LC/MS, LC/SQ
IndustriesFood & Agriculture
ManufacturerShimadzu
Importance of the Topic
Due to global guidelines capping daily sugar intake and strict labeling requirements for beverages, sensitive detection of saccharides at trace levels is essential. Conventional refractive index or light scattering detectors lack sufficient sensitivity or selectivity in complex matrices, driving the need for HILIC separation coupled with mass spectrometric detection.
Study Objectives and Overview
This work presents a simultaneous quantification method for nine mono- and disaccharides in non-sugar beverages using hydrophilic interaction liquid chromatography and a single quadrupole mass spectrometer. The goal was to achieve high sensitivity, reproducibility and matrix tolerance.
Methodology
Sample preparation involved degassing carbonated drinks, membrane filtration and dilution in 75% acetonitrile. Chromatographic separation used a HILIC column under a gradient elution of ammonium bicarbonate buffer and acetonitrile. Mass detection was performed in negative ion mode using selected ion monitoring for target m/z values.
Used Instrumentation
- Nexera XR UHPLC system
- Shodex HILICpak VG-50 2D column (150 × 2.0 mm, 5 µm)
- LCMS-2050 single quadrupole mass spectrometer with DUIS ion source
Main Results and Discussion
- All nine saccharides were baseline resolved within 22 min.
- Calibration curves showed linearity coefficients (r2) ≥ 0.998 across compound-specific ranges down to low µg/L levels.
- Repeatability tests yielded retention time RSD < 0.7% and peak area RSD < 5%.
- Spike recovery in four beverage matrices ranged from 90–110%, confirming minimal matrix effects.
- Analysis of commercial non-sugar drinks revealed total saccharides below 0.5 g/100 mL, meeting regulatory criteria.
Benefits and Practical Applications
- Superior sensitivity and selectivity over traditional RI and ELSD detectors.
- Robust quantification unaffected by beverage matrix complexity.
- Simultaneous multi-sugar profiling at trace concentrations.
- Valuable for quality control, product validation and nutritional labeling.
Future Trends and Applications
Advancements may include coupling with tandem mass spectrometry for structural confirmation, automated high-throughput platforms, expansion to other polar analytes in food matrices, and portable LC-MS solutions for on-site quality assessment.
Conclusion
The described HILIC-LCMS-2050 method enables accurate, sensitive and reproducible analysis of trace saccharides in non-sugar beverages, supporting compliance with labeling regulations and facilitating development of low-sugar products.
References
- World Health Organization. Sugars Intake for Adults and Children. Geneva: WHO; 2015.
- Consumer Affairs Agency of Japan. Food Labeling Standards, Cabinet Office Ordinance No.10; 2015.
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