Lc msd system

Manufactured by Agilent Technologies

Sourced in United States

The Agilent LC/MSD system is a liquid chromatography-mass spectrometry (LC/MS) instrument designed for analytical applications. It combines liquid chromatography for sample separation and mass spectrometry for analyte detection and identification. The core function of the LC/MSD system is to provide sensitive and selective analysis of complex samples by separating, detecting, and identifying compounds of interest.

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Lab products found in correlation

500 mhz spectrometer, by Agilent Technologies (4 mentions) 400 mhz spectrometer, by Agilent Technologies (3 mentions) Prep lc4000 system, by Phenomenex (2 mentions) C18 column, by Phenomenex (2 mentions) 400 or 500 mhz spectrometers, by Agilent Technologies (1 mentions) Advance 300 mhz, by Bruker (1 mentions) Quadrupole mass spectrometer, by Agilent Technologies (1 mentions) Vydac c18 column, by Grace Bio-Labs (1 mentions) Esi interface, by Agilent Technologies (1 mentions)

8 protocols using lc msd system

NMR Spectroscopic and Purification Procedures

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¹H and ¹³C NMR data were
obtained on 400 or 500 MHz spectrometers (Varian) and are reported
in ppm relative to TMS and referenced to the solvent in which the
spectra were collected. Solvent was removed by rotary evaporation
under reduced pressure, and anhydrous solvents were obtained commercially
and used without further drying. Purification by CombiFlash silica
gel chromatography was performed using EtOAc–hexanes solvent
systems. Preparative high-pressure liquid chromatography (HPLC) was
conducted using a Waters Prep LC4000 system having photodiode array
detection and a Phenomenex C₁₈ column (Cat. No. 00G-4436-P0-AX,
250 × 21.2 mm 10 μm particle size, 110 Å pore) at
a flow rate of 10 mL/min. Binary solvent systems consisting of A =
0.1% aqueous TFA and B = 0.1% TFA in acetonitrile were employed with
gradients as indicated. Products were obtained as amorphous solids
following lyophilization. Electrospray ionization-mass spectrometric
(ESI-MS) was acquired with an Agilent LC/MSD system equipped with
a multimode ion source. Purities of samples subjected to biological
testing were assessed using this system and shown to be ≥95%.
High resolution mass spectra (HRMS) were acquired with a LTQ-Orbitrap-XL
at 30K resolution by LC/MS-ESI.

Smith S.J., Zhao X.Z., Passos D.O., Pye V.E., Cherepanov P., Lyumkis D., Burke TR J.r, & Hughes S.H. (2021). HIV-1 Integrase Inhibitors with Modifications That Affect Their Potencies against Drug Resistant Integrase Mutants. ACS Infectious Diseases, 7(6), 1469-1482.

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Detailed Nuclear Magnetic Resonance Analysis

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¹H and ¹³C
NMR data were obtained on a Varian 400 MHz spectrometer or a Varian
500 MHz spectrometer and are reported in ppm relative to TMS and referenced
to the solvent in which the spectra were collected. Solvent was removed
by rotary evaporation under reduced pressure, and anhydrous solvents
were obtained commercially and used without further drying. Purification
by silica gel chromatography was performed using CombiFlash R_f 200i with EtOAc–hexanes solvent systems. Preparative
high pressure liquid chromatography (HPLC) was conducted using a Waters
Prep LC4000 system having photodiode array detection and Phenomenex
C₁₈ columns (catalogue no. 00G-4436-P0-AX, 250 mm ×
21.2 mm 10 μm particle size, 110 Å pore) at a flow rate
of 10 mL/min. Binary solvent systems consisting of A = 0.1% aqueous
TFA and B = 0.1% TFA in acetonitrile were employed with gradients
as indicated. Products were obtained as amorphous solids following
lyophilization. Electrospray ionization–mass spectra (ESI-MS)
were acquired with an Agilent LC/MSD system equipped with a multimode
ion source. Purities of samples subjected to biological testing were
assessed using this system and shown to be ≥95%. High-resolution
mass spectra (HRMS) were acquired by LC/MS-ESI using an LTQ-Orbitrap-XL
at 30K resolution.

Zhao X.Z., Smith S.J., Métifiot M., Marchand C., Boyer P.L., Pommier Y., Hughes S.H, & Burke TR J.r. (2014). 4-Amino-1-hydroxy-2-oxo-1,8-naphthyridine-Containing Compounds Having High Potency against Raltegravir-Resistant Integrase Mutants of HIV-1. Journal of Medicinal Chemistry, 57(12), 5190-5202.

