Development of a Multianalyte Method for the Determination of Phenolic Compounds in Residues from Beverage Production Using a Cyclofructan-Based Column in HILIC-MS/MS

This study expands and shows the versatility of applications in hydrophilic interaction chromatography coupled with triple quadrupole mass spectrometry (HILIC-MS/MS) using a FRULIC-N column to determine 31 phenolic compounds in beverage industry residues (coffee, apple juice, beer, and wine). Optimization, via Doehlert design, determined the acetonitrile proportion (50-90%) and pH (3.0-7.0) in the mobile phase (MP). A 2² factorial design assessed the concentration of ammonium acetate (10-110 mmol L^-1) in the MP and column temperature (20-60 °C). Injection volume (5-45 µL) was univariately optimized. Separations at 60 °C reduced chromatographic run time to less than 11 min. Gradient elution (500 µL min^-1) employed an MP comprising acetonitrile and ammonium acetate (110 mmol L^-1, pH 7). Validation demonstrated average coefficient of determination (R²) 0.9707, limit of detection 0.001-0.503 mg L^-1 and quantification 0.004-1.524 mg L^-1, precision < 12.2%, recovery 92.4-110.8%. The method was applied to five residues, indicating its viability for determining phenolics in beverage production residues.

Keywords:
HILIC; phenolic compounds; by-products; beverage industry; method validation