Dpx 300 spectrometer

Manufactured by Bruker

Sourced in United States, Germany, Australia

The DPX-300 spectrometer is a nuclear magnetic resonance (NMR) instrument manufactured by Bruker. It is designed to perform high-resolution NMR spectroscopy analysis. The DPX-300 operates at a 1H frequency of 300 MHz and is capable of analyzing a variety of sample types.

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Lab products found in correlation

Cary 100 spectrophotometer, by Agilent Technologies (2 mentions) Ltq orbitrap xl, by Thermo Fisher Scientific (2 mentions) Avatar series ft ir spectrophotometer, by Thermo Fisher Scientific (2 mentions) Kbr disks, by Thermo Fisher Scientific (2 mentions) 341 polarimeter, by PerkinElmer (2 mentions) Cdcl3, by Cambridge Isotopes (2 mentions) Ultrotof q instrument, by Bruker (2 mentions) Sephadex lh 20, by Cytiva (2 mentions) Silica gel 60, by Merck Group (2 mentions) Microtof spectrometer, by Bruker (2 mentions) Tensor 27 ftir spectrometer, by Bruker (2 mentions) Agilent 6460 triple quad lc ms system, by Agilent Technologies (2 mentions) Cd3od, by Cambridge Isotopes (2 mentions) Topspin 4, by Bruker (2 mentions) Oxalyl chloride, by Thermo Fisher Scientific (1 mentions) Propionic acid, by Merck Group (1 mentions) D luciferin sodium salt, by Abcam (1 mentions) Hexanoic acid, by Merck Group (1 mentions) 1 2 distearoyl sn glycero 3 phosphocholine, by Avanti Polar Lipids (1 mentions) Phosphatidyl choline from, by Avanti Polar Lipids (1 mentions)

45 protocols using dpx 300 spectrometer

Purification and Characterization of Organic Compounds

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All solvents were dried prior to
use according to known procedures; all reagents were obtained from
commercial sources or were synthesized from literature procedures
and were used without further purification unless otherwise noted.
Air-sensitive reactions were performed under slight positive pressure
of nitrogen. Room temperature is assumed to be between 20 and 25 °C.
Evaporation of solvents was accomplished under reduced pressure at
less than 40 °C, unless otherwise noted. Melting points were
taken on a Mel-Temp apparatus and are uncorrected. Chromatography
solvent systems are expressed in v:v ratios or as % v. CMA80 refers
to a solution of CHCl₃–MeOH NH₄OH−aq
(80:18:2). Thin layer chromatography was performed on aluminum oxide
IB-F plated from J. T. Baker (Phillipsburg, NJ) or silica gel 60 F₂₅₄ plates from EMD (Gibbstown, NJ). Chromatograms were visualized
under UV light at 254 nm. ¹H NMR spectra were obtained
at 300 MHz on a Bruker DPX300 spectrometer. ¹³C NMR spectra
were obtained at 75 MHz on a Bruker DPX300 spectrometer. Chemical
shift values for ¹H were determined relative to an internal
tetramethylsilane standard (0.00 ppm). Chemical shift values for ¹³C were determined relative to solvent (CDCl₃ =
77.23 ppm). Elemental analyses were performed by Atlantic Microlabs,
Norcross, GA. Purity of compounds (>95%) was established by elemental
analysis.

Kormos C.M., Cueva J.P., Gichinga M.G., Runyon S.P., Thomas J.B., Brieaddy L.E., Mascarella S.W., Gilmour B.P., Navarro H.A, & Carroll F.I. (2014). Effect of the 3- and 4-Methyl Groups on the Opioid Receptor Properties of N-Substituted trans-3,4-Dimethyl-4-(3-hydroxyphenyl)piperidines. Journal of Medicinal Chemistry, 57(7), 3140-3147.

