Optimized and validated high-performance liquid chromatography method for the determination of deoxynivalenol and aflatoxins in cereals

Abstract

A simple, sensitive and accurate analytical method was optimized and developed for the determination of deoxynivalenol and aflatoxins in cereals intended for human consumption using high-performance liquid chromatography with diode array and fluorescence detection and a photochemical reactor for enhanced detection. A response surface methodology, using a fractional central composite design, was carried out for optimization of the water percentage at the beginning of the run (X1, 80-90%), the level of acetonitrile at the end of gradient system (X2, 10-20%) with the water percentage fixed at 60%, and the flow rate (X3, 0.8-1.2 mL/min). The studied responses were the chromatographic peak area, the resolution factor and the time of analysis. Optimal chromatographic conditions were: X1 = 80%, X2 = 10%, and X3 = 1 mL/min. Following a double sample extraction with water and a mixture of methanol/water, mycotoxins were rapidly purified by an optimized solid-phase extraction protocol. The optimized method was further validated with respect to linearity (R(2) >0.9991), sensitivity, precision, and recovery (90-112%). The application to 23 commercial cereal samples from Greece showed contamination levels below the legally set limits, except for one maize sample. The main advantages of the developed method are the simplicity of operation and the low cost.

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

“…With better separation and stronger retention of AFs, the ODS‐4 column was selected for following optimization. In previous literatures, the mixture of acetonitrile and methanol was widely used as organic phase for separating AFs . Because of higher proportion of acetonitrile causing faster elution and deficient separation of AFs, a ratio of methanol/acetonitrile at 7:3 was chosen finally.…”

“…As mentioned previously, only few methods have been published for the determination of these mycotoxins using HPLC–FLD. A summarized list is given in Table to obtain a direct comparison between the present work and previous DLLME applications on mycotoxins . As shown, most of the listed works were accessible for aflatoxins group only or two groups at most, moreover, the applicable matrices were also restricted.…”

The Potential Application of Nanoparticles on Grains during Storage: Part 1 – An Overview of Inhibition against Fungi and Mycotoxin Biosynthesis

“…The impact of the sampling on sample preparation and analytical instrument contribute to the total variance during the analysis of ochratoxin A (OTA) in flour and aflatoxinB1 (AFB1) in oats was recently reported. The authors suggested that increasing sample weight (size) could potentially reduce the high heterogeneity encountered [96,97]. For efficient extraction, methods of detection and quantification of mycotoxins, the reader(s) are referred to the following good sources [95,[98][99][100][101].…”

Current methods for mycotoxins analysis and innovative strategies for their reduction in cereals: an overview

“…The majority of mycotoxins are soluble in polar solvents and insoluble in apolar solvents . The most common solvents that have been used in different studies for the extraction of mycotoxins from cereals are polar or relatively polar solvents, such as water, acetone, acetonitrile, methanol, chloroform or a mixture of them . In the case of fumonisins, an acidified solvent favours the protonation of carboxylic groups with a consequent improved separation from the matrix …”