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Determination of niacin in infant formula by solid-phase extraction/liquid chromatography: peer-verified method
Denis E LaCroix1, Wayne R Wolf, G William Chase
1US Department of Agriculture, Beltsville Human Nutrition Research Center, Food Composition Laboratory, Beltsville, MD 20705-2350, USA.
Journal of AOAC International
|June 27, 2002
Summary
This study validated a method for measuring niacin in infant formula. The AOAC Peer-Verified Method (PVM) 1:2,000 demonstrated accurate and reliable niacin determination through interlaboratory testing.
Area of Science:
- Analytical Chemistry
- Food Science
- Nutritional Analysis
Background:
- Accurate niacin determination in infant formula is crucial for nutritional assessment.
- Existing methods require validation for reliability and accuracy.
- The AOAC Peer-Verified Method (PVM) 1:2,000 offers a potential solution for standardized niacin analysis.
Purpose of the Study:
- To conduct an interlaboratory peer validation study of AOAC PVM 1:2,000 for niacin determination in infant formula.
- To assess method variability, robustness, and accuracy using a Data Quality Objectives (DQO) approach.
- To ensure the method's reliability and traceability through the use of a certified reference material.
Main Methods:
- Solid-phase extraction coupled with liquid chromatography (SPE/LC) was employed.
- A DQO approach incorporated statistical agreement, recovery, repeatability relative standard deviation (RSDr), HORRAT, interference validation, and certified reference material (CRM) analysis.
- National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1846 Infant Formula was used for accuracy assessment.
Main Results:
- The HORRAT value of 1.07 met the Horwitz "limits of acceptability" criteria.
- Niacin content determined by the originating laboratory (59.7 ± 4.0 µg/g) and the peer laboratory (56.6 ± 6.6 µg/g) showed statistical equivalence.
- Linear calibration curves and quantitative recovery were achieved, indicating method performance.
Conclusions:
- The AOAC PVM 1:2,000 is a valid and reliable method for determining niacin in infant formula.
- The integration of PVM with a CRM enhances confidence in data accuracy and traceability.
- This validated method supports accurate nutritional labeling and quality control of infant formula.