¹H-NMR Analysis of Wine Metabolites: Method Development and Validation

Area of Science:

• Analytical Chemistry
• Food Science
• Spectroscopy

Background:

• Wine is a high-value commodity susceptible to sophisticated counterfeiting and fraud.
• Innovative analytical methods are crucial for wine authentication and quality control, requiring rigorous validation.
• Proton nuclear magnetic resonance spectroscopy (¹H-NMR) offers quantitative, reproducible, and rapid analysis, making it suitable for official controls.

Purpose of the Study:

• To develop and validate a standardized, automated workflow for quantifying 20 key oenological compounds in wine using ¹H-NMR.
• To establish a high-throughput, operator-independent method for wine analysis.
• To provide a framework for harmonized and transferable ¹H-NMR workflows in wine control laboratories.

Main Methods:

• Development of an automated workflow involving optimized sample preparation, external quantification standards, and spectrometer calibration.
• Utilized a dedicated R package (RnmrQuant1D) for fully automated spectral processing.
• Performed validation according to OIV metrological standards, assessing accuracy, precision, robustness, limits of quantification, and measurement uncertainty.

Main Results:

• The automated ¹H-NMR workflow demonstrated excellent linearity, trueness, and reproducibility for 20 oenological compounds.
• Validation confirmed the method's analytical performance met targeted specifications.
• Measurement uncertainties were estimated using both conventional and dynamic approaches.

Conclusions:

• The validated workflow is robust, easy to implement, requires minimal sample, and reduces operator bias.
• This standardized ¹H-NMR method supports wine authentication, quality control, and the potential for large-scale databases and chemometric integration.
• The study provides a framework for broader adoption of ¹H-NMR in global control laboratories for wine analysis.