Development and validation of a method based on a QuEChERS procedure and heart-cutting GC-MS for determination of five mycotoxins in cereal products

被引:121
作者
Cunha, Sara C. [1 ]
Fernandes, Jose O. [1 ]
机构
[1] Univ Porto, Dept Bromatol, Fac Pharm, REQUIMTE, P-4099030 Oporto, Portugal
关键词
Deans Switch; Deoxynivalenol (DON); Heart-cutting GC-MS; QuEChERS; Trichothecenes; Zearelenone (ZON); CHROMATOGRAPHY-MASS SPECTROMETRY; GAS-CHROMATOGRAPHY; BREAKFAST CEREALS; TRICHOTHECENES; DEOXYNIVALENOL; ZEARALENONE; IDENTIFICATION; TOXINS; WHEAT;
D O I
10.1002/jssc.200900695
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A new analytical method for the rapid and simultaneous determination of five mycotoxins (zearelenone, deoxynivalenol, Fusarenon X, 15-acetyldeoxynivalenol and nivalenol) in breakfast cereals and flours by heart-cutting GC-MS has been developed and validated. Extraction was performed with MeCN, applying a modified QuEChERS (QUick, Easy, CHeap, Effective, Rugged and Safe) procedure, and the extracts were analyzed after a silylation of the analytes under study. Careful optimization of the parameters of Deans Switch device and GC-MS was achieved in order to attain a fast separation in SIM mode, allowing a total run time of only 8 min. Acceptable recoveries for all mycotoxins at two different spiking levels (20 and 100 mu g/kg) were achieved with good repeatability (from 9 to 21%). LOD ranged from 2 to 15 mu g/kg and LOQ ranged from 5 to 50 mu g/kg. which were lower than the maximum limit legal established by the European Union (EU). The method developed was applied to commercial breakfast cereals and flours; among the mycotoxins studied, deoxynivalenol and zearalenone were the most predominant.
引用
收藏
页码:600 / 609
页数:10
相关论文
共 33 条
[1]  
Anastassiades M, 2003, J AOAC INT, V86, P412
[2]   Multidimensional gas chromatography using a double cool-strand interface [J].
Begnaud, F ;
Chaintreau, A .
JOURNAL OF CHROMATOGRAPHY A, 2005, 1071 (1-2) :13-20
[3]   Mycotoxins [J].
Bennett, JW ;
Klich, M .
CLINICAL MICROBIOLOGY REVIEWS, 2003, 16 (03) :497-+
[4]   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 [J].
Biselli, S ;
Hummert, C .
FOOD ADDITIVES AND CONTAMINANTS PART A-CHEMISTRY ANALYSIS CONTROL EXPOSURE & RISK ASSESSMENT, 2005, 22 (08) :752-760
[5]   Fast analysis of multiple pesticide residues in apple juice using dispersive liquid-liquid microextraction and multidimensional gas chromatography-mass spectrometry [J].
Cunha, S. C. ;
Fernandes, J. O. ;
Oliveira, M. B. P. P. .
JOURNAL OF CHROMATOGRAPHY A, 2009, 1216 (51) :8835-8844
[6]   Fast low-pressure gas chromatography-mass spectrometry method for the determination of multiple pesticides in grapes, musts and wines [J].
Cunha, S. C. ;
Fernandes, J. O. ;
Alves, A. ;
Oliveira, M. B. P. P. .
JOURNAL OF CHROMATOGRAPHY A, 2009, 1216 (01) :119-126
[7]  
CUNHA SC, OLIVES OLIVE OIL HLT, pCH70
[8]  
Deans D.R., 1968, CHROMATOGRAPHIA, V1, P18, DOI [DOI 10.1007/BF02259005, 10.1007/BF02259005]
[9]  
FAO, 2003, Worldwide Regulations for Mycotoxins in Food and Feed in 2003
[10]   Simple and high-throughput method for the multimycotoxin analysis in cereals and related foods by ultra-high performance liquid chromatography/tandem mass spectrometry [J].
Garrido Frenich, Antonia ;
Martinez Vidal, Jose Luis ;
Romero-Gonzalez, Roberto ;
del Mar Aguilera-Luiz, Maria .
FOOD CHEMISTRY, 2009, 117 (04) :705-712