In this study, the new approach of dispersive micro-solid phase extraction using a magnetic sheet was developed. A circle magnetic sheet (diameter, 25 mm; thickness, 0.4 mm) was perforated and used as a support for fixing and re-collecting three-dimensional magnetic graphene nanoparticles as an adsorbent. The method was coupled with high-performance liquid chromatography-fluorescence detector (HPLC-FLD) and utilized for extraction of aflatoxins (B1, B2, G1, and G2). All steps of the extraction procedure including sample loading, sorbent dispersion, and re-collecting, and elution were performed using a syringe. The significant parameters such as adsorbent amount, desorption conditions, flow rates, ionic strength, and pH which influence extraction efficiency was investigated. The linear dynamic range was 0.2–1000 μg kg−1, with a coefficient of determinations > 0.9914. The limits of detection and quantification were 0.06–0.1 and 0.20–0.33 μg kg−1, respectively. The developed method was applied to the analysis of aflatoxins in real white and moldy bread samples, and the related extraction recoveries of the four aflatoxins were obtained in the range of 59–69% (RSD, 4.4–5.6%).
Aflatoxins HPLC In-syringe magnetic dispersive solid phase microextraction Magnetic three-dimensional graphene Perforated magnetic sheet
This is a preview of subscription content, log in to check access.
The authors received financial support from the Iran National Science Foundation (INSF) through Research Grants.
Compliance with Ethical Standards
Conflict of Interest
Hassan Sereshti declares that he has no conflict of interest. Farnaz Khodayari declares that he has no conflict of interest. Nina Nouri declares that he has no conflict of interest.
This article does not contain any studies with human or animal subjects.
A statement regarding “informed consent” is not applicable.
Andrade PD, da Silva JLG, Caldas ED (2013) Simultaneous analysis of aflatoxins B1, B2, G1, G2, M1, and ochratoxin A in breast milk by high-performance liquid chromatography/fluorescence after liquid–liquid extraction with low temperature purification (LLE–LTP). J Chromatogr A 1304:61–68CrossRefGoogle Scholar
Augusto F, Hantao L, Mogollo’n N, Braga S (2013) New materials and trends in sorbents for solid-phase extraction. TrAC Trends Anal Chem 43:14–23CrossRefGoogle Scholar
Brera C, Debegnach F, De Santis B, Pannunzi E, Berdini C, Prantera E, Gregori E, Miraglia M (2012) Simultaneous determination of aflatoxins and ochratoxin A in baby foods and paprika by HPLC with fluorescence detection: a single-labor. Talanta 83:1442–1446CrossRefGoogle Scholar
Campone L, Piccinelli AL, Celano R, Rastrelli L (2012) Application of dispersive liquid–liquid microextraction for the determination of aflatoxins B1, B2, G1 and G2 in cereal products. J Chromatogr A 1218:7648–7654CrossRefGoogle Scholar
Cavaliere C, Foglia P, Guarino C, Nazzari M, Samperi R, Lagana A (2007) Determination of aflatoxins in olive oil by liquid chromatography–tandem mass spectrometry. Anal Chim Acta 596:141–148CrossRefGoogle Scholar
Chen D, Cao X, Tao Y, Wu Q, Pan Y, Huang L, Wang X, Wang Y, Peng D, Liu Z, Yuan Z (2012) Development of a sensitive and robust liquid chromatography coupled with tandem mass spectrometry and a pressurized liquid extraction for the determination of aflatoxins and ochratoxin A in animal derived foods. J Chromatogr A 1253:110–119CrossRefGoogle Scholar
Deng H, Li X, Peng Q, Wang X, Chen J, Li Y (2005) Monodisperse magnetic single-crystal ferrite microspheres. Angew Chem 117:2842–2845CrossRefGoogle Scholar
Di Stefano V, Pitonzo R, Avellone G, Di Fiore A, Monte L, Tabis Ogorka AZ (2015) Determination of aflatoxins and ochratoxins in sicilian sweet wines by high-performance liquid chromatography with fluorometric detection and immunoaffinity cleanup. Food Anal Methods 8:596–577CrossRefGoogle Scholar
