Analysis of Saccharides in Non-Sugar Beverages by LC/MS (VG-50 2D)

According to the Food Labeling Standards of the Consumer Affairs Agency of Japan, foods may be labeled as “non-sugar” or “sugar free” if saccharide content is below 0.5 g per 100 mL or 100 g of the food. For sugar analysis, general-purpose detectors with low selectivity such as refractive index (RI) detectors or evaporative light scattering detectors (ELSD) are often used. However, when saccharide concentration is very low as in non-sugar beverages, a mass spectrometer, which offers high selectivity and high sensitivity, is more effective. In this application, a commercial carbonated beverage labeled non-sugar was analyzed. Saccharides were separated using a polymer-based HILIC column, HILICpak VG-50 2D, and quantified by an LC/MS. The non-sugar beverage tested was confirmed to contain less than 0.5 g of saccharides per 100 mL.

Sample preparation

  1. (1)Degas non-sugar beverages for 5 minutes to remove carbonation. Then, filter through a 0.2-µm membrane filter.
  2. (2)Dilute 1+999 with 75 % acetonitrile aqueous solution and use as LC/MS sample.

Sample: 1 µL
Mixed standard solution (0.5 mg/L each in 75 % Acetonitrile aqueous solution)

  1. 1.Rhamnose
  2. 2.Arabinose
  3. 3.Xylose
  4. 4.Fructose
  5. 5.Galactose
  6. 6.Glucose
  7. 7.Sucrose
  8. 8.Lactose
  9. 9.Maltose
chromatogram of saccharides

Sample: 1 µL
Pre-treated non-sugar beverage

  1. 6.Glucose
  2. 8.Lactose
  3. 9.Maltose
chromatogram of non-sugar beverage
Instrument
NexeraTM XR, LCMS-2050 (Shimadzu Corporation)
Column
Shodex HILICpak VG-50 2D (2.0 mm I.D. x 150 mm)
Eluent
(A) 2.5 mM Ammonium bicarbonate aq.
(B) 25 mM Ammonium bicarbonate aq./Acetonitrile=10/90
99 % B (0-11 min) → 77 % B (23-27 min) → 99 % B (27.1 min-38 min)
Flow rate
0.2 mL/min
Detector
ESI/APCI (DUISTM) (Ngeative)
Column temp.
45 ℃

Data provided by Shimadzu Corporation.
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