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How do you measure fibre in food? Understanding the Analytical Methods

4 min read

Over decades, the methodology for measuring dietary fiber has evolved significantly as scientists gain a more complete understanding of its complex nature. This has led to the development of sophisticated laboratory techniques that accurately define how you measure fibre in food for nutritional labeling purposes.

Quick Summary

The measurement of fiber in food involves complex laboratory methods, primarily enzymatic-gravimetric and enzymatic-chemical techniques, to mimic human digestion. This ensures accurate and compliant nutritional labeling for consumers.

Key Points

  • Enzymatic-Gravimetric Method: The primary approach uses enzymes to digest a food sample, leaving only the non-digestible fiber to be weighed.

  • AOAC Official Methods: The Association of Official Analytical Chemists (AOAC) establishes the standardized protocols used by most testing labs.

  • Hybrid Methods (AOAC 2017.16): The most advanced technique combines gravimetric analysis for high-molecular-weight fiber with HPLC for low-molecular-weight soluble fiber.

  • Codex Alimentarius Definition: Modern methods align with the Codex definition, which includes resistant starch and non-digestible oligosaccharides as dietary fiber.

  • Insoluble vs. Soluble Fiber: Most methods can quantify insoluble and soluble fiber separately, revealing different fiber types with distinct health benefits.

  • Factors Affecting Results: Variability can occur due to the specific method chosen, enzyme purity, and the food's composition, requiring standardized procedures for consistent results.

In This Article

The Evolution of Fibre Measurement

For decades, the concept of dietary fibre has evolved from a simple indigestible component to a complex group of substances with diverse physiological effects. Early methods, such as crude fiber analysis, were insufficient as they failed to capture all components of dietary fiber, severely underestimating the true content. Modern, official methods now aim to closely simulate the human digestive system to provide a more accurate and comprehensive measurement for both naturally occurring and added fibers.

The Gold Standard: Enzymatic-Gravimetric Methods

Most official food-testing laboratories use enzymatic-gravimetric methods, primarily standardized by the Association of Official Analytical Chemists (AOAC) International. The core principle is to use enzymes to digest and remove all components of a food sample that would be broken down in the small intestine, such as starch and protein. The remaining non-digestible residue is then filtered, dried, and weighed. The process includes several crucial steps:

Simulating Human Digestion

  1. Sample Preparation: The food sample is defatted and ground to a fine powder to ensure the enzymes can act uniformly.
  2. Enzymatic Hydrolysis: The sample is treated with a sequence of digestive enzymes, including heat-stable alpha-amylase, protease, and amyloglucosidase, to break down starch and protein. Modern methods like AOAC 2017.16 use physiological conditions (e.g., 37°C) to more accurately mimic human digestion.
  3. Filtration and Precipitation: After enzymatic treatment, the mixture is filtered. The insoluble dietary fiber (IDF) remains as a residue on the filter. The liquid filtrate, containing the soluble dietary fiber (SDF), is then mixed with ethanol to precipitate the high-molecular-weight SDF.
  4. Gravimetric Quantification: Both the IDF residue and the precipitated SDF are filtered, washed, dried, and weighed. The final weight is corrected for any residual protein and ash to ensure only fiber is quantified.

The Rise of Hybrid Methods

To address the limitations of older methods that failed to capture low-molecular-weight (LMW) fibers like fructans and polydextrose, hybrid enzymatic-gravimetric-liquid chromatography methods were developed. The current gold standard, AOAC 2017.16, is a hybrid approach that separates fiber into high molecular weight (HMWDF) and low molecular weight (LMWDF) fractions. The HMWDF is measured gravimetrically, while the LMWDF, which remains soluble in ethanol, is measured separately using High-Performance Liquid Chromatography (HPLC).

Why Different Methods Yield Different Results

The choice of analytical method can significantly influence the reported dietary fiber value. Older methods like AOAC 985.29 and 991.43 often underestimate total fiber because they do not account for resistant starch and LMW nondigestible oligosaccharides. Enzymatic-chemical methods, such as the Englyst method, also provide different values as they chemically measure the monosaccharide components of fiber, often resulting in lower totals compared to AOAC methods. Factors like sample type, enzyme purity, and incubation conditions can also introduce variability.

