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      Combining the quick, easy, cheap, effective, rugged and safe approach and clean-up by immunoaffinity column for the analysis of 15 mycotoxins by isotope dilution liquid chromatography tandem mass spectrometry.

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          Abstract

          Optimization and validation of a multi-mycotoxin method by LC-MS/MS is presented. The method covers the EU-regulated mycotoxins (aflatoxins, fumonisins, ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2), as well as nivalenol and 3- and 15-acetyldeoxynivalenol for analysis of cereals, cocoa, oil, spices, infant formula, coffee and nuts. The proposed procedure combines two clean-up strategies: First, a generic preparation suitable for all mycotoxins based on the QuEChERS (for quick, easy, cheap, effective, rugged and safe) protocol. Second, a specific clean-up devoted to aflatoxins and ochratoxin A using immunoaffinity column (IAC) clean-up. Positive identification of mycotoxins in matrix was conducted according to the confirmation criteria defined in EU Commission Decision 2002/657/EC while quantification was performed by isotopic dilution using (13)C-labeled mycotoxins as internal standards. Limits of quantification were at or below the maximum levels set in the EC/1886/2006 document for all mycotoxin/matrix combinations under regulation. In particular, the inclusion of an IAC step allowed achieving LOQs as low as 0.05 and 0.25μg/kg in cereals for aflatoxins and ochratoxin A, respectively. Other performance parameters like linearity [(r)(2)>0.99], recovery [71-118%], precision [(RSDr and RSDiR)<33%], and trueness [78-117%] were all compliant with the analytical requirements stipulated in the CEN/TR/16059 document. Method ruggedness was proved by a verification process conducted by another laboratory.

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          Author and article information

          Journal
          J Chromatogr A
          Journal of chromatography. A
          Elsevier BV
          1873-3778
          0021-9673
          Apr 11 2014
          : 1337
          Affiliations
          [1 ] Nestlé Research Centre, Nestec Ltd, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland. Electronic address: aurelien.desmarchelier@rdls.nestle.com.
          [2 ] Nestlé Research Centre, Nestec Ltd, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland.
          [3 ] Nestle Quality Assurance Center, Via Valsugana 5, 35010 San Giorgio in Bosco, Italy.
          [4 ] Nestle Quality Assurance Center, 29 Quality Road, Singapore 618802, Singapore.
          Article
          S0021-9673(14)00255-6
          10.1016/j.chroma.2014.02.025
          24636559

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