Analysis of Deoxynivalenol, Masked Deoxynivalenol, and Fusarium graminearum Pigment in Wheat Samples, Using Liquid Chromatography-UV-Mass Spectrometry

Authors: Sasanya, J.J.1; Hall, C.2; Wolf-Hall, C.3

Source: Journal of Food Protection®, Volume 71, Number 6, June 2008 , pp. 1205-1213(9)

Publisher: International Association for Food Protection

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Abstract:

Tolerable limits set for deoxynivalenol (DON) do not consider DON conjugates such as DON-3-glucoside. Conjugates may be metabolized in vivo to DON. Such masked mycotoxins and the potentially toxic Fusarium pigment are not routinely analyzed in cereals. We quantified DON, DON-3-glucoside, and a red Fusarium pigment in hard red spring wheat, using a new liquid chromatography-mass spectrometry method. Extraction protocols using centrifugation and shaking, and methanol- methylene chloride (50:50 [vol/vol]) or acetonitrile-water (84:16 [vol/vol]) were assessed. Purposively and randomly selected hard spring wheat samples were extracted with solvent filtered through a C18 column and analyzed using liquid chromatography-UV-mass spectrometry. Isocratic mobile phase (70% methanol) was used. Recoveries were 96.4% (DON) and 70.0% (DON-3-glucoside), while limits of detection were 1 μg/kg (MS) and 10 μg/kg (UV), and limits of quantification were 1 μg/kg (UV) and 0.5 μg/kg (MS), respectively. The pigment limits of quantification and limits of detection on the MS were 4.3 and 0.0005 μg/kg, respectively. The purposively selected samples had DON, DON-3-glucoside, and pigment averages of 3.4 ± 4.0 μg/g, 3.8 ± 8.3 μg/g, and 0.31 ± 3.71 g/kg, respectively. The randomly selected spring wheat had lower mean levels of DON (1.4 ± 2.3 μg/g), DON-3-glucoside (0.2 ± 1.0 μg/g), and pigment (147.93 ± 247.84 μg/g). Analytical tools such as this new liquid chromatography-UV-mass spectrometry method can be used to quantify masked and parent mycotoxins, plus a potentially toxic pigment for risk assessment.

Document Type: Research article

Affiliations: 1: Great Plains Institute of Food Safety, North Dakota State University, Fargo, North Dakota 58105, USA 2: Great Plains Institute of Food Safety, North Dakota State University, Fargo, North Dakota 58105, USA; Department of Cereal and Food Sciences, North Dakota State University, Fargo, North Dakota 58105, USA 3: Great Plains Institute of Food Safety, North Dakota State University, Fargo, North Dakota 58105, USA; Department of Veterinary and Microbiological Sciences, North Dakota State University, Fargo, North Dakota 58105, USA

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