Comparison of Major Fiber Analysis Methods

Feature Older AOAC Methods (e.g., 985.29) McCleary Method (AOAC 2009.01) Hybrid Method (AOAC 2017.16)
Principle Enzymatic-Gravimetric Enzymatic-Gravimetric Enzymatic-Gravimetric and HPLC
Scope Measures HMWDF (IDF & SDFP) only Measures all components of Codex-defined fiber Measures all components of Codex-defined fiber (HMWDF & LMWDF)
Temperature Harsh conditions (e.g., 100°C) Physiological conditions (37°C) Physiological conditions (37°C)
Measures Resistant Starch? Partially or not at all Yes Yes, accurately
Measures LMW Fibers? No No, unless a separate HPLC step is used Yes, via HPLC
Complexity Relatively simple Moderately complex More complex, requires specialized equipment

Components Measured in Modern Analysis

Modern dietary fiber analysis, particularly using hybrid methods like AOAC 2017.16, provides a comprehensive picture of fiber content by measuring various components:

  • Insoluble Dietary Fiber (IDF): Includes cellulose, hemicellulose, and lignin. These components contribute to stool bulk and support digestive regularity.
  • Soluble Dietary Fiber (SDF): Includes pectins, gums, and mucilages. This fiber type dissolves in water and is associated with cholesterol reduction and blood sugar control.
  • Resistant Starch (RS): Starch that resists digestion in the small intestine and acts like fiber. Modern methods are crucial for accurately quantifying RS, especially types that are more resistant.
  • Nondigestible Oligosaccharides (NDOs): These are smaller chain carbohydrates with prebiotic properties, such as fructans (e.g., inulin) and galacto-oligosaccharides (GOS). They are soluble and require HPLC for accurate measurement.
  • Polydextrose and Resistant Maltodextrins: Synthetically produced fibers that act as dietary fiber but are not captured by older gravimetric methods. Hybrid methods that include HPLC can quantify these.

What Factors Affect Accurate Fiber Measurement?

Beyond the choice of analytical method, several variables can influence the accuracy of fiber analysis, including incomplete starch removal, protein and ash contamination, incomplete soluble fiber precipitation, the complexity of the food matrix, and the presence of synthetic fibers. Modern methods address these factors through optimized protocols.

The Role of Fiber Measurement in the Food Industry

Accurate fiber measurement is a necessity for food manufacturers for several key reasons:

  • Nutritional Labeling: Regulatory bodies require specific methods for declaring fiber content on food labels.
  • Quality Control: Testing ensures fiber-fortified products meet labeled claims.
  • Product Development: Understanding fiber components helps formulate products with desired functional properties.
  • Health Claims: Reliable data is needed to support health claims related to fiber.

Conclusion: The Importance of Standardized Methods

For food manufacturers, knowing how do you measure fibre in food is critical for accurate nutritional labeling and regulatory compliance. The shift from outdated crude fiber analysis to modern, integrated AOAC methods reflects a deeper scientific understanding of dietary fiber's complex nature. While complex and costly, these standardized methods ensure that the fiber values declared on food labels are reliable and reflect the full spectrum of non-digestible carbohydrates present. Consumers benefit from more accurate information, enabling better-informed dietary choices for health and wellness.

For more information on these analytical methods, consult official publications from organizations like the AOAC International, which details the procedures and validations for current standards.

Frequently Asked Questions

The AOAC has validated several methods, with the current most comprehensive being AOAC 2017.16. It is a hybrid enzymatic-gravimetric and HPLC method that measures all forms of dietary fiber, including resistant starch and low-molecular-weight oligosaccharides.

Older methods, like AOAC 985.29, primarily used only enzymatic-gravimetric techniques and often underestimated total fiber by missing low-molecular-weight fibers and some types of resistant starch. Newer methods, like AOAC 2017.16, use a hybrid approach that incorporates HPLC to accurately measure the full range of fiber components.

Results can vary due to differences in the types of enzymes used, the incubation conditions (pH, temperature), and whether low-molecular-weight fibers are captured. For example, the Englyst method generally gives lower values than AOAC methods because it measures non-starch polysaccharides but excludes lignin and resistant starch.

Resistant starch is a type of starch that escapes digestion in the small intestine and is measured as part of dietary fiber in modern, integrated methods like AOAC 2017.16. Older methods often failed to capture it accurately.

Crude fiber analysis, an older and less accurate method, is still sometimes used in the livestock feed industry but is not suitable for human food labeling. It significantly underestimates total dietary fiber because harsh chemical treatments destroy a large portion of the fiber components.

Accurate fiber measurement is essential for nutritional labeling, regulatory compliance, and for providing consumers with reliable information. It also helps researchers understand the specific health effects of different fiber components.

The main steps include enzymatic digestion of starch and protein, followed by the separation of insoluble and soluble fiber. The high-molecular-weight fractions are precipitated and weighed (gravimetric analysis), while low-molecular-weight fibers are quantified using chromatography.

Yes, systems like the ANKOM dietary fiber analyzer exist to automate the enzymatic-gravimetric process, increasing efficiency and consistency in testing.

References

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Medical Disclaimer

This content is for informational purposes only and should not replace professional medical advice.