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NMR Spectroscopy and HPLC Purification

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Proton (¹H) and carbon
(¹³C) NMR spectra were recorded on a Varian 400 MHz spectrometer
or a Varian 500 MHz spectrometer and are reported in ppm relative
to TMS and referenced to the solvent in which the spectra were collected.
Solvent was removed by rotary evaporation under reduced pressure,
and anhydrous solvents were obtained commercially and used without
further drying. Purification by silica gel chromatography was performed
using Combiflash with EtOAc–hexanes solvent systems. Preparative
high pressure liquid chromatography (HPLC) was conducted using a Waters
Prep LC4000 system having photodiode array detection and Phenomenex
C₁₈ columns (catalogue no. 00G-4436-P0-AX, 250 mm ×
21.2 mm 10 μm particle size, 110 Å pore) at a flow rate
of 10 mL/min. Binary solvent systems consisting of A = 0.1% aqueous
TFA and B = 0.1% TFA in acetonitrile were employed with gradients
as indicated. Products were obtained as amorphous solids following
lyophilization. Electrospray ionization-mass spectrometric (ESI-MS)
were acquired with an Agilent LC/MSD system equipped with a multimode
ion source. Purities of samples subjected to biological testing were
assessed using this system and shown to be ≥95%. High resolution
mass spectrometric (HRMS) were acquired by LC/MS-ESI using LTQ-Orbitrap-XL
at 30K resolution.

Zhao X.Z., Smith S.J., Maskell D.P., Métifiot M., Pye V.E., Fesen K., Marchand C., Pommier Y., Cherepanov P., Hughes S.H, & Burke TR J.r. (2017). Structure-Guided Optimization of HIV Integrase Strand Transfer Inhibitors. Journal of Medicinal Chemistry, 60(17), 7315-7332.

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Characterization of Doxorubicin Precipitate

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The DOX precipitate
formed in PBS was centrifuged (10,000g for 3 min)
and resuspended in fresh water. This washing step was performed three
times. The precipitate was then solubilized with 0.1% formic acid
in a 50% aqueous solution of acetonitrile. ESI mass spectra of intact
DOX and the total DOX precipitate were obtained by FIA–MS by
using an Agilent LC/MSD system (Santa Clara, CA, USA). The DOX precipitate
was separated and analyzed using a Shimadzu LC/MS system (Kyoto, Japan)
equipped with a Vydac C18 column. The absorbance was monitored at
480 nm, and the ESI mass spectra of the components present in the
DOX precipitate were acquired. Solvent A (0.1% formic acid in water)
and solvent B (0.1% formic acid in acetonitrile) were used, and a
linear gradient of 1.5%/min of solvent B was maintained.

, & Yamada Y. (2020). Dimerization of Doxorubicin Causes Its Precipitation. ACS Omega, 5(51), 33235-33241.

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NMR Spectroscopic Characterization of Compounds

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Proton (¹H), carbon (¹³C) and phosphine (³¹P) NMR spectra were recorded on a Varian 400 MHz spectrometer or a Varian 500 MHz spectrometer and are reported in ppm relative to TMS and referenced to the solvent in which the spectra were collected. Solvent was removed by rotary evaporation under reduced pressure, and anhydrous solvents were obtained commercially and used without further drying. Purification by silica gel chromatography was performed using CombiFlash with EtOAc−hexanes solvent systems. Preparative high pressure liquid chromatography (HPLC) was conducted using a Waters Prep LC4000 system having photodiode array detection and Phenomenex C18 columns (catalogue no. 00G-4436-P0-AX, 250 mm × 21.2 mm 10 μm particle size, 110 Å pore) at a flow rate of 20 ml/min. Binary solvent systems consisting of A = 0.1% aqueous TFA and B = 0.1% TFA in acetonitrile were employed with gradients as indicated. Products were obtained as amorphous solids following lyophilization. Electrospray ionization-mass spectrometric (ESI-MS) were acquired with an Agilent LC/MSD system equipped with a multimode ion source. High resolution mass spectrometric (HRMS) were acquired by LC/MS-ESI using LTQ-Orbitrap-XL at 30K resolution.

Zhao X.Z., Wang W., Lountos G.T., Tropea J.E., Needle D., Pommier Y, & Burke TR J.r. (2022). Phosphonic acid-containing inhibitors of tyrosyl-DNA phosphodiesterase 1. Frontiers in Chemistry, 10, 910953.

