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A Validated UPLC-MS/MS Multi-mycotoxin Method for Nuts and Cerealsfor the Official Control in Cyprus within the EU Requirements

机译:经验证的UPLC-MS / MS多真菌毒素方法,可用于欧盟要求范围内的塞浦路斯官方控制的坚果和谷物

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The validation of a rapid, reliable and sensitive method for the simultaneous determination of Aflatoxins (AFB1, AFB2, AFG1, AFG2), Ochratoxin A, Zearalenone, Deoxynivalenol, Fumonisins B1 and B2, T-2 and HT-2 toxins, in nuts (peanuts, pistachio and almonds) and cereals (maize and wheat) is reported. The method was developed and validated to fulfil the requirements of the official control of mycotoxins according to EU legislation. This method is based on a single extraction step using an acetonitrile/ water mixture followed by the analysis of the diluted crude extract using ultra high performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS). The MS/MS detection was carried out using an electro spray-ionization interface (ESI) in positive ion mode. Matrix-matched calibration was used for the quantification of the mycotoxins, because of the absence of further clean up steps that reduce suppression/enhancement matrix effects. The method performance characteristics were determined after spiking blank samples on multiple levels. The mean recoveries of mycotoxins in spiked nuts ranged from 74.4% to 131.7%, while in cereals ranged from 52.8% to 113.9%. Relative standard deviations were lower than 20.4% for all target mycotoxins. Limits of detection and quantification for nuts and cereals ranged 0.08-30.0 and 0.25-99.0 μg/Κg, respectively.
机译:同时测定坚果中黄曲霉毒素(AFB1,AFB2,AFG1,AFG2),O曲毒素A,玉米赤霉烯酮,脱氧雪腐烯醇,伏马菌素B1和B2,T-2和HT-2毒素的快速,可靠和灵敏方法的验证(据报道花生,开心果和杏仁)和谷类(玉米和小麦)。该方法的开发和验证符合欧盟法规对霉菌毒素进行官方控制的要求。该方法基于使用乙腈/水混合物的单一提取步骤,然后使用超高效液相色谱-串联质谱法(UPLC-MS / MS)分析稀释的粗提物。使用正离子模式的电喷雾电离界面(ESI)进行MS / MS检测。基质匹配的校准用于真菌毒素的定量分析,因为没有进一步的纯化步骤可减少抑制/增强基质的作用。加标空白样品后,确定方法的性能特征。加标坚果中霉菌毒素的平均回收率为74.4%至131.7%,而谷物中霉菌毒素的平均回收率为52.8%至113.9%。所有目标真菌毒素的相对标准偏差均低于20.4%。坚果和谷物的检出限和定量限分别为0.08-30.0和0.25-99.0μg/Κg。

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