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General Synthetic Protocols and Analytical Methods

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All solvents were dried prior to use according to known procedures; all reagents were obtained from commercial sources or were synthesized from literature procedures, and were used without further purification unless otherwise noted. Air-sensitive reactions were performed under slight positive pressure of nitrogen. Room temperature is assumed to be between 20 and 25 °C. Evaporation of solvents was accomplished under reduced pressure at less than 40 °C, unless otherwise noted. Melting points were taken on a Mel-Temp apparatus and are uncorrected. Chromatography solvent systems are expressed in v:v ratios or as %v. CMA80 refers to a solution of CHCl₃–MeOH NH₄OH–aq (80:18:2). Thin layer chromatography was performed on aluminum oxide IB-F plated from J. T. Baker (Phillipsburg, NJ) or silica gel 60 F₂₅₄ plates from EMD (Gibbstown, NJ). Chromatograms were visualized under UV light at 254 nm. ¹H NMR spectra were obtained at 300 MHz on a Bruker DPX300 spectrometer; ¹³C NMR spectra were obtained at 75 MHz on a Bruker DPX300 spectrometer. Chemical shift values for ¹H determined relative to an internal tetramethylsilane standard (0.00 ppm); chemical shift values for ¹³C determined relative to solvent (CDCl₃ = 77.23 ppm). Elemental analyses were performed by Atlantic Microlabs, Norcross, GA. Purity of compounds (>95%) was established by elemental analysis.

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Synthesis and Characterization of Lipid Derivatives

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The 2,4-Dinitrophenol (2,4-DNP), N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide (EDC), 4-(Dimethylamino)pyridine (DMAP), N,N-Dimethylformamide (DMF, ACS reagent grade), Palmitic acid, Hexanoic acid, Propionic acid were purchased from Merck Sigma-Aldrich (Saint Louis, MO, USA). Oxalyl chloride was purchased from Acros Organics (Geel, Belgium). Phosphatidyl choline from chicken egg (eggPC), 1,2-distearoyl-sn-glycero-3-phosphocholine (DSPC), 1,2-distearoyl-sn-glycero-3-phosphoethanolamine-N-methoxy(polyethylene glycol)-2000 (DSPE-PEG-OMe) were purchased from Avanti Polar Lipids (Alabaster, AL, USA). D-Luciferin sodium salt was purchased from BioVision Inc (Milpitas, CA, USA).
¹H and ¹³C NMR spectra were registered using Bruker DPX 300 spectrometers in CDCl₃. Signals of residual ¹H and ¹³C nuclei were used for scale calibration. Preparative column chromatography was performed using Merck 40/60 430 silica gel sorbent.

Vlasova K.Y., Ostroverkhov P., Vedenyapina D., Yakimova T., Trusova A., Lomakina G.Y., Vodopyanov S.S., Grin M., Klyachko N., Chekhonin V, & Abakumov M. (2022). Liposomal Form of 2,4-Dinitrophenol Lipophilic Derivatives as a Promising Therapeutic Agent for ATP Synthesis Inhibition. Nanomaterials, 12(13), 2162.

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NMR Characterization of Compounds

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The samples were characterized by nuclear magnetic resonance using Bruker DPX-300 spectrometers. ¹H and ¹³C NMR spectra were measured at 300 MHz. Chemical shifts are expressed in ppm, downfield from Me₄Si (TMS), used as internal standard.

Benisvy-Aharonovich E., Zandany A., Saady A., Kinel-Tahan Y., Yehoshua Y, & Gedanken A. (2020). An efficient method to produce 1,4-pentanediol from the biomass of the algae Chlorella ohadi with levulinic acid as intermediate. Bioresource Technology Reports, 11, 100514.

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Spectroscopic Analysis of Compounds

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All NMR spectra were measured on an Agilent VNS-600 spectrometer or on a Bruker DPX 300 spectrometer operating at 600 or 300 MHz for ¹H-NMR and 150 or 75 MHz for ¹³C-NMR in DMSO-d₆ using TMS as an internal standard. EIMS was measured on a Hewlett Packard model 5989B GC/ MS spectrometer. HPLC (Agilent 1200 series system) composed of vacuum degasser, quaternary pump, diode array detector (DAD), manual injector, thermostatted column compartment using a Luna C18(2) 100A column (4.6×250 mm 5 μm, Phenomenex) was used for isolation and purification of compounds. Silica gels (70–230 mesh, Merck, Darmstadt, Germany), Sephadex LH-20 (GE Healthcare, Uppsala, Sweden) were used for open column chromatography. TLC was performed on silica gel 60 F₂₅₄ (Merck).

