Bìa tạp chí



First step in development and evaluation simultaneous determination of mycotoxins in cereals by liquid chromatography - mass spectrometry

Nguyen Huu Vinh Nguyen Hong Thao Nguyen Cong Tuan Tran Vuong Duc Nghia Ho Tran Ngoc Quyen Nguyen Huu Tin Nguyen Thanh Cong Ngo Quoc Viet
Published 09/12/2022

Article Details

How to Cite
Nguyen Huu Vinh, Nguyen Hong Thao, Nguyen Cong Tuan, Tran Vuong Duc Nghia, Ho Tran Ngoc Quyen, Nguyen Huu Tin, Nguyen Thanh Cong, Ngo Quoc Viet. "First step in development and evaluation simultaneous determination of mycotoxins in cereals by liquid chromatography - mass spectrometry". Vietnam Journal of Food Control. vol. 5, no. 3, pp. 402-413, 2022

Main Article Content


Currently, solid phase extraction (SPE) with immunoaffinity columns is applied in most standardized methods for mycotoxin determination to purify extracts and analysis by HPLC-FLD, HPLC-UV/VIS or LC-MS/MS. Therefore, sample preparation and analysis by instruments are time-consuming and high operating costs. The novel method allow simultaneously identify nine mycotoxin compounds with selective, stable and accurate results. The new method has been evaluated through three stages including validation as requirements of CEN/TR 16059:2010 (phase 1), comparison with current standard methods (phase 2), evaluate the method using an interlaboratory comparison program (phase 3).

Cereal samples were extracted by QuEChERS and analyzed by LC-MS/MS. The limit of quantitation (LOQ) was 0,5 μg/kg for each aflatoxin compound and 40 μg/kg, 25 μg/kg, 1 μg/kg, 75 μg/kg for deoxynivalenol, zearalenone, ochratoxin A, each toxin fumonisin (B1&B2), respectively. The recovery is in the range of 70-120%, relative standard deviation RSD < 20%. The novel method also gives the same results compared to the individual standardized methods, using the immunoaffinity column in the extraction stage. At the present, the method is being evaluated through an interlaboratory comparison program with two rounds: round 1 (for survey) and round 2 (official round), which is expected to be implemented in 2022.


mycotoxin, LC-MS/MS, simultaneous determination.


[1]. An Giang Department of Health, "Ensuring food safety, preventing food poisoning
and food-borne diseases in 2022", Available: https://soyte.angiang.gov.vn/wps/portal/Home /trang-chu/tin-chi-tiet/sa-khoitin/savsattp/syt184, [accessed 15/06/2022].
[2]. M. A. A. Adam, Y. M Tabana, K. B.Musa, and D. A. Sandai, “Effects of different mycotoxins on humans, cell genome and their involvement in cancer,” Oncology Reports, vol. 37, pp. 1321-1336, 2017.
[3]. S. A. Adeyeye, “Fungal mycotoxins in foods: A review,” Cogent Food & Agriculture, vol. 2, no. 1, pp. 121-127, 2016.
[4]. International Agency for Research on Cancer, “IARC monographs on the identification of carcinogenic hazards to humans,” Địa chỉ: https://monographs.iarc.who.int/agents-classified-by-the-iarc/ [Truy cập 30/3/2021].
[5]. Ministry of Health, Decision No. 46/2007/QD-BYT on promulgation “Regulation of maximum level of biological and chemical pollution in food,” 2007.
[6]. Ministry of Health, QCVN 8-1:2011/BYT “National technical regulation on the limits of mycotoxins contaminantion in food,” 2011.
[7]. N. T. H. Binh, N. N. Son, N. Thi Lan, and T. Cao Son, “The occurrence of mycotoxins in food collected from some northern provinces of Vietnam in 2019”, Vietnam Journal of Food Control, vol. 3, no.3, pp. 183-190, 2020.
[8]. J. Sun, W. Li, Y. Zhang, X. Hu, L. Wu, and B. Wang, “QuEChERS purification combined with ultrahigh-performance liquid chromatography tandem mass spectrometry for simultaneous quantification of 25 mycotoxins in cereals,” Toxins, vol. 8, no. 12, pp. 375, 2016.
[9]. V. Lippolis, M. Pascale, S. Valenzano, and A. Visconti, “Comparison of slurry mixing and dry milling in laboratory sample preparation for determination of ochratoxin A and deoxynivalenol in wheat,” Journal of AOAC International, vol. 95, no. 2, pp. 452-458, 2012.
[10]. J. Velasco and S. L. Morris, “Use of water slurries in Aflatoxin analysis,” Journal of Agriculture and Food Chemistry, vol. 24, no.1, 1976.
[11]. P. Yogendrarajah, C. V. Poucke, B. De Meulenaer, and S. De Saeger, “Development and validation of a QuEChERS based liquid chromatography tandem mass spectrometry method for the determination of multiple mycotoxins in spices,” Journal of Chromatography A, vol. 1297, pp. 1-11, 2013.
[12]. European Committee Standardization, “CEN/TR 16059:2010 - Food analysis - Performance criteria for single laboratory validated methods of analysis for the determination of mycotoxins,” 2010.
[13]. European Communities, “2002/657/EC Commission - COMMISSION DECISION of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results,” Official Journal of the European Communities, 2002.
[14]. Tran Cao Son, Method validation in chemical and microbiological analysis. Hanoi: Science and Technics Publishing House, 2010.