Multi-mycotoxin stable isotope dilution LC-MS/MS method for Fusarium toxins in cereals
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- 作者：Katharina Habler ; Michael Rychlik
- 关键词：Trichothecenes ; Enniatins ; Stable isotope dilution assay ; LC ; MS/MS ; Solid ; phase extraction ; Barley
- 刊名：Analytical and Bioanalytical Chemistry
- 出版年：2016
- 出版时间：January 2016
- 年：2016
- 卷：408
- 期：1
- 页码：307-317
- 全文大小：768 KB
- 参考文献：1.Rodricks JV, Hesseltine CW, Mehlman MA (1977) Mycotoxins in human and animal health. Proceedings of a conference on mycotoxins in human and animal health, convened at University of Maryland University College, Center of Adult Education, October 4-8, 1976. Pathotox, Park Forest South, Ill
2.Desjardins AE (2006) Fusarium mycotoxins. Chemistry, genetics and biology. APS Press, St. Paul
3.Rychlik M, Humpf H, Marko D, Dänicke S, Mally A, Berthiller F, Klaffke H, Lorenz N (2014) Proposal of a comprehensive definition of modified and other forms of mycotoxins including “masked” mycotoxins. Mycotoxin Res 30(4):197–205CrossRef
4.Sulyok M, Berthiller F, Krska R, Schuhmacher R (2006) Development and validation of a liquid chromatography/tandem mass spectrometric method for the determination of 39 mycotoxins in wheat and maize. Rapid Commun Mass Spectrom 20(18):2649–2659CrossRef
5.Berthiller F, Schuhmacher R, Buttinger G, 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 Chromatogr A 1062(2):209–216CrossRef
6.Berthiller F, Sulyok M, Krska R, Schuhmacher R (2007) Chromatographic methods for the simultaneous determination of mycotoxins and their conjugates in cereals. Int J Food Microbiol 119(1–2):33–37CrossRef
7.Klötzel M, Gutsche B, Lauber U, Humpf H (2005) Determination of 12 type A and B trichothecenes in cereals by liquid chromatography-electrospray ionization tandem mass spectrometry. J Agric Food Chem 53(23):8904–8910CrossRef
8.Klötzel M, Lauber U, Humpf H (2006) A new solid phase extraction clean-up method for the determination of 12 type A and B trichothecenes in cereals and cereal-based food by LC-MS/MS. Mol Nutr Food Res 50(3):261–269CrossRef
9.Asam S, Rychlik M (2006) Synthesis of four carbon-13-labeled type a trichothecene mycotoxins and their application as internal standards in stable isotope dilution assays. J Agric Food Chem 54(18):6535–6546CrossRef
10.Asam S, Rychlik M (2007) Quantitation of type B-trichothecene mycotoxins in foods and feeds by a multiple stable isotope dilution assay. Eur Food Res Technol 224(6):769–783CrossRef
11.Hu L, Rychlik M (2012) Biosynthesis of 15 N 3-labeled enniatins and beauvericin and their application to stable isotope dilution assays. J Agric Food Chem 60(29):7129–7136CrossRef
12.Vogelgesang J, Hädrich J (1998) Limits of detection, identification and determination: a statistical approach for practitioners. Accred Qual Assur 3:242–255CrossRef
13.Sørensen JL, Nielsen KF, Rasmussen PH, Thrane U (2008) Development of a LC-MS/MS method for the analysis of enniatins and beauvericin in whole fresh and ensiled maize. J Agric Food Chem 56(21):10439–10443CrossRef
14.Berger U, Oehme M, Kuhn F (1999) Quantitative determination and structure elucidation of type A- and B-trichothecenes by HPLC/ion trap multiple mass spectrometry. J Agric Food Chem 47(10):4240–4245CrossRef
15.Asam S, Rychlik M (2007) Studies on accuracy of trichothecene multitoxin analysis using stable isotope dilution assays. Mycotoxin Res 23(4):191–198CrossRef
16.Wilcox J, Donnelly C, Leeman D, Marley E (2015) The use of immunoaffinity columns connected in tandem for selective and cost-effective mycotoxin clean-up prior to multi-mycotoxin liquid chromatographic-tandem mass spectrometric analysis in food matrices. J Chromatogr A 1400:91–97CrossRef
17.Nathanail AV, Syvähuoko J, Malachová A, Jestoi M, Varga E, Michlmayr H, Adam G, Sieviläinen E, Berthiller F, Peltonen K (2015) Simultaneous determination of major type A and B trichothecenes, zearalenone and certain modified metabolites in Finnish cereal grains with a novel liquid chromatography-tandem mass spectrometric method. Anal Bioanal Chem 407(16):4745–4755CrossRef
18.Njumbe Ediage E, van Poucke C, de Saeger S (2015) A multi-analyte LC-MS/MS method for the analysis of 23 mycotoxins in different sorghum varieties: the forgotten sample matrix. Food Chem 177:397–404CrossRef
