Quantitative Analysis of Carbohydrates and Artificial Sweeteners in Food Samples Using GFC- MS with APCI Interface and Post-column Reagent Addition

Importance of the Topic

Food safety and quality control require reliable quantification of both natural sugars and artificial sweeteners. Advances in analytical chemistry enable comprehensive profiling of carbohydrates and sugar substitutes in diverse food matrices. A single, sensitive method capable of simultaneously detecting multiple compounds reduces analysis time and resources while meeting regulatory and nutritional monitoring needs.

Study Objectives and Overview

This work presents a unified gel filtration chromatography–mass spectrometry (GFC-MS) method using an atmospheric pressure chemical ionization (APCI) interface and post-column reagent addition. The goals were to separate and quantify sixteen carbohydrates and three artificial sweeteners in one run, to evaluate method performance (linearity, sensitivity, repeatability), and to apply the approach to real food and mouthrinse samples.

Methodology

The chromatographic separation employed a Shim-pack SCR-101 P size-exclusion column with pure water as the mobile phase under isocratic conditions (0.60 mL/min, 80 °C). A post-column mix of methanol/chloroform (95:5, 0.1 mL/min) delivered a low level (0.7 %) of chloroform to enhance APCI ionization in negative mode (SIM detection). Calibration standards covered wide concentration ranges (0.04–500 mg/L), and samples were diluted 1 000-fold and filtered before injection.

Used Instrumentation

• Shimadzu LCMS-2020 single quadrupole mass spectrometer
• APCI interface operated in negative SIM mode
• Shim-pack SCR-101 P GFC column (7.9 × 300 mm)
• Post-column reagent addition system for methanol/chloroform delivery

Results and Discussion

The method achieved baseline separation or selective SIM detection of co-eluting pairs (e.g., galactose/rhamnose, myo-inositol/glycerol) by exploiting distinct m/z values of chloride adducts ([M+Cl]–). Linear calibration curves exhibited r2 values above 0.999 for all analytes. Limits of detection ranged from 0.01 to 1 mg/L. Repeatability was excellent (RSD ≤ 9.5 % at target levels). Application to beverages, soy sauce, sake, soft and diet drinks, probiotic drinks, and a mouthrinse yielded quantification results consistent with product labels.

Benefits and Practical Applications

• A single-run method covers a broad panel of sugars, sugar alcohols, and sweeteners.
• Minimal organic modifier and low chloroform usage reduce contamination and instrument maintenance.
• High sensitivity and repeatability support routine QA/QC in food and beverage industries.
• Applicable to complex matrices with simple sample preparation (dilution and filtration).

Future Trends and Opportunities

Potential developments include integration with high-resolution MS for untargeted carbohydrate profiling, automation of sample handling for high throughput, exploration of alternative benign ionization enhancers, and coupling with chemometric tools for rapid screening of novel sweeteners and glycan structures.

Conclusion

The presented GFC-MS approach with APCI and post-column reagent addition is a robust, sensitive, and efficient solution for simultaneous quantification of multiple carbohydrates and artificial sweeteners. It streamlines analysis in food, beverage, and personal care products while maintaining high analytical performance.

References

• Application News No. C74, Shimadzu Corporation.
• Kato Y., Numajiri Y., Journal of Chromatography 562:81–97 (1991).