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In-house validation of a rapid and efficient procedure for simultaneous determination of ergot alkaloids and other mycotoxins in wheat and maize

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Abstract
A fundamental step in addressing the global problem of mycotoxins is the development of highly sensitive, multi-class extraction and detection methods. This constitutes a field of research that has in recent years enjoyed a steady advance. Such methods, generally based on liquid chromatography coupled to mass spectrometry, are widely reported successfully detecting various mycotoxins in different food and feed samples. In this work, an innovative approach to multi-class mycotoxin control is proposed, offering specific advantages: a broader inclusion of more mycotoxin classes, robust and thorough extraction for all target compounds despite their varied chemical properties, and determination of all analytes from a single injection. The method involved the extraction and quantification of the main mycotoxins produced by Aspergillus, Fusarium, and Penicillium fungi, as well as their reported derivatives, together with 12 other compounds most commonly produced by Claviceps purpurea. The popularly reported QuEChERS technique has been reduced to a simple "salting-out liquid-liquid extraction" (SO-LLE) to obtain the most efficient extraction of the aforementioned mycotoxin classes in a very short time. This is in particular extremely important in ensuring correct determination of individual ergot alkaloids, for which short and robust sample preparation as well as short analytical sequences were key for minimizing the epimerization during analysis. The analyses of wheat and maize samples were performed using ultra-high performance liquid chromatography coupled with tandem mass spectrometry. Matrix-matched calibration curves were established and limits of quantification were below the maximum levels established by the EU regulation. The precision (repeatability and intermediate precision) was lower than 13% in all cases and recoveries ranged between 60 and 98% in maize and between 62 and 103% in wheat, fulfilling the current legislation. The method was applied to study the co-occurrence of these mycotoxins in wheat (n = 13) and maize (n = 15) samples from six European countries. A successful quantification of 23 different mycotoxins, from all major classes, in 85% of wheat and 93% of maize samples was achieved
Keywords
Mycotoxins, Co-occurrence, Cereals, Ultra-high performance liquid chromatography, Mass spectrometry, QuEChERS, SO-LLE, LC-MS/MS METHOD, INTESTINAL EPITHELIAL-CELLS, TANDEM MASS-SPECTROMETRY, QUANTIFICATION, FLOUR, FOOD, DEOXYNIVALENOL, METABOLITES, CEREALS, SAMPLES

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Citation

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Chicago
Arroyo-Manzanares, Natalia, Karl De Ruyck, Valdet Uka, Laura Gamiz-Gracia, Ana M Garcia-Campana, Sarah De Saeger, and José Diana Di Mavungu. 2018. “In-house Validation of a Rapid and Efficient Procedure for Simultaneous Determination of Ergot Alkaloids and Other Mycotoxins in Wheat and Maize.” Analytical and Bioanalytical Chemistry 410 (22): 5567–5581.
APA
Arroyo-Manzanares, N., De Ruyck, K., Uka, V., Gamiz-Gracia, L., Garcia-Campana, A. M., De Saeger, S., & Diana Di Mavungu, J. (2018). In-house validation of a rapid and efficient procedure for simultaneous determination of ergot alkaloids and other mycotoxins in wheat and maize. ANALYTICAL AND BIOANALYTICAL CHEMISTRY, 410(22), 5567–5581.
Vancouver
1.
Arroyo-Manzanares N, De Ruyck K, Uka V, Gamiz-Gracia L, Garcia-Campana AM, De Saeger S, et al. In-house validation of a rapid and efficient procedure for simultaneous determination of ergot alkaloids and other mycotoxins in wheat and maize. ANALYTICAL AND BIOANALYTICAL CHEMISTRY. 2018;410(22):5567–81.
MLA
Arroyo-Manzanares, Natalia, Karl De Ruyck, Valdet Uka, et al. “In-house Validation of a Rapid and Efficient Procedure for Simultaneous Determination of Ergot Alkaloids and Other Mycotoxins in Wheat and Maize.” ANALYTICAL AND BIOANALYTICAL CHEMISTRY 410.22 (2018): 5567–5581. Print.
@article{8582863,
  abstract     = {A fundamental step in addressing the global problem of mycotoxins is the development of highly sensitive, multi-class extraction and detection methods. This constitutes a field of research that has in recent years enjoyed a steady advance. Such methods, generally based on liquid chromatography coupled to mass spectrometry, are widely reported successfully detecting various mycotoxins in different food and feed samples. In this work, an innovative approach to multi-class mycotoxin control is proposed, offering specific advantages: a broader inclusion of more mycotoxin classes, robust and thorough extraction for all target compounds despite their varied chemical properties, and determination of all analytes from a single injection. The method involved the extraction and quantification of the main mycotoxins produced by Aspergillus, Fusarium, and Penicillium fungi, as well as their reported derivatives, together with 12 other compounds most commonly produced by Claviceps purpurea. The popularly reported QuEChERS technique has been reduced to a simple {\textacutedbl}salting-out liquid-liquid extraction{\textacutedbl} (SO-LLE) to obtain the most efficient extraction of the aforementioned mycotoxin classes in a very short time. This is in particular extremely important in ensuring correct determination of individual ergot alkaloids, for which short and robust sample preparation as well as short analytical sequences were key for minimizing the epimerization during analysis. The analyses of wheat and maize samples were performed using ultra-high performance liquid chromatography coupled with tandem mass spectrometry. Matrix-matched calibration curves were established and limits of quantification were below the maximum levels established by the EU regulation. The precision (repeatability and intermediate precision) was lower than 13\% in all cases and recoveries ranged between 60 and 98\% in maize and between 62 and 103\% in wheat, fulfilling the current legislation. The method was applied to study the co-occurrence of these mycotoxins in wheat (n = 13) and maize (n = 15) samples from six European countries. A successful quantification of 23 different mycotoxins, from all major classes, in 85\% of wheat and 93\% of maize samples was achieved},
  author       = {Arroyo-Manzanares, Natalia and De Ruyck, Karl and Uka, Valdet and Gamiz-Gracia, Laura and Garcia-Campana, Ana M and De Saeger, Sarah and Diana Di Mavungu, Jos{\'e}},
  issn         = {1618-2642},
  journal      = {ANALYTICAL AND BIOANALYTICAL CHEMISTRY},
  language     = {eng},
  number       = {22},
  pages        = {5567--5581},
  title        = {In-house validation of a rapid and efficient procedure for simultaneous determination of ergot alkaloids and other mycotoxins in wheat and maize},
  url          = {http://dx.doi.org/10.1007/s00216-018-1018-6},
  volume       = {410},
  year         = {2018},
}

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