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Vitamin D3 quantification in a cod liver oil-based supplement.

Gianluca Bartolucci1, Elisa Giocaliere, Francesca Boscaro

  • 1Department of Pharmaceutical Sciences, University of Florence, Florence, Italy. gianluca.bartolucci@unifi.it

Journal of Pharmaceutical and Biomedical Analysis
|February 9, 2011
PubMed
Summary

A new method accurately quantifies vitamin D3 (Vit. D3) in supplements. This analysis revealed dangerous levels of Vit. D3 in some cod liver oil products, exceeding label claims by 1000-fold.

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Area of Science:

  • Analytical Chemistry
  • Nutritional Science
  • Pharmacology

Background:

  • Three cases of vitamin D3 (Vit. D3) intoxication were linked to cod liver oil supplements.
  • Accurate quantification of Vit. D3 in complex oily matrices is challenging.
  • Existing methods may not adequately address the safety concerns associated with high-dose Vit. D3 supplements.

Purpose of the Study:

  • To develop and validate a reliable analytical method for quantifying Vit. D3 in oily dietary supplements.
  • To investigate the actual Vit. D3 content in supplements implicated in patient intoxications.
  • To ensure consumer safety by verifying supplement label accuracy.

Main Methods:

  • Development of a liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) method.

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  • Incorporation of a deuterium-labeled internal standard for enhanced accuracy.
  • Utilization of solid-phase extraction (SPE) to overcome matrix complexity.
  • Employing both MS and MS/MS acquisition modes for data reliability.
  • Method validation including linearity, precision, accuracy, and robustness testing.

    • Main Results:

    • The developed LC-APCI-MS and MS/MS method accurately quantifies Vit. D3 in the 1-5 μg/mL range.
    • Analysis of supplements from intoxicated patients revealed Vit. D3 levels approximately three orders of magnitude higher than declared.
    • Other batches of the same commercial product showed Vit. D3 content consistent with label claims.

    Conclusions:

    • The validated LC-APCI-MS/MS method provides a reliable tool for assessing Vit. D3 content in oily supplements.
    • Significant discrepancies between declared and actual Vit. D3 content can exist in some supplements, posing health risks.
    • Quality control and accurate labeling of dietary supplements are crucial for public health.