Determination of Mycotoxins Using Hollow Fiber Dispersive Liquid–Liquid–Microextraction (HF-DLLME) Prior to High-Performance Liquid Chromatography – Tandem Mass Spectrometry (HPLC - MS/MS)

Abstract

A modified hollow-fiber-supported dispersive liquid-liquid microextraction (HF-DLLME) method was developed for the determination of aflatoxins and ochratoxin A in food samples. The various parameters affecting the efficiency of extraction, such as pH, salt addition, extraction time, stirring rate, desorption time, type and volume of extractant and disperser solvents were carefully studied and optimized using two step strategies. The linearity of the evaluated results was 0.1 to 30 μg L⁻¹ for aflatoxins and 0.1 to 20 μg L⁻¹ for ochratoxin A, with regression coefficients (R²) exceeding 0.9990. The precision was satisfactory with relative standard deviation values less than 11%. The method accuracy was within the recommended range from 70% to 120% and analyte accuracy between 83% and 101%. The limits of detection and quantification were in the range from 0.04 to 0.06 μg L⁻¹ and 0.08 to 0.13 μg L⁻¹, respectively, for multi-aflatoxins, and 0.02 to 0.04 µg L⁻¹ and 0.08 to 0.10 µg L⁻¹, respectively, for ochratoxin A. The developed method was successfully applied for the determination of mycotoxins in food samples.

Keywords:

• Central composite design (CCD)
• high performance liquid chromatography – tandem mass spectrometry (HPLC - MS/MS)
• hollow fiber dispersive liquid–liquid–microextraction (HF-DLLME)
• response surface methodology (RSM)

Disclosure statement

No potential conflict of interest was reported by the authors.

Additional information

Funding

This work has been supported by the Postgraduate Research Fund of University Malaya under Grant PG171 2014 and Government of Malaysia FRGS fund under Grant FP058-2014A.