A rapid and sensitive method for the control of selected regulated and emerging mycotoxins in beer

Abstract

A fast method using automated online solid-phase extraction (SPE) coupled to liquid-chromatography/high resolution mass spectrometric (LC-HRMS) detection for the determination of 12 mycotoxins in beer was developed and fully validated according to the performance criteria set in the European Union (EU) guidelines. Mycotoxin detection was achieved by full-scan HRMS with electrospray ionisation in positive ion mode within 13 min. No significant matrix interferences were observed. The lowest limits of detection (LODs) were achieved for emerging mycotoxins (beauvericin and enniatins) and ochratoxin A at levels between 0.01 and 0.02 μg/l, while the overall LODs were in the range of 0.01-0.30 μg/l. The elaborated method showed good performance in the analysis of beer samples with good linearity (R2>0.999), intra-day and inter-day precision at the levels of <12% and <13%, respectively, and recoveries in the range of 80-119%. Finally, this fully automated, sensitive, and reliable online SPE-HPLC-HRMS method was successfully applied for the analysis of 25 Latvian beers and the obtained results were comparable or even better than those obtained using the well-established Quick, Easy, Cheap, Effective, Rugged, and Safe, the QuEChERS, methodology.