Extraction of Vanillin From a Cola Soft Drink Using SOLA with Analysis by GC-MS

Significance of the Topic

Rapid and reliable quantification of vanillin in beverages is essential as the food industry increasingly relies on synthetic flavorings. Vanillin’s prevalence in complex matrices like cola necessitates efficient purification and sensitive detection methods to ensure quality control and compliance with regulatory standards.

Objectives and Study Overview

This application study aims to demonstrate the extraction of vanillin from cola soft drinks using SOLA solid phase extraction cartridges, followed by quantification via GC-MS employing an acid-deactivated polyethylene glycol phase column. The goal is to assess method linearity, recovery, precision, and solvent consumption compared with conventional SPE approaches.

Methodology

• Sample Pre-treatment: Cola samples were sonicated for 30 minutes to homogenize.
• SPE Procedure:
  • Cartridge: SOLA 10 mg/1 mL
  • Conditioning: 1 mL methanol, 1 mL water
  • Application: 200 µL of cola sample
  • Washing: 200 µL water
  • Elution: 200 µL methanol
  • Internal Standard: 200 µL benzyl benzoate solution added after elution
• Calibration: Standards of vanillin (10–1000 ng/mL) mixed 1:1 with 200 ng/mL benzyl benzoate were used to build a calibration curve.
• GC-MS Detection: Selected ion monitoring (SIM) at m/z 152 for vanillin, m/z 212 for internal standard.

Used Instrumentation

• Solid Phase Extraction: Thermo Scientific SOLA cartridges, HyperSep glass manifold
• GC System: Thermo Scientific Trace GC Ultra with TraceGOLD TG-WaxMS A column (30 m × 0.25 mm × 0.25 µm)
• Autosampler: Thermo Scientific TriPlus
• Mass Spectrometer: Thermo Scientific ISQ single quadrupole MS (EI mode, 70 eV)

Main Results and Discussion

• Linearity: Calibration curve showed R² = 0.9987 over 10–1000 ng/mL.
• Recoveries in Water: 96–103% (mean 99%, RSD 2.7%) for 20 ng/mL vanillin spike (n=6).
• Recoveries in Cola: Extracted concentrations ranged 23.2–26.7 ng/mL (mean 25.6 ng/mL, RSD 4.6%) for 20 ng/mL spike.
• Solvent Reduction: SPE procedure required only 200 µL of solvents versus > 1 mL for traditional cartridges, eliminating lengthy drying steps.
• Chromatographic Performance: The acid-deactivated TG-WaxMS A column provided sharp peaks and robust performance for acidic analytes.

Benefits and Practical Applications

• High accuracy and precision with low relative standard deviations.
• Minimal solvent consumption and faster sample throughput.
• Simplified workflow without solvent evaporation and reconstitution.
• Applicability to routine quality control in food and beverage laboratories.

Future Trends and Opportunities

• Expansion of SOLA SPE technology to other flavor and aroma compounds in complex foods.
• Integration with high-throughput and automated platforms for large-scale testing.
• Development of greener eluents and further miniaturized extraction formats.
• Coupling with advanced detection techniques for multi-analyte screening.

Conclusion

The combination of SOLA solid phase extraction cartridges and a TraceGOLD TG-WaxMS A GC column enables efficient, accurate, and reproducible quantification of vanillin in cola with reduced solvent usage and simplified sample preparation, making it well-suited for high-throughput analytical settings.

References

• United Nations Environment Programme, OECD Screening Information Data Set (SIDS) 121335.