz for carbon over 32 K complex points. The signals were assigned according to the literature [5 (link),57 (link)].
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9

Chemical Characterization of AGE Derivatives

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S1PC and SAC were prepared from AGE as previously described12 (link). The chemical structures of compounds were determined by a LC-MS system consisting of an Ultimate 3000 and a Q-Exactive (Thermo Scientific, Waltham, MA, USA), and by a VNMRS-500 NMR spectrometer (VARIAN Inc., Palo Alto, CA, USA) at 500 MHz and 125 MHz. Cysteine derivatives were prepared according to previous report6 (link).
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10

Characterization of Deuterated Perovskite

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The synthesized CD3ND3PbI3 was characterized using 13C NMR spectroscopy obtained on a Varian VNMRS 500 NMR spectrometer at 23°C in dimethylformamide-d7 (DMF-d7), and inverse-gated decoupling with pw = 90 and a recycle delay of 60 s were used. The peaks around 164, 35, and 29 ppm are from the deuterated DMF-d7 solvent (see fig. S1). The peaks around 25 ppm are from the methyl carbon in CD3ND3 PbI3. The multiple splits of the peaks demonstrated the success of preparing deuterated perovskite, CD3ND3PbI3, because a proton-decoupled carbon spectrum will not remove coupling to deuterium and proton due to different spin (s = 1/2 for proton; s = 1 for deuterium). This is supported by the time-of-flight inelastic neutron scattering comparing both deuterated and protonated powders samples (Fig. 2), because there are no hydrogen peaks in the deuterated measurements. The inelastic scattering intensity, which scales as the neutron cross section divided by mass, is about 23 times stronger for H than for D, making a sensitive test for any hydrogen contamination in the deuterated material. From the neutron spectroscopy, we estimate that there is less than 0.00015 H per D in the deuterated crystal.
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