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Development and in-house validation of a robust and sensitive solid-phase extraction liquid chromatography/tandem mass spectrometry method for the quantitative determination of aflatoxins B1, B2, G1, G2, ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2 toxins in cereal-based foods.
Rapid Commun Mass Spectrom. 2011 Jul 15; 25(13):1869-80.RC

Abstract

A sensitive and robust liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was developed for the simultaneous determination of aflatoxins (B(1), B(2), G(1), G(2)), ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2 toxins in cereal-based foods. Samples were extracted with a mixture of acetonitrile/water (84:16, v/v) and cleaned up through a polymeric solid-phase extraction column. Detection and quantification of the nine mycotoxins were performed by reversed-phase liquid chromatography coupled with electrospray ionization triple quadrupole mass spectrometry (LC/ESI-MS/MS), using fully (13)C-isotope-labelled mycotoxins as internal standards. The method was validated in-house for five different cereal processed products, namely barley, oat and durum wheat flours, rye- and wheat-based crisp bread. Recoveries and repeatability of the whole analytical procedure were evaluated at contamination levels encompassing the EU maximum permitted levels for each tested mycotoxin. Recoveries ranged from 89 to 108% for deoxynivalenol, from 73 to 114% for aflatoxins, from 85 to 114% for T-2 and HT-2 toxins, from 64 to 97% for zearalenone, from 74 to 102% for ochratoxin A. Relative standard deviations were less than 16% for all tested mycotoxins and matrices. Limits of detection (signal-to-noise ratio 3:1) ranged from 0.1 to 59.2 µg/kg. The trueness of the results obtained by the proposed method was demonstrated by analysis of reference materials for aflatoxins, deoxynivalenol, zearalenone. The use of inexpensive clean-up cartridges and the increasing availability of less expensive LC/MS/MS instrumentation strengthen the potential of the proposed method for its effective application for reliable routine analysis to assess compliance of tested cereal products with current regulation.

Authors+Show Affiliations

Institute of Sciences of Food Production, National Research Council of Italy (ISPA-CNR), via Amendola 122/O, 70126 Bari, Italy. veronica.lattanzio@ispa.cnr.itNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

21638363

Citation

Lattanzio, Veronica M T., et al. "Development and In-house Validation of a Robust and Sensitive Solid-phase Extraction Liquid Chromatography/tandem Mass Spectrometry Method for the Quantitative Determination of Aflatoxins B1, B2, G1, G2, Ochratoxin A, Deoxynivalenol, Zearalenone, T-2 and HT-2 Toxins in Cereal-based Foods." Rapid Communications in Mass Spectrometry : RCM, vol. 25, no. 13, 2011, pp. 1869-80.
Lattanzio VM, Gatta SD, Suman M, et al. Development and in-house validation of a robust and sensitive solid-phase extraction liquid chromatography/tandem mass spectrometry method for the quantitative determination of aflatoxins B1, B2, G1, G2, ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2 toxins in cereal-based foods. Rapid Commun Mass Spectrom. 2011;25(13):1869-80.
Lattanzio, V. M., Gatta, S. D., Suman, M., & Visconti, A. (2011). Development and in-house validation of a robust and sensitive solid-phase extraction liquid chromatography/tandem mass spectrometry method for the quantitative determination of aflatoxins B1, B2, G1, G2, ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2 toxins in cereal-based foods. Rapid Communications in Mass Spectrometry : RCM, 25(13), 1869-80. https://doi.org/10.1002/rcm.5047
Lattanzio VM, et al. Development and In-house Validation of a Robust and Sensitive Solid-phase Extraction Liquid Chromatography/tandem Mass Spectrometry Method for the Quantitative Determination of Aflatoxins B1, B2, G1, G2, Ochratoxin A, Deoxynivalenol, Zearalenone, T-2 and HT-2 Toxins in Cereal-based Foods. Rapid Commun Mass Spectrom. 2011 Jul 15;25(13):1869-80. PubMed PMID: 21638363.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Development and in-house validation of a robust and sensitive solid-phase extraction liquid chromatography/tandem mass spectrometry method for the quantitative determination of aflatoxins B1, B2, G1, G2, ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2 toxins in cereal-based foods. AU - Lattanzio,Veronica M T, AU - Gatta,Stefania Della, AU - Suman,Michele, AU - Visconti,Angelo, PY - 2011/6/4/entrez PY - 2011/6/4/pubmed PY - 2011/9/2/medline SP - 1869 EP - 80 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 25 IS - 13 N2 - A sensitive and robust liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was developed for the simultaneous determination of aflatoxins (B(1), B(2), G(1), G(2)), ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2 toxins in cereal-based foods. Samples were extracted with a mixture of acetonitrile/water (84:16, v/v) and cleaned up through a polymeric solid-phase extraction column. Detection and quantification of the nine mycotoxins were performed by reversed-phase liquid chromatography coupled with electrospray ionization triple quadrupole mass spectrometry (LC/ESI-MS/MS), using fully (13)C-isotope-labelled mycotoxins as internal standards. The method was validated in-house for five different cereal processed products, namely barley, oat and durum wheat flours, rye- and wheat-based crisp bread. Recoveries and repeatability of the whole analytical procedure were evaluated at contamination levels encompassing the EU maximum permitted levels for each tested mycotoxin. Recoveries ranged from 89 to 108% for deoxynivalenol, from 73 to 114% for aflatoxins, from 85 to 114% for T-2 and HT-2 toxins, from 64 to 97% for zearalenone, from 74 to 102% for ochratoxin A. Relative standard deviations were less than 16% for all tested mycotoxins and matrices. Limits of detection (signal-to-noise ratio 3:1) ranged from 0.1 to 59.2 µg/kg. The trueness of the results obtained by the proposed method was demonstrated by analysis of reference materials for aflatoxins, deoxynivalenol, zearalenone. The use of inexpensive clean-up cartridges and the increasing availability of less expensive LC/MS/MS instrumentation strengthen the potential of the proposed method for its effective application for reliable routine analysis to assess compliance of tested cereal products with current regulation. SN - 1097-0231 UR - https://www.unboundmedicine.com/medline/citation/21638363/Development_and_in_house_validation_of_a_robust_and_sensitive_solid_phase_extraction_liquid_chromatography/tandem_mass_spectrometry_method_for_the_quantitative_determination_of_aflatoxins_B1_B2_G1_G2_ochratoxin_A_deoxynivalenol_zearalenone_T_2_and_HT_2_toxins_in_cereal_based_foods_ L2 - https://doi.org/10.1002/rcm.5047 DB - PRIME DP - Unbound Medicine ER -