Simultaneous determination of deoxynivalenol, and 15- and 3-acetyldeoxynivalenol in cereals by HPLC-UV detection
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Fusarium head blight is an important cereal crop disease, which not only causes yield losses but also mycotoxin contamination in wheat and other cereal grains. Developing an accurate, rapid and efficient assay is critical to minimise the risk ofFusarium mycotoxins for human and animal health. In this study, HPLC with UV detection was used to separate and quantify deoxynivalenol, 15-acetyldeoxynivalenol and 3-acetyldeoxynivalenol in cereals. Samples were extracted with water, and the extracting solution was precipitated by adding an equal volume of ethanol followed by solid-phase extraction. The analytes were separated on a reversed-phase C18 column by a mobile phase composed of acetonitrile and 1 mM H3PO4 with gradient elution. 15- and 3-acetyldeoxynivalenol showed effective baseline separation. All analytes were well-resolved from matrix co-extractives and detected at 224 nm. The results showed good linearity of calibration curves (R2 ranged from 0.997 to 0.999) and excellent precision for inter- and intra-day determinations. Average recovery rates for the tested matrices ranged from 71 to 92%. The limits of detection and quantification ranged from 16 to 25 ng/g and 48 to 60 ng/g, respectively. The results indicate that the feasibility and practicality of the presented LC-UV method are excellent and that the method is suitable for routine analysis of DON and its acetyl derivatives in cereal grains.
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Simultaneous determination of deoxynivalenol, and 15- and 3-acetyldeoxynivalenol in cereals by HPLC-UV detection
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Fusarium head blight is an important cereal crop disease, which not only causes yield losses but also mycotoxin contamination in wheat and other cereal grains. Developing an accurate, rapid and efficient assay is critical to minimise the risk ofFusarium mycotoxins for human and animal health. In this study, HPLC with UV detection was used to separate and quantify deoxynivalenol, 15-acetyldeoxynivalenol and 3-acetyldeoxynivalenol in cereals. Samples were extracted with water, and the extracting solution was precipitated by adding an equal volume of ethanol followed by solid-phase extraction. The analytes were separated on a reversed-phase C18 column by a mobile phase composed of acetonitrile and 1 mM H3PO4 with gradient elution. 15- and 3-acetyldeoxynivalenol showed effective baseline separation. All analytes were well-resolved from matrix co-extractives and detected at 224 nm. The results showed good linearity of calibration curves (R2 ranged from 0.997 to 0.999) and excellent precision for inter- and intra-day determinations. Average recovery rates for the tested matrices ranged from 71 to 92%. The limits of detection and quantification ranged from 16 to 25 ng/g and 48 to 60 ng/g, respectively. The results indicate that the feasibility and practicality of the presented LC-UV method are excellent and that the method is suitable for routine analysis of DON and its acetyl derivatives in cereal grains.
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