Multiresidue Mycotoxin Analysis in Corn Grain by Column High-Performance Liquid Chromatography with Postcolumn Photochemical and Chemical Derivatization: Single-Laboratory Validation

Abstract

A multiresidue method was developed and validated for simultaneous analysis of 5 families of mycotoxins in corn grain. Deoxynivalenol (DON); aflatoxins B1, B2, G1, G2; ochratoxin A; zearalenone; and fumonisins FB1 and FB2 are extracted from corn grain samples with watermethanol, and extracts are cleaned up using immunoaffinity and solid-phase extraction columns. The column high-performance liquid chromatographic method uses postcolumn photochemical derivatization for detection of aflatoxins and derivatization with o-phthalaldehyde for detection of fumonisins. Mean recoveries and relative standard deviation values () over studied fortification levels for the chosen matrixes were: DON 89.9, 8.7; aflatoxin B1 85, 9.4; aflatoxin B2 82.4, 9.7; aflatoxin G1 74.8, 13.5; aflatoxin G2 79.2, 10.0; fumonisin B1 96.2, 8.0; fumonisin B2 84.5, 6.4; zearalenone 91.7, 11.5; and ochratoxin A 87.4, 15.8. The method performance criteria, including specificity, accuracy, repeatability, operational range, and detection limits, were found to be within specifications set by the Feed Additives and Contaminants Group of the AOAC Agricultural Materials Community.

Mycotoxin Detection in Maize, Commercial Feed, and Raw Dairy Milk Samples from Assiut City, Egypt

“…During the past few years, the simultaneous determination of several toxins in one analytical run was developed with the aim of reducing time and cost of the analysis and to get a better evidence of multi-mycotoxin occurrence in agriculture commodities [9,15,17]. HPLC has proved to be a powerful tool for mycotoxin detection and quantification.…”

“…The chromatographic parameters for the analysis are described in Ofitserova et al (2009) [9]. Chromatographic separation was performed by using an Agilent 1100 HPLC equipped with an ACE ® C18 column (25 cm × 4.6 mm, particle size 5 µm) and a C18 4 × 3 mm i.d.…”

“…On the other hand, several methods have been developed in order to simultaneously detect mycotoxins in different matrices, especially maize and feeds, using HPLC coupled with a fluorescence detector (FLD) [8,9]. The literature shows that most of the previous surveys conducted in Egypt have focused on a single or a few mycotoxins in maize and/or feed using screening methods for qualitative detection.…”

Occurrence, Toxicity, and Analysis of Major Mycotoxins in Food

“…By this technique, it is possible to obtain sensitivity that is comparable to those achieved by LC-MS/MS; however, HPLC-FLD methods are usually most suitable for single mycotoxins or a group of chemically related mycotoxins [ 93 , 94 ]. Recently, a HPLC-FLD method has been employed for the simultaneous detection of multiple mycotoxins: (1) AFs and OTA in maize cereal products, peanut butter, ginseng and ginger [ 95 , 96 ]; (2) AFs, OTA, and ZEA in cereal grains, rye and rice [ 97 , 98 ]; (3) AFs, OTA, ZEA and DON in corn [ 99 ]. Although these HPLC-FLD detection methods have relatively good sensitivity and recovery, the requirement for extensive cleanup and pre-/post-column derivatization for proper detection of mycotoxins are downsides.…”

Development of an Improved Method of Sample Extraction and Quantitation of Multi-Mycotoxin in Feed by LC-MS/MS

“…A variety of analytical instrumentations have been reported for mycotoxins such as TLC, GC-MS, LC-MS, HPLC-FLD, HPLC-UV and LC-MS/MS [17][18][19][20][21]. Liquid chromatography coupled with triple mass spectroscopy is the most recognized analytical instrumentation for the wide range of chemical contaminants such as mycotoxins in agricultural commodities.…”