Multi-mycotoxin analysis in Indonesian commercial corn oil using high-resolutionl chromatography-mass spectrometry (UHPLC-HRMS)
DOI:
https://doi.org/10.3989/gya.0757241.2208Keywords:
acetonitrile, isotope dilution, matrix effects, oil matrix, Q-Orbitrap, UHPLC QE-MSAbstract
Detecting mycotoxins in corn oil poses significant technical challenges due to its complex matrix, which can disrupt both extraction and analysis processes. This research aimed to establish a robust method for accurately and efficiently detecting mycotoxins in corn oil. Commercial corn oil sourced from Indonesia was used, employing sample pretreatment through complementary liquidliquid extraction. UHPLC-HRMS was utilized to identify multiple mycotoxins. The research showed that complementary liquid-liquid extraction greatly improved mycotoxin recovery (95 - 106%). Method validation included assessing parameters such as linearity (R2 > 0.99), recovery (RSD < 11.7%), intra-day and inter-day precision (RSD < 16%), LOD < 0.03 ppb, and LOQ < 0.40 ppb. Method precision was confirmed by comparing results to LC-ID-MS/MS and certified reference materials (CRM). Analysis of commercial corn samples from Indonesia revealed elevated levels of mycotoxins in both animal feed and corn intended for human consumption, with fumonisin B1 (FB1) levels reaching up to 3214 ppb.
Downloads
References
Abdolmaleki K, Khedri S, Alizadeh L, Javanmardi F, Oliveira CAF, & Khaneghah AM. 2021. The mycotoxins in edible oils: An overview of prevalence, concentration, toxicity, detection and decontamination techniques. Trends Food Sci. Technol. 115, 500-511. https://doi.org/10.1016/j.tifs.2021.06.057
Adegbeye MJ, Reddy PRK, Chilaka CA, Balogun OB, Elghandour MMMY, Rivas-Caceres RR, & Salem AZM. 2020. Mycotoxin toxicity and residue in animal products: Prevalence, consumer exposure and reduction strategies-A review. Toxicon 177, 96-108. https://doi.org/10.1016/j.toxicon.2020.01.007 PMid:31972175
Annunziata L, Schirone M, Visciano P, Campana G, De Massis MR, Migliorati G. 2021. Determination of aflatoxins, deoxynivalenol, ochratoxin A and zearalenone in organic wheat flour under different storage conditions. Int. J. Food Sci. Technol. 56 (8), 4139-4148. https://doi.org/10.1111/ijfs.15042
Arumsari, A. G., Lenin, A., Suparmi, A., Arifin, M. J., & Haryani, R. (2022). Effectiveness Of Collaborative Strategy To Reduce Aflatoxin Contamination In Corn. Bulletin of The Transilvania University of Brasov, 15 (2), 123-138. https://doi.org/10.31926/but.fwiafe.2022.15.64.2.9
Awuchi CG, Ondari EN, Ogbonna CU, Upadhyay AK, Baran K, Okpala COR, Guiné RPF. 2021. Mycotoxins affecting animals, foods, humans, and plants: Types, occurrence, toxicities, action mechanisms, prevention, and detoxification strategies-A revisit. Foods 10 (6), 1279. https://doi.org/10.3390/foods10061279 PMid:34205122 PMCid:PMC8228748
Cavaliere C, Foglia P, Pastorini E, Samperi R, Laganà A. 2005. Development of a multiresidue method for analysis of major Fusarium mycotoxins in corn meal using liquid chromatography/tandem mass spectrometry. Rapid Communications in Mass Spectr. 19 (14), 2085-2093. https://doi.org/10.1002/rcm.2030 PMid:15988722
Cheli F, Battaglia D, Gallo R, Dell'Orto V. 2014. EU legislation on cereal safety: An update with a focus on mycotoxins. Food Control. 37, 315-325. https://doi.org/10.1016/j.foodcont.2013.09.059
Chen S, Zhang X, Yan Z, Hu Y, Lu Y. 2019. Development and application of immunoaffinity column purification and ultrahigh performance liquid chromatography-tandem mass spectrometry for determination of domoic acid in shellfish. Toxins 11 (2), 83. https://doi.org/10.3390/toxins11020083 PMid:30717167 PMCid:PMC6409838
Decheng S, Zhiming X, Shulin W, Shi W, Peilong W. 2021. Trace analysis of progesterone and 21 progestins in milk by ultra-performance liquid chromatography coupled with high-field quadrupole-orbitrap highresolution mass spectrometry. Food Chem. 361, 130115. https://doi.org/10.1016/j.foodchem.2021.130115 PMid:34049049
Desmarchelier A, Tessiot S, Bessaire T, Racault L, Fiorese E, Urbani A, Mottier P. 2014. 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. J. Chromatog. A 1337, 75-84. https://doi.org/10.1016/j.chroma.2014.02.025 PMid:24636559
