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Temperature-programmed high-performance liquid chromatography coupled to isotope ratio mass spectrometry
Jean-Philippe Godin1, Gérard Hopfgartner, Laurent Fay
1Nestle Research Center, Nestec Ltd., Department of Bioanalytical Science, P.O. Box 44, CH-1000 Lausanne 26, Switzerland. jean-philippe.godin@rdls.nestle.com
Analytical Chemistry
|August 12, 2008
Summary
This study introduces temperature-programmed liquid chromatography coupled to isotope ratio mass spectrometry (LC-IRMS) for precise carbon-13 isotopic analysis. The method overcomes limitations of aqueous mobile phases, enabling accurate measurements for phenolic acids.
Area of Science:
- Analytical Chemistry
- Mass Spectrometry
- Chromatography
Background:
- Liquid chromatography coupled to isotope ratio mass spectrometry (LC-IRMS) is valuable but limited by aqueous mobile phases.
- High-precision carbon-13 isotopic analysis requires advanced separation techniques.
Purpose of the Study:
- To develop and evaluate a temperature-programmed LC-IRMS strategy for high-precision (13)C isotopic analysis using aqueous mobile phases.
- To assess the impact of isothermal and gradient temperature conditions on isotopic accuracy and precision.
Main Methods:
- Utilized temperature-programmed LC-IRMS with aqueous mobile phases.
- Conducted experiments under isothermal high-temperature (170°C) and temperature gradient conditions.
- Analyzed phenolic acids, including p-coumaric acid and its conjugates, and ferulic acid.
Main Results:
- Isothermal conditions at 170°C yielded reliable isotopic ratios for p-coumaric acid and its glucuronide (precision/accuracy < 0.3‰).
- Sulfate conjugate accuracy was affected by coelution; ferulic acid degraded at high temperatures.
- Temperature gradient LC-IRMS required strategies to mitigate background drift for accurate measurements.
Conclusions:
- Temperature-programmed LC-IRMS offers a viable approach for high-precision (13)C analysis with aqueous mobile phases.
- Optimized temperature control is crucial for accurate isotopic measurements, especially for compounds with varying elution times or conjugates.
- The developed method demonstrates potential for quantitative analysis and handling of residual solvents.
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