Josephs R D, Schuhmacher R, Krska R
Center for Analytical Chemistry, Institute for Agrobiotechnology, Tulln, Austria.
Food Addit Contam. 2001 May;18(5):417-30. doi: 10.1080/02652030120332.
Twenty-eight laboratories from 12 different countries participated in an interlaboratory study for the determination of the Fusarium mycotoxin zearalenone (ZON) in maize and deoxynivalenol (DON) in maize and wheat employing their usual in-house methods. The aim of this study was to obtain information about the state-of-the-art of ZON and DON analysis in cereals and to support a knowledge and experience exchange between the participating laboratories in the field of mycotoxin analysis. Eight different sample types were distributed to the participants, 'blank' materials, spiked samples (102 microg/kg ZON in maize and 475 microg/kg DON in wheat) and naturally-contaminated maize and wheat. For the final separation and quantification either gas chromatography (GC), high performance liquid chromatography (HPLC), thin layer chromatography (TLC) or enzyme linked immunosorbent assays (ELISA) were employed by the participating laboratories. Coefficients of variation (CV) between laboratory mean results (outliers rejected) ranged from 28 to 41% for ZON and from 32 to 38% for DON. The results are close to the between laboratory CV criteria of 40% for DON and ZON at concentration levels of >100 microg/kg established by the CEN in 1999. A good trueness was obtained for the wheat samples spiked at 475 microg/kg DON. However, a significant deviation at p = 0.01 from the respective target value was observed for the maize samples spiked at 102 microg/kg ZON. The high CVs can be traced back to problems occurring by determination of the concentration of the participants' own calibrant solutions. Additionally, the variability of the results is strongly influenced by the use of different final separation and quantification procedures.
来自12个不同国家的28个实验室参与了一项实验室间研究,采用各自常用的内部方法测定玉米中的镰刀菌霉菌毒素玉米赤霉烯酮(ZON)以及玉米和小麦中的脱氧雪腐镰刀菌烯醇(DON)。本研究的目的是获取谷物中ZON和DON分析的最新技术信息,并支持参与实验室在霉菌毒素分析领域的知识和经验交流。向参与者分发了8种不同类型的样品,即“空白”材料、加标样品(玉米中ZON含量为102微克/千克,小麦中DON含量为475微克/千克)以及天然污染的玉米和小麦。参与实验室采用气相色谱法(GC)、高效液相色谱法(HPLC)、薄层色谱法(TLC)或酶联免疫吸附测定法(ELISA)进行最终的分离和定量分析。实验室平均结果(剔除异常值后)之间的变异系数(CV),ZON为28%至41%,DON为32%至38%。这些结果接近欧洲标准化委员会(CEN)在1999年确定的浓度水平>100微克/千克时DON和ZON的实验室间CV标准40%。对于加标量为475微克/千克DON的小麦样品,获得了良好的准确度。然而,对于加标量为102微克/千克ZON的玉米样品,在p = 0.01时观察到与各自目标值存在显著偏差。高CV可追溯到测定参与者自己校准溶液浓度时出现的问题。此外,结果的变异性还受到使用不同最终分离和定量程序的强烈影响。