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Characterization of Organic Compounds

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Example 1

All reagents and solvents were obtained commercially and used without further purification unless otherwise noted. ¹H NMR and ¹³C NMR spectra were recorded on a Bruker Advance 300 MHz instrument, and chemical shifts are reported in ppm on the 5 scale relative to TMS. Electrospray ionization-mass spectra (ESI-MS) were acquired using an Agilent LC/MSD system equiped with a multimode ion. Elemental analyses were performed by Galbraith Lab. Inc. (Knoxville, Tenn.) using combustion analysis methods for C, H, and N.

US10858306B2. Method for synthesizing iodo- or astatoarenes using diaryliodonium salts (2020-12-08). INSTITUT NATIONAL DE LA SANTE ET DE LA RECHERCHE MEDICALE (INSERM) [FR], CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE [FR], UNIVERSITE DE NANTES [FR], UNIVERSITE D'ANGERS [FR], THE GOVERNMENT OF THE UNITED STATES OF AMERICA, AS REPRESENTED BY THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES [US]. Inventors: François Guerard [FR], Jean-François Gestin [FR], Martin W. Brechbiel [US], Yong-Sok Lee [US].

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Comprehensive Spectroscopic Characterization

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¹H and ¹³C
NMR data were obtained on a Varian 400 MHz spectrometer or a Varian
500 MHz spectrometer and are reported in ppm relative to TMS and referenced
to the solvent in which the spectra were collected. The solvent was
removed by rotary evaporation under reduced pressure, and anhydrous
solvents were obtained commercially and used without further drying.
Purification by silica gel chromatography was performed using CombiFlash
R_f 200i with EtOAc–hexanes solvent systems. Preparative
high pressure liquid chromatography (HPLC) was conducted using a Waters
Prep LC4000 system having photodiode array detection and Phenomenex
C₁₈ columns (Cat. No. 00G-4436-P0-AX, 250 mm × 21.2
mm, 10 μm particle size, 110 Å pore) at a flow rate of
10 mL/min. Binary solvent systems consisting of A = 0.1% aqueous TFA
and B = 0.1% TFA in acetonitrile were employed with gradients as indicated.
Products were obtained as amorphous solids following lyophilization.
Electrospray ionization-mass spectra (ESI-MS) were acquired with an
Agilent LC/MSD system equipped with a multimode ion source. Purities
of samples subjected to biological testing were assessed using this
system and shown to be ≥95%. High-resolution mass spectra (HRMS)
were acquired by LC/MS-ESI using an LTQ-Orbitrap-XL at 30K resolution.

Zhao X.Z., Smith S.J., Métifiot M., Johnson B.C., Marchand C., Pommier Y., Hughes S.H, & Burke TR J.r. (2014). Bicyclic 1-Hydroxy-2-oxo-1,2-dihydropyridine-3-carboxamide-Containing HIV-1 Integrase Inhibitors Having High Antiviral Potency against Cells Harboring Raltegravir-Resistant Integrase Mutants. Journal of Medicinal Chemistry, 57(4), 1573-1582.

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Identification of Compounds via HPLC-ESI-MS/MS

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The HPLC-ESI-MS/MS analyses were performed using a 1100 Series Agilent Technologies LC/MSD system equipped with a diode array detector coupled to a quadrupole mass spectrometer with an ESI interface (Agilent Technologies, Mississagua, Ont.). The reverse-phase separation was performed on a Vydac C18 column (5 μm; 250 mm × 4.6 mm; Grace, Hespedia, CA.). The compounds were separated using eluent (A): 4.5% aqueous formic acid and eluent (B): acetonitrile diluted to 80% with 4.5% formic acid in water. The gradient was as follows: 7 min 15% B; 15 min 20% B; 16 min 100% B and in 24 min returned to 100% of eluent A. MS parameters were as follows: capillary voltage 4000 V; drying gas temperature 350 o C; nitrogen fl ow 12 L/min; nebulizer pressure 60 psi. The instrument was scanned positive and negative ions in the range from 100 to 1500 m/z at a rate of 2.0 s/cycle. Compounds identifi cation is based on spectra library developed in laboratory and published data (Gil-Izquierdo and Mallenthin, 2001) .

Klensporf-Pawlik D, & Przybylski R. (2015). Antioxidant activity of selected wild Canadian prairie fruits. Acta scientiarum polonorum. Technologia alimentaria, 14(4).

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