Dos Reis LC, Vidal L, Canals A (2017) Graphene oxide/Fe3O4 as sorbent for magnetic solid-phase extraction coupled with liquid chromatography to determine 2,4,6-trinitrotoluene in water samples. Anal Bioanal Chem 409:2665–2674CrossRefGoogle Scholar
Elsanhoty RM, Fawzy Ramadan M, El-Gohery SS, Abol-Ela MF, Azeke MA (2013) Ability of selected microorganisms for removing aflatoxins in vitro and fate of aflatoxins in contaminated wheat during baladi bread baking. Food Control 33:287–292CrossRefGoogle Scholar
Es’haghi Z, Sorayaei H, Samadi F, Masrournia M, Bakherad Z (2011) Fabrication of a novel nanocomposite based on sol–gel process for hollow fiber–solid phase microextraction of aflatoxins: B1 and B2 in cereals combined with high performance liquid chromatography–diode array detection. J Chromatogr B 879:3034–3040CrossRefGoogle Scholar
European commission, (EC) No 1881/2006 (2006). Off J Eur Union 364:5-24.Google Scholar
Folloni S, Bellocchi G, Kagkli DM, Pastor-Benito S, Aguilera M, Mazzeo A, Querci M, Van den Eede G, Ermolli M (2011) Development of an ELISA reverse-based assay to assess the presence of mycotoxins in cereal flour. Food Anal Methods 4:221–227CrossRefGoogle Scholar
Han Z, Zheng Y, Luan L, Cai Z, Ren Y, Wu Y (2010) An ultra-high performance liquid chromatography–tandem mass spectrometry method for simultaneous determination of aflatoxins B1, B2, G1, G2, M1 and M2 in traditional Chinese medicines. Anal Chim Acta 664:165–171CrossRefGoogle Scholar
Hashemi M, Taherimaslak Z, Rashidib S (2014) Application of magnetic solid phase extraction for separation and determination of aflatoxins B1 and B2 in cereal products by high performance liquid chromatography-fluorescence detection. J Chromatogr B 960:200–208CrossRefGoogle Scholar
Hassan J, Habibi S (2011) Reverse homogeneous liquid–liquid extraction as a miniaturized method for extraction of aflatoxins from pistachio and wheat and LC post-column derivatization-fluorescence detection. Chromatographia 73:9–10Google Scholar
Holcmb M, Thompson HC, Cooper WM, Hooper ML (1996) SFE extraction of aflatoxins (B1, B2, G1 and G2) from corn and analysis by HPLC. J Supercrit Fluids 9:118–121CrossRefGoogle Scholar
IARC (2012) IARC Monograph on the evalution of carcinogenic risk to humans. IARC, Lyon 182 (2002) 171–300.Google Scholar
Kabak B (2012) Determination of aflatoxins and ochratoxin A in retail cereal products from Turkey by high performance liquid chromatography with fluorescence detection. Food Control 28:1–6CrossRefGoogle Scholar
Kim HJ, Lee MJ, Kim HJ, Cho SK, Park HJ, Jeong MH (2017) Analytical method development and monitoring of Aflatoxin B1, B2, G1, G2 and Ochratoxin A in animal feed using HPLC with Fluorescence detector and photochemical reaction device. Cogent Food Agric 3(1-8):1419788Google Scholar
Krusong W, Pothimon R, Vichitraka A (2019) Inhibitory impact of vapor-phase ethanol on conidia germination and mycelial growth of Aspergillus fumigatus on bread. Food Control 95:165–169CrossRefGoogle Scholar
Mahpishanian S, Sereshti H (2016) Three-dimensional graphene aerogel-supported iron oxide nanoparticles as an efficient adsorbent for magnetic solid phase extraction of organophosphorus pesticide residues in fruit juices followed by gas chromatographic determination. J Chromatogr A 1443:43–53CrossRefGoogle Scholar
Nouri N, Sereshti H, Farahani A (2018) Graphene-coated magnetic-sheet solid-phase extraction follow by HPLC with fluorescence for the determination of aflatoxins B1, B2, G1, G2 in soy-based samples. J Sep Sci 41:3258–3266CrossRefGoogle Scholar