Gab-Allah MA, Choi K, Kim B. 2021. Development of isotope dilution-liquid chromatography/tandem mass spectrometry for the accurate determination of type-A trichothecenes in grains. Food Chem. 344, 128698. https://doi.org/10.1016/j.foodchem.2020.128698 PMid:33272759
Hidalgo-Ruiz JL, Romero-González R, Martínez Vidal JL, Garrido Frenich A. 2019. A rapid method for the determination of mycotoxins in edible vegetable oils by ultra-high performance liquid chromatographytandem mass spectrometry. Food Chem. 288, 22-28. https://doi.org/10.1016/j.foodchem.2019.03.003 PMid:30902285
Imran M, Cao S, Wan SF, Chen Z, Saleemi MK, Wang N, Munawar J. 2020. Mycotoxins-a global one health concern: A review. Agrobiol. Records 2, 1-16. https://doi.org/10.47278/journal.abr/2020.006
Iqbal SZ. 2021. Mycotoxins in food, recent development in food analysis and future challenges; a review. Current Opinion Food Sci. 42, 237-247. https://doi.org/10.1016/j.cofs.2021.07.003
Jabran M, Chen D, Muhae-Ud-Din G, Liu T, Chen W, Liu C, Gao L. 2022. Metabolomic Analysis of Wheat Grains after Tilletia laevis Kühn Infection by Using Ultrahigh-Performance Liquid Chromatography-QExactive Mass Spectrometry. Metabolites 12 (9), 805. https://doi.org/10.3390/metabo12090805 PMid:36144210 PMCid:PMC9502932
Jedziniak P, Panasiuk Ł, Pietruszka K, Posyniak A. 2019. Multiple mycotoxins analysis in animal feed with LC-MS/MS: Comparison of extract dilution and immunoaffinity clean-up. J. Sep. Sci. 42 (6), 1240-1247. https://doi.org/10.1002/jssc.201801113 PMid:30638302
Kusmardini D, Anggraeni S, Lisdiani V, Murni AP, Selvina F, Anggira KA. 2025. Multiple Mycotoxin Analysis In Areca Seed Oil Using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry (Uplc-Ms/Ms). Carpathian J. Food Sci. Technol. 17 (1).
Mao S, Sun B, Yu T, Mao W, Zhu S, Ni Y. 2019. pH-Modulated memristive behavior based on an edible garlic-constructed bio-electronic device. New J. Chem. 43 (24), 9634-9640. https://doi.org/10.1039/C9NJ02433F
Negi K, Asthana A K, Chaturvedi P. 2020. GC-MS analysis and antifungal activity of acetone extract of Conocephalum conicum (L) Underw (Liverwort) against aflatoxins producing fungi. South African J. Botany 131, 384-390. https://doi.org/10.1016/j.sajb.2020.02.035
Nugraha A, Khotimah K, & Rietjens IMCM. 2018 Risk assessment of aflatoxin B1 exposure from maize and peanut consumption in Indonesia using the margin of exposure and liver cancer risk estimation approaches. Food Chem. Toxicol. 113, 134-144. https://doi.org/10.1016/j.fct.2018.01.036 PMid:29374592
Nuryono, Noviandi CT, Böhm J, Agus A, Wedhastri S, Maryudani YB, Razzazi E. 2002. A survey of fumonisins (B1, B2, B3) in indonesian corn-based food and feed samples. Mycotoxin Research 18 (2 Suppl.), 117-120. https://doi.org/10.1007/BF02946077 PMid:23606144
Putz M, Piper T, Dubois M, Delahaut P, Thevis M. 2019. Analysis of endogenous steroids in urine by means of multi-immunoaffinity chromatography and isotope ratio mass spectrometry for sports drug testing. Anal. Bioanal. Chem. 411, 7563-7571. https://doi.org/10.1007/s00216-019-02169-3 PMid:31641821
Qian M, Zhang H, Wu L, Jin N, Wang J, Jiang K. 2015. Simultaneous determination of zearalenone and its derivatives in edible vegetable oil by gel permeation chromatography and gas chromatography-triple quadrupole mass spectrometry. Food Chem. 166, 23-28. https://doi.org/10.1016/j.foodchem.2014.05.133 PMid:25053023
Sharmili K, Jinap S, Sukor R. 2016. Development, optimization and validation of QuEChERS based liquid chromatography tandem mass spectrometry method for determination of multimycotoxin in vegetable oil. Food Control 70, 152-160. https://doi.org/10.1016/j.foodcont.2016.04.035
Slobodchikova I, Vuckovic D. 2018. Liquid chromatography - high resolution mass spectrometry method for monitoring of 17 mycotoxins in human plasma for exposure studies. J. Chromatog. A 1548, 51-63. https://doi.org/10.1016/j.chroma.2018.03.030 PMid:29576275
Somantri ASM. 2016. Sistem Keamanan Pangan Berbahan Baku Jagung. Buletin Teknol. Pasca Panen, 8 (2), 112-119.
