Quantitative determination of cereulide by LC-MS/MS requires partitioning/salting-out extraction with water/acetonitrile for a reliable measurement in powdered infant formula.

Authors

Mathieu Dubois, Thomas Bessaire, Xanthippi Theurillat, Christophe Fuerer, Marie-Claude Courtet-Compondu, Bjørn Eriksen, Adrienne Tarres, Rosemarie Jenni, Sabine Lahrichi, Thierry Delatour, Michael Affolter, Marjorie Guitard-Uldry, Alexandre Panchaud

Published in

International journal of food microbiology. Volume 459. Pages 111919. Jun 19, 2026. Epub Jun 19, 2026.

Abstract

The current reference method ISO 18465:2017 for cereulide analysis in food relies on acetonitrile-only extraction and was originally validated across diverse food matrices. Our investigations demonstrate a systematic underestimation of cereulide concentration by one order of magnitude in powdered infant formula when contamination is caused by tainted ingredients. Lipids and proteins forming compact, low moisture complex structures in the powder, acetonitrile alone used in ISO 18465:2017 extraction is unable to fully solubilize and access cereulide trapped inside the matrix. In response to this critical limitation, we validated an alternative sample preparation procedure based upon a partitioning/salting-out extraction with water/acetonitrile (QuEChERS-based approach). Combined with LC-MS/MS determination and isotope-dilution quantification, this method achieved robust analytical performances, including recoveries between 94.9 and 115.0%, repeatability and intermediate reproducibility below 17.7%. Limits of quantification were set at the lowest validated levels (0.05 μg/kg for powdered infant formula and oils and 0.005 μg/kg for liquid formula), meeting the requirements derived from the EFSA acute reference dose (ARfD) for cereulide. The determination of cereulide extraction yield on a set of samples confirmed the trueness of the QuEChERS-based procedure and highlighted the inefficiency of ISO 18465:2017 for powdered infant formula. Overall, this study provides compelling evidence that ISO 18465:2017 should not be applied to powdered infant formula and supports the adoption of a QuEChERS-based extraction as a reliable, accurate, and operationally efficient method for routine monitoring of cereulide.

PMID:
42320125
Bibliographic data and abstract were imported from PubMed on 20 Jun 2026.

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