Josephs Ralf Dieter, Krska Rudolf, MacDonald Susan, Wilson Pete, Pettersson Hans
Center for Analytical Chemistry, Institute for Agrobiotechnology (IFA-Tulln), Konrad Lorenz Strasse 20, 3430, Tulln, Austria.
Anal Bioanal Chem. 2004 Mar;378(5):1182-9. doi: 10.1007/s00216-003-2300-8. Epub 2004 Jan 21.
Several previous interlaboratory studies in the field of mycotoxin analysis have revealed considerable problems, apparent as high between-laboratory standard deviations, or rather non-comparable and non-traceable results. A major reason is lack of proper calibrants for external calibration. Public awareness of substances that mimic or interfere with the activity of natural hormones (endocrine disrupters) has led to increased interest in mycotoxins with estrogenic potential, e.g. zearalenone (ZON). During a large-scale standard measurement and testing (SMT) project of the European Commission (EC) dealing with the preparation and certification of reference materials for determination of the mycotoxin ZON in maize, a ZON calibrant in acetonitrile was prepared and intensively checked for purity, homogeneity, and stability. Preparation of the material, study of its homogeneity and stability, and characterisation of the calibrant on the basis of its preparation, with discussion of the results obtained, are described in this paper. The certified value of 9.95 micro g mL(-1) for ZON in acetonitrile and its corresponding expanded uncertainty of +/-0.30 micro g mL(-1) were calculated in compliance with the Guide to the Expression of Uncertainty in Measurement (GUM).
此前在霉菌毒素分析领域开展的多项实验室间研究揭示了相当多的问题,表现为实验室间标准偏差较高,或者说结果不可比且无法溯源。一个主要原因是缺乏用于外部校准的合适校准物。公众对模拟或干扰天然激素(内分泌干扰物)活性的物质的认知,导致对具有雌激素潜力的霉菌毒素(如玉米赤霉烯酮,ZON)的兴趣增加。在欧盟委员会(EC)开展的一个大规模标准测量与测试(SMT)项目中,该项目涉及玉米中霉菌毒素ZON测定参考物质的制备和认证,制备了乙腈中的ZON校准物,并对其纯度、均匀性和稳定性进行了深入检查。本文描述了该物质的制备、其均匀性和稳定性研究,以及基于其制备过程对校准物的特性描述,并对所得结果进行了讨论。根据《测量不确定度表示指南》(GUM)计算得出,乙腈中ZON的认证值为9.95微克/毫升,其相应的扩展不确定度为±0.30微克/毫升。