Van Pamel E, Verbeken A, Vlaemynck, G, De Boever J, Daeseleire E. 2011. Ultrahigh-Performance Liquid Chromatographic-Tandem Mass Spectrometric Multimycotoxin Method for Quantitating 26 Mycotoxins in Maize Silage. J. Agric. Food Chem. 59 (18), 9747-9755. https://doi.org/10.1021/jf202614h PMid:21888373
Wang Y, Dong Y, Li Z, Deng L, Guo C, Zhang S, Zhao S. 2016. Fast determination of multi-mycotoxins in corn by dispersive solid-phase extraction coupled with ultra-performance liquid chromatography with tandem quadrupole time-of-flight mass spectrometry. J. Integrat. Agric. 15(7), 1656-1666. https://doi.org/10.1016/S2095-3119(15)61287-4
Xu H, Sun J, Wang H, Zhang Y, Sun, X. 2021. Adsorption of aflatoxins and ochratoxins in edible vegetable oils with dopamine-coated magnetic multi-walled carbon nanotubes. Food Chem. 365, 130409. https://doi.org/10.1016/j.foodchem.2021.130409 PMid:34256225
Yao K, Wen K, Shan W, Xie S, Peng T, Wang, Shao B. 2018. Development of an immunoaffinity column for the highly sensitive analysis of bisphenol A in 14 kinds of foodstuffs using ultra-high-performance liquid chromatography tandem mass spectrometry. J. Chromatog. B. 1080, 50-58. https://doi.org/10.1016/j.jchromb.2018.02.013 PMid:29477067
Yu X, Li Z, Zhao M, Lau SCS, Ru Tan H, Teh WJ, Zhang Y. 2019. Quantification of aflatoxin B1 in vegetable oils using low temperature clean-up followed by immuno-magnetic solid phase extraction. Food Chem. 275, 390-396. https://doi.org/10.1016/j.foodchem.2018.09.132 PMid:30724212
Zhang K, Schaab MR, Southwood G, Tor ER, Aston LS, Song, W, Begley TH. 2017. A Collaborative Study: Determination of Mycotoxins in Corn, Peanut Butter, and Wheat Flour Using Stable Isotope Dilution Assay (SIDA) and Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS). J. Agric. Food Chem. 65 (33), 7138-7152. https://doi.org/10.1021/acs.jafc.6b04872 PMid:27983809
Zhou C, Xu Z, Shi H, Zhang G, Cao W, Xu X. 2022. Simple and Rapid Method for the Quantitation of Trace-Level 3-Alkyl-2-methoxypyrazines in Fragrant Vegetable Oils by Gas Chromatography-Tandem Mass Spectrometry. J. Agric. Food Chem.70 (20), 6247-6252. https://doi.org/10.1021/acs.jafc.1c07380 PMid:35536735
Downloads
Published
How to Cite
Issue
Section
License
Copyright (c) 2025 Consejo Superior de Investigaciones Científicas (CSIC)
This work is licensed under a Creative Commons Attribution 4.0 International License.
© CSIC. Manuscripts published in both the print and online versions of this journal are the property of the Consejo Superior de Investigaciones Científicas, and quoting this source is a requirement for any partial or full reproduction.
All contents of this electronic edition, except where otherwise noted, are distributed under a Creative Commons Attribution 4.0 International (CC BY 4.0) licence. You may read the basic information and the legal text of the licence. The indication of the CC BY 4.0 licence must be expressly stated in this way when necessary.
Self-archiving in repositories, personal webpages or similar, of any version other than the final version of the work produced by the publisher, is not allowed.
