液相色谱-质谱联用分析镰刀菌毒素的研究进展

Mycotoxins Pub Date : 2014-01-01 DOI:10.2520/MYCO.64.55
H. Nakagawa
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引用次数: 0

摘要

采用液相色谱串联质谱(LC-MS/MS)技术建立了小麦和大麦中5种镰刀菌毒素(脱氧雪腐镰刀菌醇、雪腐镰刀菌醇、T- 2毒素、HT- 2毒素和玉米赤霉烯酮)的同时多重检测方法,并由12个实验室的参与者进行了协调协作验证。虽然有很多关于仪器分析同时和多重检测镰刀菌毒素的报道,但发展到统一协同验证的报道很少。用LC-MS/MS分析霉菌毒素时,提取效率的差异和基质对电离的影响有时是不可忽略的,然而,本方法采用内标显然有助于弥补这些影响。这是第一个采用LC-MS/MS同时和多重测定a型和B型毛霉烯以及ZEA的方法,并通过协调协作验证进行验证。另一方面,采用LC-Orbitrap MS进行精确的质量和高分辨率测量,用于筛选新的隐匿真菌毒素。因此,分别检测了小麦籽粒中B型曲霉烯的单葡萄糖苷衍生物(雪腐镰刀菌醇和fusarenon-X)和玉米粉样品中A型曲霉烯的单葡萄糖苷衍生物(T- 2毒素、HT- 2毒素、新茄油醇、二乙酰氧基旋甲醇和单乙酰氧基旋甲醇)。还发现了T- 2毒素和HT- 2毒素的二糖苷衍生物。我们的研究结果表明,隐匿真菌毒素的存在并不局限于某些特定的真菌毒素,如脱氧雪腐镰刀菌醇和玉米赤霉烯酮,但可能与其他镰刀菌毒素。
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State of the art in the analyisis of Fusarium toxins by liquid chromatography-mass spectrometry (LC-MS)
A simultaneous and multiple determination method for the major five Fusarium toxins (deoxynivalenol, nivalenol, T- 2 toxin, HT- 2 toxin, and zearalenone) contaminating wheat and barley was developed with liquid chromatography tandem-mass spectrometry (LC-MS/MS), and a harmonized collaborative validation of the method was conducted by the participants of 12 laboratories. Although there are many reports on the simultaneous and multiple determination of Fusarium toxins by instrumental analysis, only a few of them are developed to the harmonized collaborative validation. The variance in the extraction efficiency and the matrix effects on the ionization were occasionally innegli gible with the mycotoxin analysis by LC-MS/MS, however, the employment of internal standards with the present method apparently contributed to compensate for these effects. This is the first report of a simultaneous and multiple determination method for both type A and B trichothecenes along with ZEA by LC-MS/MS that was validated through the harmonized collaborative validation. On the other hand, the accurate mass and high-resolution measurement was carried out with LC-MS (LC-Orbitrap MS) for the screening of new masked mycotoxins. Consequently, mono-glucoside derivatives of type B trichothecenes (nivalenol and fusarenon-X) in wheat grains and those of type A trichothecenes (T- 2 toxin, HT- 2 toxin, neosolaniol, diacetoxyscirpenol, and monoacetoxyscirpenol) in corn powder sample were detected, respectively. Di-glucoside derivatives were also found for T- 2 toxin and HT- 2 toxin. Our findings indicate that the presence of masked mycotoxins is not limited to some specific mycotoxins such as deoxynivalenol and zearalenone, but likely with the other Fusarium toxins.
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