title: Optimisation of a sample preparation method for the determination of fumonisin B(1) in rice.
abstract: A simple, rapid and cost-effective sample preparation method for the determination of fumonisin B1 in rice was optimised using a strategy of sequential experimental designs. Initially, a Plackett-Burman design was applied to select the statistically significant variables for the determination of fumonisin B1, and then, a central composite rotatable design was used to define the optimal conditions of these variables. The method involves extraction with a 50% acetonitrile aqueous solution and glacial acetic acid, liquid-liquid partitioning with addition of anhydrous sodium sulphate and sodium chloride, followed by dispersive SPE clean-up with diatomaceous earth. The final extract was analysed by HPLC-FLD after precolumn derivatisation with ortho-phthaldialdehyde. The optimised method was validated for selectivity, linearity, matrix effect, limits of detection and quantification, trueness, and precision, and then applied to commercial samples of polished rice. This is the first report of the occurrence of fumonisin B1 in commercial samples of polished rice from the Southeast region of Brazil.
authors.affiliation: Department of Food and Nutrition, Faculty of Pharmaceutical Sciences, São Paulo State University (UNESP), P.O. Box 502, 14801-902 Araraquara, SP, Brazil. Electronic address: mateuspetrarca@ig.com.br.
authors.forename: Mateus Henrique
authors.initials: MH
authors.lastname: Petrarca
authors.affiliation: Department of Food Engineering, Faculty of Food Engineering, University of Campinas (UNICAMP), P.O. Box 6121, 13083-970 Campinas, SP, Brazil.
authors.forename: Maria Isabel
authors.initials: MI
authors.lastname: Rodrigues
authors.affiliation: Department of Food and Nutrition, Faculty of Pharmaceutical Sciences, São Paulo State University (UNESP), P.O. Box 502, 14801-902 Araraquara, SP, Brazil.
authors.forename: Elizeu Antonio
authors.initials: EA
authors.lastname: Rossi
authors.affiliation: Department of Food and Nutrition, Faculty of Pharmaceutical Sciences, São Paulo State University (UNESP), P.O. Box 502, 14801-902 Araraquara, SP, Brazil.
authors.forename: Célia Maria
authors.initials: CM
authors.lastname: de Sylos
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D037341:Fumonisins / Q000737:chemistry*; D012275:Oryza / Q000737:chemistry*
chemical_list: D037341:Fumonisins; C056933:fumonisin B1
keywords: Fumonisin B(1); In-house validation; Plackett–Burman design; Response surface methodology; Rice; Sample preparation