نوع مقاله : مقاله پژوهشی

نویسندگان

1 پژ<هشگاه استاندارد-پژوهشکده غذایی کشاورزی کرج

2 استادیار، گروه فراورده های غذایی، حلال و کشاورزی، پژوهشکده صنایع غذایی و فراورده های کشاورزی، پژوهشگاه استاندارد، کرج، ایران

3 مدرس دانشگاه، صنایع غذایی، دانشکده علوم دارویی، دانشگاه علوم پزشکی آزاد اسلامی تهران، تهران، ایران

10.22092/fooder.2024.366594.1399

چکیده

برای تعیین همزمان آفلاتوکسین ها، اکراتوکسین آ، زئارالنون، دئوکسی نیوالنول، سموم T2، HT2 و فومونیسین ها در غلات، یک روش کروماتوگرافی جرمی/ جرمی LC-MS/MS به کار گرفته شد و در آن کارایی دو روش استخراج سموم (یک و دو مرحله‌ای) و چهار روش خالص‌سازی (شامل ستون MycoSep 226، Oasis HLB و ستون ایمیونوافینیتی و بدون خالص‌سازی) برای به دست آوردن حداکثر میزان بازیافت مایکوتوکسین‌ها بررسی گردید. استفاده از حلال استونیتریل: آب: اسیداستیک به نسبت حجمی (1:20:79) به عنوان حلال استخراج، بدون خالص‌سازی عصارۀ حاصل از استخراج، بالاترین میزان بازیابی به میزان 64.3 تا 112.1 درصد را به­ دست داد، در حالی که با استفاده از MycoSep 226 ، Oasis HLB و ستون ایمیونوافینیتی میزان بازیابی به ترتیب 7 99.6، 10- 94.9 و 61.3- 97.6 درصد برای همۀ مایکوتوکسین‌ها بود. تجزیه و تحلیل نمونه‌های غلات (برنج، گندم، جو و ذرت) با استفاده از شرایط انتخاب شده، میزان بازیابی قابل قبول 75.1 تا 106.3 درصد را برای همه مایکوتوکسین‌ها در بین همه نمونه‌ها تأیید کرد. کاربرد این روش روی 30 نمونۀ غلات نمونه برداری شده از بازار نشان داد که روش یاد شده دارای دقت کافی برای استفاده به عنوان روش معمول تجزیه و تحلیل برای سطوح کمی از مایکوتوکسین ها خواهد بود.
 

کلیدواژه‌ها

موضوعات

عنوان مقاله [English]

Multi-Mycotoxin Determination in Cereals Using LC-MS/MS Method

نویسندگان [English]

  • َAnosheh Rahmani 1
  • Maryam Jalili 2
  • Farhang Soleimany 3

1 Department of Food, Halal and Agricultural Products, Food Technology and Agricultural Products Research Center, Standard Research Institute (SRI), Karaj, Iran.

2 2- Assistant Professor, Department of Food, Halal and Agricultural Products, Food Technology and Agricultural Products Research Center, Standard Research Institute (SRI), Karaj, Iran

3 3- University Lecturer, Department of Food technology, Faculty of Pharmaceutical Sciences, Tehran Islamic Azad University of Medical Sciences, Tehran, Iran

چکیده [English]

A chromatography mass/mass method (LC-MS/MS) was used for the simultaneous determination of aflatoxins, ochratoxin A, zearalenone, deoxynivalenol, toxins T2, HT2 and fumonisins in cereals, and the efficiency of two methods of extracting toxins (one and two steps) and four purification methods (including MycoSep 226, Oasis HLB, immunoaffinity column (IAC) and No clean-up method) were investigated to obtain the maximum amount of recovery of myconoxins. The use of acetonitrile solvent: water: acetic acid in a volume ratio (79:20:1) as the extraction solvent, without purification, achieved the highest recovery rate of 64.3 to 112.1%. However, using MycoSep 226, Oasis HLB and IAC, the recovery rate was 7- 99.6, 10- 94.9 and 61.3- 97.6% for all mycotoxins, respectively. Analysis of cereal samples (rice, wheat, barley, and corn) using the selected sample preparation method confirmed acceptable recovery rates of 75.1–106.3% for all mycotoxins among all samples. The application of the method on 30 grain samples taken from market showed that the method has sufficient accuracy to be used as a routine analysis method for small levels of mycotoxins.