Suh W., Nam G., Yang W.S., Sung G.H., Shim S.H, & Cho J.Y. (2016). Chemical Constituents Identified from Fruit Body of Cordyceps bassiana and Their Anti-Inflammatory Activity. Biomolecules & Therapeutics, 25(2), 165-170.

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NMR Spectroscopy and UPLC-MS Analysis

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Reagents and solvents
were obtained from Fluka, Sigma-Aldrich or Bachem, and were used without
further purification. NMR spectra in either CDCl₃, DMSO-d₆ or D₂O solution were recorded on
a Bruker DPX 300 spectrometer (300 MHz) or on a Bruker Avance 400
spectrometer (400 MHz); chemical shifts δ_H are reported
in ppm with reference to the solvent resonance (CDCl₃:
δ_H = 7.26 ppm; DMSO: δ_H = 2.50 ppm;
H₂O: δ_H = 4.79 ppm); coupling constants
J are reported in Hz. UHPLC analyses were carried out on a Thermo
Scientific Dionex UltiMate 3000 Standard system including an autosampler
unit, a thermostated column compartment and a photodiode array detector,
using UV absorbance detection at λ = 273 nm. HPLC/ESI-MS analyses
were carried out on a Waters UPLC Acquity H-Class system including
a photodiode array detector (acquisition in the 200–400 nm
range), coupled to a Waters Synapt G2-S mass spectrometer, with capillary
and cone voltage of 30 kV and 30 V, respectively, source and desolvation
temperature of 140 and 450 °C, respectively. ESI⁺ and
ESI^– refer to electrospray ionization in positive
and negative mode, respectively. HRMS spectra were recorded on the
same spectrometer, using the same source settings as above.

Pressman A.D., Liu Z., Janzen E., Blanco C., Müller U.F., Joyce G.F., Pascal R, & Chen I.A. (2019). Mapping a Systematic Ribozyme Fitness Landscape Reveals a Frustrated Evolutionary Network for Self-Aminoacylating RNA. Journal of the American Chemical Society, 141(15), 6213-6223.

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Synthesis of Nitrogen-Containing Heterocycles

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All reactions were performed under an N₂ atmosphere. Unless otherwise stated, all reagents were purchased from commercial suppliers and used without further purification. Organic solvents were concentrated under reduced pressure using a rotary evaporator or oil pump. Flash column chromatography was performed using Qingdao Haiyang flash silica gel (200–300 mesh). Meting points were measured on a Yanagimoto apparatus and uncorrected. Infrared spectra were recorded using a Shimadzu IR-435 instrument with KBr plates. ¹H- and ¹³C-NMR spectra were obtained on Bruker DPX 300 spectrometer (Bruker Biospin Co., Stuttgart, Germany) with CDCl₃ as the solvent and TMS as the internal standard. HR-MS were obtained on a Brüker Apex II mass spectrometer using nitrobenzoyl alcohol and sodium chloride as matrix (ThermoFisher scientific Inc., Waltham, MA, USA).

Wang R., Liu G., Yang M., Wang M, & Zhou L. (2016). Total Synthesis and Antifungal Activity of Palmarumycin CP17 and Its Methoxy Analogues. Molecules, 21(5), 600.

