LC-MS/MS multi-analyte method for mycotoxin determination in food supplements

Area of Science:

• Analytical Chemistry
• Food Science
• Mass Spectrometry

Background:

• Mycotoxins are toxic secondary metabolites produced by fungi that can contaminate food products, including dietary supplements.
• Ensuring the safety of food supplements requires reliable analytical methods for detecting a wide range of mycotoxins.

Purpose of the Study:

• To develop and validate a multi-analyte method for determining 23 mycotoxins in food supplements using liquid chromatography-tandem mass spectrometry (LC-MS/MS).
• To assess the applicability of the method across various food supplement matrices.

Main Methods:

• Simultaneous extraction and sample pretreatment optimized using maca (Lepidium meyenii) supplements.
• Extraction with ethyl acetate/formic acid, followed by liquid-liquid partition with n-hexane and clean-up on Oasis HLB cartridges.
• Analysis using an Acquity UPLC system coupled to a triple quadrupole mass spectrometer with an electrospray interface.

Main Results:

• The method achieved limits of detection (LOD) and quantification (LOQ) in the range of 0.3–30 ng g⁻¹ and 1–100 ng g⁻¹, respectively.
• Recovery yields exceeded 60% for most mycotoxins, with good precision and trueness demonstrated.
• The method was successfully applied to various food supplements, with the standard addition approach used to address matrix effects.

Conclusions:

• A robust LC-MS/MS method was established for the simultaneous determination of 23 mycotoxins in diverse food supplements.
• The majority of analyzed food supplement samples (56/62) were found to be free of the target mycotoxins.
• Fumonisins (B1, B2, B3) and ochratoxin A were the primary mycotoxins detected in positive samples, highlighting their potential presence in these products.