title: Automated solid-phase extraction coupled online with HPLC-FLD for the quantification of zearalenone in edible oil.
abstract: Established maximum levels for the mycotoxin zearalenone (ZEN) in edible oil require monitoring by reliable analytical methods. Therefore, an automated SPE-HPLC online system based on dynamic covalent hydrazine chemistry has been developed. The SPE step comprises a reversible hydrazone formation by ZEN and a hydrazine moiety covalently attached to a solid phase. Seven hydrazine materials with different properties regarding the resin backbone, pore size, particle size, specific surface area, and loading have been evaluated. As a result, a hydrazine-functionalized silica gel was chosen. The final automated online method was validated and applied to the analysis of three maize germ oil samples including a provisionally certified reference material. Important performance criteria for the recovery (70-120 %) and precision (RSDr <25 %) as set by the Commission Regulation EC 401/2006 were fulfilled: The mean recovery was 78 % and RSDr did not exceed 8 %. The results of the SPE-HPLC online method were further compared to results obtained by liquid-liquid extraction with stable isotope dilution analysis LC-MS/MS and found to be in good agreement. The developed SPE-HPLC online system with fluorescence detection allows a reliable, accurate, and sensitive quantification (limit of quantification, 30 μg/kg) of ZEN in edible oils while significantly reducing the workload. To our knowledge, this is the first report on an automated SPE-HPLC method based on a covalent SPE approach.
authors.affiliation: Department 1 Analytical Chemistry, Reference Materials, Federal Institute for Materials Research and Testing (BAM), Richard-Willstätter-Str. 11, 12489, Berlin, Germany.
authors.forename: Sarah S
authors.initials: SS
authors.lastname: Drzymala
authors.forename: Stefan
authors.initials: S
authors.lastname: Weiz
authors.forename: Julia
authors.initials: J
authors.lastname: Heinze
authors.forename: Silvia
authors.initials: S
authors.lastname: Marten
authors.forename: Carsten
authors.initials: C
authors.lastname: Prinz
authors.forename: Annett
authors.initials: A
authors.lastname: Zimathies
authors.forename: Leif-Alexander
authors.initials: LA
authors.lastname: Garbe
authors.forename: Matthias
authors.initials: M
authors.lastname: Koch
mesh_terms: D001331:Automation; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D002853:Chromatography, Liquid; D004867:Equipment Design; D005504:Food Analysis / Q000379:methods*; D006834:Hydrazines / Q000737:chemistry; D010938:Plant Oils / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000295:instrumentation / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods; D015025:Zearalenone / Q000032:analysis*
chemical_list: D006834:Hydrazines; D010938:Plant Oils; C029424:hydrazine; D015025:Zearalenone