کلیدواژه‌ها [English]

  • Mycotoxin
  • Extraction
  • Purification؛ Cereals؛ LC-MS/MS
Berthiller, F., Schuhmacher, R., Buttinger, G., and Krska, R. 2005. Rapid simultaneous determination of major type A- and B-trichothecenes as well as zearalenone in maize by high performance liquid chromatography–tandem mass spectrometry. J. Chromatography A, 1062(2), 209-216. https://doi.org/https://doi.org/10.1016/j.chroma.2004.11.011
Biselli, S., and Hummert, C. 2005. Development of a multicomponent method for Fusarium toxins using LC-MS/MS and its application during a survey for the content of T-2 toxin and deoxynivalenol in various feed and food samples. Food additives and contaminants, 22(8), 752-760.
Cheli, F., Battaglia, D., Gallo, R., and Dell'Orto, V. 2014. EU legislation on cereal safety: An update with a focus on mycotoxins. Food Control, 37, 315-325.
European Commission. 2006. Commission Regulation (EC) No 401/2006 of 23 February 2006 laying down the methods of sampling and analysis for the official control of the levels of mycotoxins in foodstuffs. Off J Eur Union L, 70, 12-34.
De Boevre, M., Di Mavungu, J. D., Maene, P., Audenaert, K., Deforce, D., Haesaert, G., Eeckhout, M., Callebaut, A., Berthiller, F., Van Peteghem, C., and De Saeger, S. 2012. Development and validation of an LC-MS/MS method for the simultaneous determination of deoxynivalenol, zearalenone, T-2-toxin and some masked metabolites in different cereals and cereal-derived food. Food Additives & Contaminants: Part A, 29(5), 819-835. https://doi.org/10.1080/19440049.2012.656707
De Girolamo, A., Solfrizzo, M., Lattanzio, V. M. T., Stroka, J., Alldrick, A., van Egmond, H. P., and Visconti, A. 2013. Critical evaluation of LC-MS-based methods for simultaneous determination of deoxynivalenol, ochratoxin A, zearalenone, aflatoxins, fumonisins and T-2/HT-2 toxins in maize. World Mycotoxin Journal, 6(3), 317-334. https://doi.org/https://doi.org/10.3920/WMJ2012.1538
Diana Di Mavungu, J., Monbaliu, S., Scippo, M.-L., Maghuin-Rogister, G., Schneider, Y.-J., Larondelle, Y., Callebaut, A., Robbens, J., Van Peteghem, C., and De Saeger, S. 2009. LC-MS/MS multi-analyte method for mycotoxin determination in food supplements. Food additives and contaminants, 26(6), 885-895.
Driehuis, F., Spanjer, M. C., Scholten, J. M., and te Giffel, M. C. 2008. Occurrence of Mycotoxins in Feedstuffs of Dairy Cows and Estimation of Total Dietary Intakes. Journal of Dairy Science, 91(11), 4261-4271. https://doi.org/https://doi.org/10.3168/jds.2008-1093
Fernandes, P. J., Barros, N., Santo, J. L., and Câmara, J. S. 2015. High-throughput analytical strategy based on modified QuEChERS extraction and dispersive solid-phase extraction clean-up followed by liquid chromatography-triple-quadrupole tandem mass spectrometry for quantification of multiclass mycotoxins in cereals. Food Analytical Methods, 8, 841-856.
Garon, D., Richard, E., Sage, L., Bouchart, V., Pottier, D., and Lebailly, P. 2006. Mycoflora and multimycotoxin detection in corn silage: experimental study. Journal of Agricultural and Food Chemistry, 54(9), 3479-3484.
Gilbert, J., and Anklam, E. 2002. Validation of analytical methods for determining mycotoxins in foodstuffs. TrAC Trends in Analytical Chemistry, 21(6-7), 468-486.