Peña R, Alcaraz MC, Arce L, Rı́os A, Valcárcel M (2002) Screening of aflatoxins in feed samples using a flow system coupled to capillary electrophoresis. J Chromatogr A 967:303–314CrossRefGoogle Scholar
Rezaee M, Assadi Y, Hosseini MRM, Aghaee E, Ahmadi F, Berijani S (2006) Determination of organic compounds in water using dispersive liquid-liquid microextraction. J Chromatogr A 1116:1–9CrossRefGoogle Scholar
Saalia FK, Phillips RD (2010) Degradation of aflatoxins in aqueous buffer in the presence of nucleophiles. Food Control 21:1066–1069CrossRefGoogle Scholar
Sadeghi A, Ebrahimi M, Mortazavi SA, Abedfar A (2019) Application of the selected antifungal LAB isolate as a protective starter culture in pan whole-wheat sourdough bread. Food Control 95:298–307CrossRefGoogle Scholar
Safarikova M, Safarik I (1999) Magnetic solid-phase extraction. J Magn Magn Mater 194:108–112CrossRefGoogle Scholar
Saladino F, Luz C, Manyes L, Fernández-Franzón M, Meca G (2016) In vitro antifungal activity of lactic acid bacteria against mycotoxigenic fungi and their application in loaf bread shelf life improvement. Food Control 67:273–277CrossRefGoogle Scholar
Serrano AB, Font G, Mañes J, Ferrer E (2016) Dispersive liquid-liquid microextraction for the determination of emerging fusarium mycotoxins in water. Food Anal Methods 9:856–862CrossRefGoogle Scholar
Sheibani A, Tabrizchi M, Ghaziaskar HS (2008) Determination of aflatoxins B1 and B2 using ion mobility spectrometry. Talanta 75:233–238Google Scholar
Simão V, Merib J, Dias AN, Carasek E (2016) Novel analytical procedure using a combination of hollow fiber supported liquid membrane and dispersive liquid–liquid microextraction for the determination of aflatoxins in soybean juice by high performance liquid chromatography – fluorescence detector. Food Chem 196:292–300CrossRefGoogle Scholar
Vasconcelos I, Fernandes C (2017) Magnetic solid phase extraction for determination of drugs in biological matrices. TrAC Trends Anal Chem 89:41–52CrossRefGoogle Scholar
Vosough M, Bayat M, Salemi A (2010) Matrix-free analysis of aflatoxins in pistachio nuts using parallel factor modeling of liquid chromatography diode-array detection data validation study. Anal Chim Acta 663:11–18CrossRefGoogle Scholar
Wilcox J, Donnelly C, Leeman D, Marley E (2015) The use of immunoaffinity columns and connected in tandem for selective cost-effective mycotoxin clean-up liquid prior to multi-mycotoxin chromatographic–tandem mass matrices spectrometric analysis in food. J Chromatogr A 1400:91–97CrossRefGoogle Scholar
Yang X, An R (2011) Application engineer of liquid chromatography life science and chemical analysis group. Agilent Technologies shanghai, China www.agilent.com/chem. Accessed 6 July 2019
Yogendrarajah P, Pouckeb CV, De Meulenaera B, De Saeger S (2013) Development and validation of a QuEChERS based liquid chromatography tandem mass spectrometry method for the determination of multiple mycotoxins in spices. J Chromatogr A 1297:1–11CrossRefGoogle Scholar
Yu L, Li P, Zhang Q, Zhang W, Ding X, Wang X (2013) Graphene oxide: an adsorbent for the extraction and quantification of aflatoxins in peanuts by high-performance liquid chromatography. J Chromatogr A 1318:27–34CrossRefGoogle Scholar
Zhao J, Zhu Y, Jiao Y, Ning J, Yang Y (2016) Ionic-liquid-based dispersive liquid–liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1, B2, G1, and G2 in animal feeds by high-performance liquid chromatography with fluorescence detection. J Sep Sci 39:3789–3797CrossRefGoogle Scholar
Zhou N, Liu P, Su XC, Liao YH, Lei NS, Liang YH, Zhou SH, Lin WS, Chen J, Feng YQ, Tang Y (2017) Low-cost humic acid-bonded silica as an effective solid-phase extraction sorbent for convenient determination of aflatoxins in edible oils. Anal Chim Acta 970:38–46CrossRefGoogle Scholar