High‐performance liquid chromatographic determination of multi‐mycotoxin in cereals and bean foodstuffs using interference‐removal solid‐phase extraction combined with optimized dispersive liquid–liquid microextraction

• Published in: Journal of separation science Vol. 40; no. 10; pp. 2141 - 2150
• Main Authors: Zhou, Jian, Xu, Jiao‐Jiao, Huang, Bai‐Fen, Cai, Zeng‐Xuan, Ren, Yi‐Ping
• Format: Journal Article
• Language: English
• Published: Germany Wiley Subscription Services, Inc 01.05.2017
• Subjects: Aflatoxins; Beans; central composite design; Cereals; Chromatography, High Pressure Liquid; Design optimization; Dispersion; dispersive liquid–liquid microextraction; Economic conditions; Edible Grain - chemistry; Extraction processes; Fluorescence; Food Contamination - analysis; High performance liquid chromatography; Interference; Liquid Phase Microextraction; Liquid-liquid extraction; multi‐mycotoxin; Mycotoxins; Mycotoxins - analysis; Pretreatment; Reference materials; Response surface methodology; Salting; Solid Phase Extraction; Zearalenone; central composite design; response surface methodology; multi-mycotoxin; solid-phase extraction; dispersive liquid-liquid microextraction
• ISSN: 1615-9306; 1615-9314
• DOI: 10.1002/jssc.201601326

A novel pre‐treatment was proposed for the simultaneous determination of aflatoxins, ochratoxin A and zearalenone in foodstuffs using high‐performance liquid chromatography with fluorescence detection. The analytical procedure was based on a first step using a quick, easy, cheap, effective, rugged, and safe based extraction procedure, followed by salting out and purification with a C18 solid‐phase extraction column as interference removal clean‐up. Subsequently, collected supernatant was subjected to dispersive liquid–liquid microextraction. Response surface methodology based on central composite design was employed to optimize conditions in the microextraction procedure. Under the optimum conditions, satisfactory analytical performance with recoveries ranging from 63.22 to 107.6% were achieved in different types of cereals and beans, as well as desirable precisions (0.81–8.13%). Limits of detections and quantifications for these six mycotoxins ranging from 0.03 to 13 μg/kg and 0.22 to 44 μg/kg, respectively, were obtained. Finally, the established method was successfully validated by four certified reference materials (P = 0.897 > 0.05) and applied to 79 samples from local markets.