Shodex Columns for AOAC 2009.01 Method (Total Dietary Fiber in Food)

Record: 707

Category: Column Selection
Product: SC1011, SP0810, KS-800
Sample: Dietary Fiber

Question

Do you have Shodex column recommendations or applications for AOAC 2009.01 Method – Total Dietary Fiber in Food?

Answer

Yes. AOAC Method 2009.01 determines total, soluble, and insoluble dietary fiber using an enzymatic–gravimetric–chromatographic workflow. After enzymatic digestion and ethanol precipitation, the soluble low–molecular-weight dietary-fiber fraction (SDFS) is analyzed by HPLC or SEC using an RI detector.

Two Shodex column families are suitable for this chromatographic step:

1. Carbohydrate Columns for Monosaccharides and Oligosaccharides

Shodex offers Ca²⁺-form (SC series) and Pb²⁺-form (SP series) carbohydrate columns—each suited for different versions of the AOAC method.

• Ca²⁺ form – SUGAR SC1011
  A polymer-based Ca²⁺ cation-exchange column for separating mono-, di-, and oligosaccharides, as well as soluble dietary-fiber components.
  • Eluent: Water or aqueous Ca-salt solution (Ca(NO₃)₂ or CaSO₄). Optional use of 10–50 µg/mL Ca-EDTA helps prevent performance loss in samples containing heavy metals.
  • Usable range: 0.5–1.0 mL/min; ≤ 4 MPa; up to 95 °C.
  • Do not use non-Ca salts, as they can replace Ca²⁺ ions on the resin.
• Pb²⁺ form – SUGAR SP0810
  A Pb²⁺-form strong cation-exchange column designed for high-resolution separation of sugars in pure water.
  • Eluent: Water only (optionally ≤ 20 % v/v acetonitrile or ethanol).
  • Usable range: 0.5–1.0 mL/min; ≤ 3 MPa; up to 95 °C.
  • Do not use acids, bases, or EDTA-type eluents, which can strip Pb²⁺ from the resin.

These columns are widely used for food carbohydrate and soluble-fiber profiling under AOAC-style analytical conditions.

Recommended applications:

• Saccharides in Food – SUGAR SC1011
• Monosaccharides and Disaccharides – SUGAR SP0180 Series

2. Aqueous SEC Columns for Soluble-Fiber Distribution

For molecular-weight distribution of soluble polysaccharides or resistant maltodextrins, use the Shodex OHpak KS-801 or KS-802 columns. These are Na⁺-form cation-exchange polymer-gel SEC columns that separate saccharides and polysaccharides primarily by size exclusion.

• Eluent: Water or aqueous Na-salt solution (NaNO₃ or Na₂SO₄); up to 20 % v/v acetonitrile or ethanol.
• Temperature range: 50–85 °C.
• Do not use non-sodium salts, acids, or bases that may exchange counter ions.

Recommended application:

• Analysis of Fructooligosaccharide Sugar Components – KS-802 & KS-801

Comparison applications:

• Column Selection by Combination of Saccharides
• Comparison of Columns with Different Counter-Ions

Additional Comments

Although the customer question concerns AOAC 2009.01, it is important to note that AOAC has since released updated integrated dietary fiber methods:

• AOAC 2011.25 – Clarifies IDF/SDF workflow and aligns with Codex
• AOAC 2017.16 – A rapid integrated method explicitly described by AOAC as an update of 2009.01
• AOAC 2022.01 – The latest rapid enzymatic–gravimetric–LC method (Final Action 2024)

All of these updated methods retain the same requirement for HPLC analysis of the SDFS carbohydrate fraction, using monosaccharide/oligosaccharide profiling or SEC distribution. Therefore, the same Shodex columns listed above (SC1011, SP0810, KS-801/KS-802) remain fully compatible with the LC step in AOAC 2011.25, 2017.16, and 2022.01. This ensures continuity for labs upgrading to the newer methods.

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