Köppen, R., Bremser, W., Rasenko, T., and Koch, M. 2013. Development and certification of a reference material for Fusarium mycotoxins in wheat flour. Analytical and Bioanalytical Chemistry, 405, 4755-4763.
Lattanzio, V. M., Pascale, M., and Visconti, A. 2009. Current analytical methods for trichothecene mycotoxins in cereals. TrAC Trends in Analytical Chemistry, 28(6)768-758.
Lattanzio, V. M. T., Solfrizzo, M., Powers, S., and Visconti, A. 2007. Simultaneous determination of aflatoxins, ochratoxin A and Fusarium toxins in maize by liquid chromatography/tandem mass spectrometry after multitoxin immunoaffinity cleanup. Rapid Communications in Mass Spectrometry: An International Journal Devoted to the Rapid Dissemination of Up‐to‐the‐Minute Research in Mass Spectrometry, 21(20), 3253-3261.
Monbaliu, S., Van Poucke, C., Detavernier, C. l., Dumoulin, F., Van De Velde, M., Schoeters, E., Van Dyck, S., Averkieva, O., Van Peteghem, C., and De Saeger, S. 2010. Occurrence of Mycotoxins in Feed as Analyzed by a Multi-Mycotoxin LC-MS/MS Method. Journal of Agricultural and Food Chemistry, 58(1), 66-71. https://doi.org/10.1021/jf903859z
Paepens, C., De Saeger, S., Van Poucke, C., Dumoulin, F., Van Calenbergh, S., and Van Peteghem, C. 2005. Development of a liquid chromatography/tandem mass spectrometry method for the quantification of fumonisin B1, B2 and B3 in cornflakes. Rapid Communications in Mass Spectrometry: An International Journal Devoted to the Rapid Dissemination of Up‐to‐the‐Minute Research in Mass Spectrometry, 19(14), 2021-2029.
Qiao, J., Qi, L., Ma, H., Liu, H., Yang, J., Chen, Y., and Yang, G. 2009. A block copolymer covalent coating acting as surfactants in separation of 2-[hydroxy (4-nitrophenyl) methyl]-cyclopent-2-enone and 4-nitrobenzaldehyde by capillary electrophoresis. Talanta, 80(2), 770-776.
Rahmani, A., Jinap, S., and Soleimany, F. 2009. Qualitative and quantitative analysis of mycotoxins. Comprehensive Reviews in Food Science and Food Safety, 8(3), 202-251.
Ren, Y., Zhang, Y., Shao, S., Cai, Z., Feng, L., Pan, H., and Wang, Z. 2007. Simultaneous determination of multi-component mycotoxin contaminants in foods and feeds by ultra-performance liquid chromatography tandem mass spectrometry. Journal of Chromatography A, 1143(1), 48-64. https://doi.org/https://doi.org/10.1016/j.chroma.2006.12.064
Richard, E., Heutte, N., Sage, L., Pottier, D., Bouchart, V., Lebailly, P., and Garon, D. 2007. Toxigenic fungi and mycotoxins in mature corn silage. Food and Chemical Toxicology, 45(12), 2420-2425.
Sáez, J. M., Medina, Á., Gimeno-Adelantado, J. V., Mateo, R., and Jiménez, M. 2004. Comparison of different sample treatments for the analysis of ochratoxin A in must, wine and beer by liquid chromatography. Journal of Chromatography A, 1029(1-2), 125-133.
Shi, H., Li, S., Bai, Y., Prates, L. L., Lei, Y., and Yu, P. 2018. Mycotoxin contamination of food and feed in China: Occurrence, detection techniques, toxicological effects and advances in mitigation technologies. Food Control, 91, 202-215.
