UPLC-MS Analysis of Grayanotoxin I and II standards in Negative Mode

Grayanotoxin I and II standards were serially diluted in methanol from 1 mg/mL to 0.03 ug/mL for analysis. Ultra-high Pressure (UP) LC-MS data were acquired using an Orbitrap Fusion Lumos Tribrid mass spectrometer (ThermoScientific, Waltham, MA, U.S.A.) with an electrospray ionization source coupled to a Vanquish UHPLC system (ThermoScientific). 5 μL injections were separated by reverse-phase UPLC using an Acquity BEH C18 column (150 × 1 mm, 1.7 μm particle size (Waters Corp., Milford, MA, U.S.A.)) held at 55 °C with a flow rate of 100 μL/min. The following binary solvent gradient was employed with solvent A (LC-MS grade water with 0.1% formic acid), and solvent B (LC-MS grade acetonitrile with 0.1% formic acid): initial isocratic composition of 97:3 (A:B), increasing linearly to 55:45 over 10 min, increasing linearly to 25:75 over 2 min, increasing linearly to 0:100 over 0.5 min followed by an isocratic hold at 0:100 for 4 min, gradient returned to 97:3 over 0.2 min and held for 3.3 min. The negative ionization mode was utilized over a full scan of m/z 100–1000 with the following settings: spray voltage, 2.5 kV; IT tube temperature, 275 °C; vaporizer temperature, 75 °C; sheath gas and auxiliary gas flow, 25 and 5 units, respectively. Each concentration of standard was run in triplicate. Mass spectral data were converted to mzML format using MSConvert.

Citation

Anez, Savannah; Burkhart, Eric; Kellogg, Joshua (2025). UPLC-MS Analysis of Grayanotoxin I and II standards in Negative Mode [Data set]. Scholarsphere. https://doi.org/10.26207/aefw-wx98

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Metadata

Work Title UPLC-MS Analysis of Grayanotoxin I and II standards in Negative Mode
Access
Open Access
Creators
  1. Savannah Anez
  2. Eric Paul Burkhart
  3. Joshua Kellogg
License CC BY-NC-SA 4.0 (Attribution-NonCommercial-ShareAlike)
Work Type Dataset
Acknowledgments
  1. Standards for Grayanotoxins I and II were generously gifted by Dr. A. Douglas Kinghorn at the Ohio State University, Columbus, OH.
Publication Date March 4, 2025
DOI doi:10.26207/aefw-wx98
Deposited March 04, 2025

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Version 1
published

  • Created

    March 04, 2025 16:17 by sga5169

  • Updated Description, Publication Date Show Changes

    March 04, 2025 16:19 by sga5169

    Description
    • Grayanotoxin I and II standards were serially diluted in methanol from 1 mg/mL to 0.03 ug/mL for analysis. Ultra-high Pressure (UP) LC-MS data were acquired using an Orbitrap Fusion Lumos Tribrid mass spectrometer (ThermoScientific, Waltham, MA, U.S.A.) with an electrospray ionization source coupled to a Vanquish UHPLC system (ThermoScientific). 5 μL injections were separated by reverse-phase UPLC using an Acquity BEH C18 column (150 × 1 mm, 1.7 μm particle size (Waters Corp., Milford, MA, U.S.A.)) held at 55 °C with a flow rate of 100 μL/min. The following binary solvent gradient was employed with solvent A (LC-MS grade water with 0.1% formic acid), and solvent B (LC-MS grade acetonitrile with 0.1% formic acid): initial isocratic composition of 97:3 (A:B), increasing linearly to 55:45 over 10 min, increasing linearly to 25:75 over 2 min, increasing linearly to 0:100 over 0.5 min followed by an isocratic hold at 0:100 for 4 min, gradient returned to 97:3 over 0.2 min and held for 3.3 min. The negative ionization mode was utilized over a full scan of m/z 100–1000 with the following settings: spray voltage, 2.5 kV; IT tube temperature, 275 °C; vaporizer temperature, 75 °C; sheath gas and auxiliary gas flow, 25 and 5 units, respectively. Mass spectral data were converted to mzML format using MSConvert.
    Publication Date
    • 2025-03-04
  • Updated Acknowledgments Show Changes

