title: Exploring the potentialities of an improved ultrasound-assisted quick, easy, cheap, effective, rugged, and safe-based extraction technique combined with ultrahigh pressure liquid chromatography-fluorescence detection for determination of Zearalenone in cereals.
abstract: Zearalenone (ZEA), a secondary metabolite from Fusarium graminearum fungi that invade crops and grow during blooming in moist cool field conditions, is a nonsteroidal oestrogen, biologically very potent, although hardly toxic. Different analytical methods, among which a quick, easy, cheap, effective, rugged, and safe (QuEChERS) strategy, combined with or liquid chromatography, have been proposed for ZEA determination in foods. However, this extraction procedure has the disadvantage of using large amount of organic solvents, partitioning salts and sample volume, which limits the technique application on the fields where the sample amount is critical. Therefore in this work an improved sample preparation step based on the original QuEChERS (O-QuEChERS) approach, the μ-QuEChERS, combined with ultrasound-assisted extraction (USAE) and ultrahigh pressure liquid chromatography (UHPLC) analysis with fluorescence detection (FLR) is proposed for the sensitive and high-throughput quantification of ZEA in cereals. The proposed analytical strategy, μ-QuEChERSUSAE, uses up to 32 times lower amounts of partitioning salts, lower sample amount and lower extraction solvents, in comparison with O-QuEChERS technique. The performance of the analytical approach was assessed by studying the selectivity, specificity, limits of detection and quantification, linear dynamic range, matrix effect and precision. Good linearity (r(2)>0.99) was achieved for ZEA, and limits of detection (LOD=3.4μgkg(-1)) and limits of quantification (LOQ=4.7μgkg(-1)) were found below the tolerance levels set by European Commission. Good recoveries were obtained with different spiked concentrations, ranged from 80.2% to 109.7%, with relative standard deviations (RSD) lower than 5.0%. The comparison of the analytical performance of the proposed μ-QuEChERSUSAE with O-QuEChERS showed the powerful ability of the proposed strategy since it gives comparable results but using lower amounts of sample, partitioning salts and volume of the organic solvent, revealing of great potential and improvement of the proposed method.
authors.affiliation: CQM-UMa, Centro de Química da Madeira, Campus Universitário da Penteada, 9000-390 Funchal, Portugal.
authors.forename: Priscilla
authors.initials: P
authors.lastname: Porto-Figueira
authors.affiliation: Centro de Competência das Ciências da Vida, Universidade da Madeira, Campus da Penteada, 9000-390 Funchal, Portugal.
authors.forename: Irene
authors.initials: I
authors.lastname: Camacho
authors.affiliation: CQM-UMa, Centro de Química da Madeira, Campus Universitário da Penteada, 9000-390 Funchal, Portugal; Centro de Competências das Ciências Exactas e da Engenharia da Universidade da Madeira, Campus Universitário da Penteada, 9000-390 Funchal, Portugal. Electronic address: jsc@uma.pt.
authors.forename: José S
authors.initials: JS
authors.lastname: Câmara
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D002523:Edible Grain / Q000737:chemistry*; D005453:Fluorescence; D012680:Sensitivity and Specificity; D012997:Solvents; D013016:Sound; D053719:Tandem Mass Spectrometry / Q000379:methods; D015025:Zearalenone / Q000032:analysis*
chemical_list: D012997:Solvents; D015025:Zearalenone
keywords: Cereals; O-QuEChERS; Ultrahigh pressure liquid chromatography; Ultrasound assisted extraction; Zearalenone; μ-QuEChERS