Soleimany, F., Jinap, S., and Abas, F. 2012a. Determination of mycotoxins in cereals by liquid chromatography tandem mass spectrometry. Food Chemistry, 130(4), 1055-1060. https://doi.org/https://doi.org/10.1016/j.foodchem.2011.07.131
Soleimany, F., Jinap, S., Faridah, A., and Khatib, A. 2012b. A UPLC–MS/MS for simultaneous determination of aflatoxins, ochratoxin A, zearalenone, DON, fumonisins, T-2 toxin and HT-2 toxin, in cereals. Food Control, 25(2), 647-653. https://doi.org/https://doi.org/10.1016/j.foodcont.2011.11.012
Spanjer, M. C., Rensen, P. M., and Scholten, J. M. 2008. LC–MS/MS multi-method for mycotoxins after single extraction, with validation data for peanut, pistachio, wheat, maize, cornflakes, raisins and figs. Food Additives & Contaminants: Part A, 25(4), 472-489. https://doi.org/10.1080/02652030701552964
Stecher, G., Jarukamjorn, K., Zaborski, P., Bakry, R., Huck, C. W., and Bonn, G. K. 2007. Evaluation of extraction methods for the simultaneous analysis of simple and macrocyclic trichothecenes. Talanta, 73(2), 251-257.
Sulyok, M., Krska, R., and Schuhmacher, R. 2007. Application of a liquid chromatography–tandem mass spectrometric method to multi-mycotoxin determination in raw cereals and evaluation of matrix effects. Food additives and contaminants, 24(10), 1184-1195.
Sulyok, M., Krska, R., and Schuhmacher, R. 2010. Application of an LC–MS/MS based multi-mycotoxin method for the semi-quantitative determination of mycotoxins occurring in different types of food infected by moulds. Food Chemistry, 119(1), 408-416.
Tanaka, H., Takino, M., Sugita‐Konishi, Y., and Tanaka, T. 2006. Development of a liquid chromatography/time‐of‐flight mass spectrometric method for the simultaneous determination of trichothecenes, zearalenone and aflatoxins in foodstuffs. Rapid Communications in Mass Spectrometry: An International Journal Devoted to the Rapid Dissemination of Up‐to‐the‐Minute Research in Mass Spectrometry, 20(9), 1422-1428.
Tevell Åberg, A., Solyakov, A., and Bondesson, U. 2013. Development and in-house validation of an LC-MS/MS method for the quantification of the mycotoxins deoxynivalenol, zearalenone, T-2 and HT-2 toxin, ochratoxin A and fumonisin B1 and B2 in vegetable animal feed. Food Additives & Contaminants: Part A, 30(3), 541-549. https://doi.org/10.1080/19440049.2012.760208
Vasquez-Martinez, Y., VILLEGAS R, L., Villa, A., and Massiff, G. 2011. Validation of a liquid chromatography-fluorescence spectrometric method for the quantification of four quinolones in pig and chicken muscle following the European Union guideline EC/657/2002. Journal of the Chilean Chemical Society, 56(1), 554-558.
Ventura, M., Guillén, D., Anaya, I., Broto‐Puig, F., Lliberia, J. L., Agut, M., and Comellas, L. 2006. Ultra‐performance liquid chromatography/tandem mass spectrometry for the simultaneous analysis of aflatoxins B1, G1, B2, G2 and ochratoxin A in beer. Rapid Communications in Mass Spectrometry: An International Journal Devoted to the Rapid Dissemination of Up‐to‐the‐Minute Research in Mass Spectrometry, 20(21), 3199-3204.
Wang, H.-Y., Yang, Y.-L., Wang, Y., Zhang, S.-F., and Li, L. 2019. Development of disk-shaped monolithic microplates for detecting multiple mycotoxins. Analytical Methods, 11(48), 6084-6091.