title: 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.
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.
authors.affiliation: Nestlé Research Centre, Nestec Ltd, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland. Electronic address: aurelien.desmarchelier@rdls.nestle.com.
authors.forename: Aurélien
authors.initials: A
authors.lastname: Desmarchelier
authors.affiliation: Nestlé Research Centre, Nestec Ltd, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland.
authors.forename: Sabine
authors.initials: S
authors.lastname: Tessiot
authors.affiliation: Nestlé Research Centre, Nestec Ltd, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland.
authors.forename: Thomas
authors.initials: T
authors.lastname: Bessaire
authors.affiliation: Nestlé Research Centre, Nestec Ltd, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland.
authors.forename: Lucie
authors.initials: L
authors.lastname: Racault
authors.affiliation: Nestle Quality Assurance Center, Via Valsugana 5, 35010 San Giorgio in Bosco, Italy.
authors.forename: Elisa
authors.initials: E
authors.lastname: Fiorese
authors.affiliation: Nestle Quality Assurance Center, Via Valsugana 5, 35010 San Giorgio in Bosco, Italy.
authors.forename: Alessandro
authors.initials: A
authors.lastname: Urbani
authors.affiliation: Nestle Quality Assurance Center, 29 Quality Road, Singapore 618802, Singapore.
authors.forename: Wai-Chinn
authors.initials: WC
authors.lastname: Chan
authors.affiliation: Nestle Quality Assurance Center, 29 Quality Road, Singapore 618802, Singapore.
authors.forename: Pearly
authors.initials: P
authors.lastname: Cheng
authors.affiliation: Nestlé Research Centre, Nestec Ltd, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland.
authors.forename: Pascal
authors.initials: P
authors.lastname: Mottier
mesh_terms: D002099:Cacao / Q000737:chemistry; D002247:Carbon Isotopes; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D003069:Coffee / Q000737:chemistry; D006801:Humans; D007201:Indicator Dilution Techniques; D007223:Infant; D007225:Infant Food; D007231:Infant, Newborn; D059021:Laboratory Proficiency Testing; D009183:Mycotoxins / Q000032:analysis*; D011786:Quality Control; D012680:Sensitivity and Specificity; D017365:Spices / Q000032:analysis; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D002247:Carbon Isotopes; D003069:Coffee; D009183:Mycotoxins
keywords: Immunoaffinity cleanup; Isotope dilution; LC–MS/MS; Mycotoxins; QuEChERS