Jestoi Marika, Ritieni Alberto, Rizzo Aldo
National Veterinary and Food Research Institute (EELA), Department of Chemistry, P.O. Box 45 (Hämeentie 57), FIN-00581 Helsinki, Finland.
J Agric Food Chem. 2004 Mar 24;52(6):1464-9. doi: 10.1021/jf035130g.
A method is described using gas chromatography-mass spectrometry (GC-MS) for the simultaneous detection of the Fusarium mycotoxins fusaproliferin and seven trichothecenes from grains. Sample purification of the raw extract was carried out with commercial solid phase extraction columns, and the recovery of the more polar analytes was increased by rinsing the column with acetonitrile. A significant matrix effect was found for the analysis of fusaproliferin and trichothecenes; thus, the calibrants should be prepared in a blank matrix. The response was linear in the range used. The mean recovery for fusaproliferin was 60.4 or 62.9%, depending on the spiking level. With respect to the trichothecenes, the recovery was generally higher (70.2-125.3%). The method proved to be repeatable for the analysis of fusaproliferin and trichothecenes. The limit of detection for fusaproliferin in the blank matrix mixture was 50 microg/kg, and that for trichothecenes was 5-15 microg/kg. Thirty-eight Finnish grain samples were analyzed for fusaproliferin and trichothecenes with the method developed. Fusaproliferin was not detected in any of the samples. The mean levels of deoxynivalenol, 3-acetyldeoxynivalenol, nivalenol, HT-2 toxin, and T-2 toxin in Finnish grain samples were 272, 17, 150, 40, and <20 microg/kg, respectively.
本文描述了一种使用气相色谱 - 质谱联用仪（GC-MS）同时检测谷物中镰刀菌霉菌毒素镰刀菌增殖素和七种单端孢霉烯族毒素的方法。粗提物的样品净化采用市售固相萃取柱进行，通过用乙腈冲洗柱子提高了极性更强的分析物的回收率。在分析镰刀菌增殖素和单端孢霉烯族毒素时发现了显著的基质效应；因此，校准物应在空白基质中制备。在所使用的范围内响应呈线性。镰刀菌增殖素的平均回收率根据加标水平为60.4%或62.9%。对于单端孢霉烯族毒素，回收率通常更高（70.2 - 125.3%）。该方法被证明对镰刀菌增殖素和单端孢霉烯族毒素的分析具有可重复性。空白基质混合物中镰刀菌增殖素的检测限为50微克/千克，单端孢霉烯族毒素的检测限为5 - 15微克/千克。使用所开发的方法对38个芬兰谷物样品进行了镰刀菌增殖素和单端孢霉烯族毒素的分析。在任何样品中均未检测到镰刀菌增殖素。芬兰谷物样品中脱氧雪腐镰刀菌烯醇、3 - 乙酰脱氧雪腐镰刀菌烯醇、雪腐镰刀菌烯醇、HT - 2毒素和T - 2毒素的平均含量分别为272、17、150、40和<20微克/千克。
