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Determination of type B trichothecenes and macrocyclic lactone mycotoxins in field contaminated maize

机译:田间污染玉米中B型毛虫和大环内酯真菌毒素的测定

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摘要

A sensitive, reliable liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for determining some commonly found mycotoxins produced by Fusarium strains in maize was evaluated and applied to field samples. The selected substances were: trichothecenes B (nivalenol, deoxynivalenol, fusarenon X, 3- and 15-acetyldeoxynivalenol) and some macrocyclic lactones (zearalenone, α- and β-zearalenol, zearalanone, α- and β-zearalanol). Analytes were extracted from a 1 g sample by homogenization with acetonitrile/water (75:25, v/v, 25 mL final volume). 5 mL of crude extracts was cleaned-up on Carbograph-4 cartridges. Two fractions were obtained and were analyzed by HPLC-electrospray ionization (ESI) in negative mode. Recoveries for spiked maize samples were in the range 79-106% and method detection limits (MDLs) were ≤ 6 ng/g for all compounds, except fusarenon X (12 ng/g). 25 random maize samples were analyzed both by the ELISA-based methods specific for deoxynivalenol and zearalenone and by this method for trichothecenes B and macrocyclic lactones. Results were comparable for zearalenone (R~2 = 0.982), but disagreed for deoxynivalenol. Finally, a total of 78 freshly harvested maize samples, collected from central and northern Italy during 2002, and divided in two different experiments, were analyzed by the developed method. Data show that there exists a phenomenon of random contamination from the target fusariotoxins just before harvest and an increase of trichothecene B and zearalenone abundance on field crop possibly related to damp climate, temperature range and delayed harvest period. Deoxynivalenol was the most abundant (up to 3430 ng/g) and frequent mycotoxin (40%) detected, followed by acetyldeoxynivalenol. Derivatives of zearalenone were present in traces and p-zearalanol was never found.
机译:评价了一种敏感,可靠的液相色谱-串联质谱(HPLC-MS / MS)方法,用于确定玉米中镰刀菌菌株产生的一些常见真菌毒素,并将其应用于田间样品。选定的物质为:天花粉菌素B(新戊烯醇,脱氧新戊烯醇,富沙隆X,3-和15-乙酰基脱氧新戊烯醇)和一些大环内酯(玉米赤霉烯酮,α-和β-玉米赤霉烯醇,泽拉拉酮,α-和β-泽拉罗醇)。通过用乙腈/水(75:25,v / v,25 mL最终体积)匀浆从1 g样品中提取分析物。在Carbograph-4柱上纯化5 mL粗提物。获得了两个级分,并通过HPLC-电喷雾电离(ESI)以负模式进行了分析。加标玉米样品的回收率在79-106%范围内,所有方法的方法检出限(MDL)≤6 ng / g,除了富马农X(12 ng / g)。通过特异于脱氧雪腐烯醇和玉米赤霉烯酮的基于ELISA的方法以及针对毛孢菌素B和大环内酯的这种方法,分析了25个随机玉米样品。玉米赤霉烯酮的结果可比(R〜2 = 0.982),但脱氧雪腐烯醇的结果不同。最后,通过发达的方法分析了2002年从意大利中部和北部收集的总共78​​份新鲜收获的玉米样品,并分为两个不同的实验。数据表明,就在收获前,靶标fusario毒素有随机污染的现象,并且大田作物上的天花粉B和玉米赤霉烯酮的丰度增加可能与潮湿的气候,温度范围和延迟的收获期有关。脱氧雪茄烯醇含量最高(高达3430 ng / g),检出的真菌毒素最多(40%),其次是乙酰基脱氧雪茄烯醇。玉米赤霉烯酮的衍生物存在于痕量中,从未发现对-泽拉醇。

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