    March 04, 2025 16:20 by sga5169

    Acknowledgments
    • Standards for Grayanotoxins I and II were generously gifted by Dr. A. Douglas Kinghorn at the Ohio State University, Columbus, OH.
  • Added Creator Savannah Anez

    March 04, 2025 16:20 by sga5169

  • Added Creator Joshua Kellogg

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  • Updated

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  • Added Creator Eric Paul Burkhart

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  • Updated Description Show Changes

    March 07, 2025 13:06 by sga5169

    Description
    • Grayanotoxin I and II standards were serially diluted in methanol from 1 mg/mL to 0.03 ug/mL for analysis. Ultra-high Pressure (UP) LC-MS data were acquired using an Orbitrap Fusion Lumos Tribrid mass spectrometer (ThermoScientific, Waltham, MA, U.S.A.) with an electrospray ionization source coupled to a Vanquish UHPLC system (ThermoScientific). 5 μL injections were separated by reverse-phase UPLC using an Acquity BEH C18 column (150 × 1 mm, 1.7 μm particle size (Waters Corp., Milford, MA, U.S.A.)) held at 55 °C with a flow rate of 100 μL/min. The following binary solvent gradient was employed with solvent A (LC-MS grade water with 0.1% formic acid), and solvent B (LC-MS grade acetonitrile with 0.1% formic acid): initial isocratic composition of 97:3 (A:B), increasing linearly to 55:45 over 10 min, increasing linearly to 25:75 over 2 min, increasing linearly to 0:100 over 0.5 min followed by an isocratic hold at 0:100 for 4 min, gradient returned to 97:3 over 0.2 min and held for 3.3 min. The negative ionization mode was utilized over a full scan of m/z 100–1000 with the following settings: spray voltage, 2.5 kV; IT tube temperature, 275 °C; vaporizer temperature, 75 °C; sheath gas and auxiliary gas flow, 25 and 5 units, respectively. Mass spectral data were converted to mzML format using MSConvert.
    • Grayanotoxin I and II standards were serially diluted in methanol from 1 mg/mL to 0.03 ug/mL for analysis. Ultra-high Pressure (UP) LC-MS data were acquired using an Orbitrap Fusion Lumos Tribrid mass spectrometer (ThermoScientific, Waltham, MA, U.S.A.) with an electrospray ionization source coupled to a Vanquish UHPLC system (ThermoScientific). 5 μL injections were separated by reverse-phase UPLC using an Acquity BEH C18 column (150 × 1 mm, 1.7 μm particle size (Waters Corp., Milford, MA, U.S.A.)) held at 55 °C with a flow rate of 100 μL/min. The following binary solvent gradient was employed with solvent A (LC-MS grade water with 0.1% formic acid), and solvent B (LC-MS grade acetonitrile with 0.1% formic acid): initial isocratic composition of 97:3 (A:B), increasing linearly to 55:45 over 10 min, increasing linearly to 25:75 over 2 min, increasing linearly to 0:100 over 0.5 min followed by an isocratic hold at 0:100 for 4 min, gradient returned to 97:3 over 0.2 min and held for 3.3 min. The negative ionization mode was utilized over a full scan of m/z 100–1000 with the following settings: spray voltage, 2.5 kV; IT tube temperature, 275 °C; vaporizer temperature, 75 °C; sheath gas and auxiliary gas flow, 25 and 5 units, respectively. Each concentration of standard was run in triplicate. Mass spectral data were converted to mzML format using MSConvert.
  • Added README.txt

    March 25, 2025 16:40 by sga5169

  • Updated Creator Eric Paul Burkhart

    March 25, 2025 16:40 by sga5169

  • Updated Creator Joshua Kellogg

    March 25, 2025 16:40 by sga5169

  • Updated License Show Changes

    April 03, 2025 14:32 by sga5169

    License
    • https://creativecommons.org/licenses/by-nc-sa/4.0/
  • Published

    April 03, 2025 14:33 by sga5169

  • Updated

    April 03, 2025 22:05 by [unknown user]

Version 2
published

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  • Published

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  • Updated

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