19.Mahnine N, Meca G, Elabidi A, Fekhaoui M, Saoiabi A, Font G, Mañes J, Zinedine A (2011) Further data on the levels of emerging Fusarium mycotoxins enniatins (A, A1, B, B1), beauvericin and fusaproliferin in breakfast and infant cereals from Morocco. Food Chem 124(2):481–485CrossRef
20.Tolosa J, Font G, Mañes J, Ferrer E (2014) Natural occurrence of emerging Fusarium mycotoxins in feed and fish from aquaculture. J Agric Food Chem 62(51):12462–12470CrossRef
21.Biselli S, 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 Addit Contam 22(8):752–760CrossRef
22.Hu L, Gastl M, Linkmeyer A, Hess M, Rychlik M Fate of enniatins and beauvericin during the brewing process determined by stable isotope dilution assays. Accepted Manuscript
23.Uhlig S, Torp M, Heier BT (2006) Beauvericin and enniatins A, A1, B and B1 in Norwegian grain: a survey. Food Chem 94(2):193–201CrossRef
24.Vaclavikova M, Malachova A, Veprikova Z, Dzuman Z, Zachariasova M, Hajslova J (2013) ‘Emerging’ mycotoxins in cereals processing chains: changes of enniatins during beer and bread making. Food Chem 136(2):750–757CrossRef
25.Meca G, Zinedine A, Blesa J, Font G, Mañes J (2010) Further data on the presence of Fusarium emerging mycotoxins enniatins, fusaproliferin and beauvericin in cereals available on the Spanish markets. Food Chem Toxicol 48(5):1412–1416CrossRef
26.Maul R, Müller C, Rieß S, Koch M, Methner F, Nehls I (2012) Germination induces the glucosylation of the Fusarium mycotoxin deoxynivalenol in various grains. Food Chem 131(1):274–279CrossRef
27.Berthiller F, Dall’Asta C, Schuhmacher R, Lemmens M, Adam G, Krska R (2005) Masked mycotoxins: determination of a deoxynivalenol glucoside in artificially and naturally contaminated wheat by liquid chromatography–tandem mass spectrometry. J Agric Food Chem 53(9):3421–3425CrossRef
28.Kostelanska M, Zachariasova M, Lacina O, Fenclova M, Kollos A, Hajslova J (2011) The study of deoxynivalenol and its masked metabolites fate during the brewing process realised by UPLC–TOFMS method. Food Chem 126(4):1870–1876CrossRef
29.Kostelanska M, Hajslova J, Zachariasova M, Malachova A, Kalachova K, Poustka J, Fiala J, Scott PM, Berthiller F, Krska R (2009) Occurrence of deoxynivalenol and its major conjugate, deoxynivalenol-3-glucoside, in beer and some brewing intermediates. J Agric Food Chem 57(8):3187–3194CrossRef
30.Die Kommission der Europäischen Gemeinschaften (2006) Verordnung (EG) Nr. 1881/2006 zur Festsetzung der Höchstgehalte für bestimmte Kontaminanten in Lebensmitteln - 作者单位：Katharina Habler (1)
Michael Rychlik (1)
1. Chair of Analytical Food Chemistry, Technische Universität München, Alte Akademie 10, 85354, Freising, Germany - 刊物类别：Chemistry and Materials Science
- 刊物主题：Chemistry
Analytical Chemistry
Food Science
Inorganic Chemistry
Physical Chemistry
Monitoring, Environmental Analysis and Environmental Ecotoxicology - 出版者：Springer Berlin / Heidelberg
- ISSN：1618-2650
文摘
A multi-mycotoxin stable isotope dilution LC-MS/MS method was developed for 14 Fusarium toxins including modified mycotoxins in cereals (deoxynivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, HT2-toxin, T2-toxin, enniatin B, enniatin B1, enniatin A1, enniatin A, beauvericin, fusarenone X, nivalenol, deoxynivalenol-3-glucoside, and zearalenone). The chromatographic separation of the toxins with particular focus on deoxynivalenol and deoxynivalenol-3-glucoside was achieved using a C18-hydrosphere column. An expedient sample preparation method was developed that uses solid-phase extraction for the purification of trichothecenes combined with zearalenone, enniatins, and beauvericin and provides excellent validation data. Linearity, intra-day precision, inter-day precision, and recoveries were ≥0.9982, 1–6 %, 5–12 %, and 79–117 %, respectively. Method accuracy was verified by analyzing certified reference materials for deoxynivalenol, HT2-toxin, and T2-toxin with deviations below 7 %. The results of this method found barley malt samples from 2012, 2013, and 2014 frequently contaminated with high concentrations of enniatin B, deoxynivalenol, and its modified mycotoxin deoxynivalenol-3-glucoside. Samples from 2012 were especially contaminated. Fusarenone X was not detected in any of the analyzed samples.