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NMR and Mass Spectrometry Analysis

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NMR experiments were recorded at ICB-NMR Service Centre on a DRX 600 MHz Bruker spectrometer equipped with a TXI CryoProbe™, on a Bruker Avance-400 spectrometer using an inverse probe fitted with a gradient along the z-axis, and on a Bruker DPX-300 spectrometer. The NMR spectra were acquired in CDCl₃ and in CD₃OD. ESIMS and HRESIMS spectra were measured on a Micromass Q-TOF Microspectrometer coupled with HPLC Waters Alliance 2695. The instrument was calibrated by using a PEG mixture from 200 to 1000 MW. Optical rotations were measured using a Jasco DIP 370 digital spectropolarimeter. Analytical and preparative TLC were performed on precoated silica gel plates (Merck Kieselgel 60 F254, 0.2 mm and 0.5 mm), with detection provided by UV light (254 nm) and by spraying with ceric sulfate (CeSO₄) reagent followed by heating (120°C). Silica gel column chromatography was performed using Merck Kieselgel 60 powder whereas size-exclusion chromatography was achieved on Sephadex LH-20 column.

BenRedjem Romdhane Y., Elbour M., Carbone M., Ciavatta M.L., Gavagnin M., Mathieu V., Lefranc F., Ktari L., Ben Mustapha K., Boudabous A., Kiss R, & Mollo E. (2016). In Vitro Growth Inhibitory Activities of Natural Products from Irciniid Sponges against Cancer Cells: A Comparative Study. BioMed Research International, 2016, 5318176.

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Characterization of SWCNT-Based Drug Delivery System

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FTIR spectra were recorded on a Nicolet iS10 spectrometer (Thermo Fisher Scientific, Waltham, MA, USA) and ¹HNMR spectrum was obtained on a Bruker DPX 300 spectrometer. Moreover, the morphology of SWCNTs, SWCNTs-HA, SWCNTs-HA-ss-DOX, and SWCNTs-HA-DOX were characterized by TEM and hyperspectral microscopy, respectively. The DOX content in the SWCNTs-HA-ss-DOX was determined by fluorescence measurement. Briefly, 0.25 mg/mL of SWCNTs-HA-ss-DOX solution was mixed with 10 mM of dithiothreitol in the nitrogen. After stirring for 4 hours, the resulting solution was ultrafiltered and detected using fluorospectrophotometer with the wavelength of excitation at 480 nm and emission at 557 nm. For SWCNTs-HA-DOX, the content of DOX was also estimated by fluorescence measurement based on a standard curve generated with known concentrations of DOX in ethanol.

Hou L., Yang X., Ren J., Wang Y., Zhang H., Feng Q., Shi Y., Shan X., Yuan Y, & Zhang Z. (2016). A novel redox-sensitive system based on single-walled carbon nanotubes for chemo-photothermal therapy and magnetic resonance imaging. International Journal of Nanomedicine, 11, 607-624.

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Synthetic Organic Characterization Methods

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Commercially available reagents were purchased from Fluka (Sydney, NSW, Australia), Aldrich (Sydney, NSW, Australia), Acros Organics (Morris Plains, NJ, USA), Alfa Aesar (Lancashire, UK) and Lancaster (Lancashire, UK) and purified if necessary. The synthetic procedures have been reported for all compounds as general methods and appropriate references have been given for known compounds. ¹H (300 MHz) and ¹³C-NMR (75 MHz) spectra were obtained in the designated solvents on a DPX 300 spectrometer (Bruker, Sydney, NSW, Australia). Melting points were measured using a Mel-Temp melting point apparatus and are uncorrected. Infrared spectra were recorded on Avatar Series FT-IR spectrophotometer as KBr disks (Thermo Nicolet, Waltham, MA, USA). Ultraviolet spectra were measured using a Cary 100 spectrophotometer (Varian, Santa Clara, CA, USA) in the designated solvents and data reported as wavelength (λ) in nm and adsorption coefficient (ε) in cm⁻¹M⁻¹. High-resolution [ESI] mass spectra were recorded by the UNSW Bioanalytical Mass Spectrometry Facility, on an Orbitrap LTQ XL (Thermo Scientific, Waltham, MA, USA) ion trap mass spectrometer using a nanospray (nano-electrospray) ionization source.

Bingul M., Arndt G.M., Marshall G.M., Cheung B.B., Kumar N, & Black D.S. (2020). Synthesis, Characterization and Biological Evaluation of Novel Dihydropyranoindoles Improving the Anticancer Effects of HDAC Inhibitors. Molecules, 25(6), 1377.

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