Visconti A, Boenke A, Solfrizzo M, Pascale M, Doko M B
Istituto Tossine e Micotossine da Parassiti Vegetali, Consiglio Nazionale delle Ricerche, Bari, Italy.
Food Addit Contam. 1996 Nov-Dec;13(8):909-27. doi: 10.1080/02652039609374479.
The results of an intercomparison study for the analysis of fumonisin B1 (FB1) and fumonisin B2 (FB2) in a contaminated maize material (Maize B, containing approximately 2 micrograms/g FB1 and 1 micrograms/g FB2) and its 'blank' counterpart (Maize A, containing less than 20 ng/g FB1 and FB2) are reported. Maize materials were distributed in 60 g sachets, submitted to gamma-irradiation at 15 kGy, and distributed to participating laboratories. The study was carried out by 24 European laboratories, most of which have national or international responsibilities for food/feed quality control. Participants used basically one method with some modifications, based on clean-up through SAX minicolumn and reversed phase HPLC with fluorescence detection of the OPA-fumonisin derivatives. The intercomparison study generated data (after correction for recoveries) with repeatability and reproducibility levels of: RSDr = 10% and RSDR = 11% for FB1; RSDr = 11% and RDSR = 13% for FB2. The recoveries obtained by most participants were considered low (70% for FB1 and 69% for FB2), being considerably affected by the extraction mode. Average recoveries for laboratories using blending were 62% and 60%, whereas for laboratories using shaking they were 85% and 86% for FB1 and FB2, respectively. The day-to-day- data showed a between-day, within-laboratory repeatability lower than 15% (CV < 15%) for FB1 for all laboratories, whereas only three laboratories obtained a between-day, within-laboratory reproducibility higher than 15% (CV > 15%) for FB2.
本文报告了一项比对研究的结果，该研究分析了受污染玉米材料（玉米B，含有约2微克/克伏马菌素B1（FB1）和1微克/克伏马菌素B2（FB2））及其“空白”对照物（玉米A，含有低于20纳克/克FB1和FB2）中的FB1和FB2。玉米材料被分装在60克的小包装中，经15千戈瑞的伽马射线辐照后分发给参与研究的实验室。该研究由24个欧洲实验室开展，其中大多数实验室负责国家或国际层面的食品/饲料质量控制。参与者基本采用一种经改进的方法，该方法基于通过SAX微型柱净化以及采用荧光检测OPA - 伏马菌素衍生物的反相高效液相色谱法。比对研究得出的数据（校正回收率后）显示，FB1的重复性和再现性水平为：相对标准偏差（RSDr）= 10%，相对标准偏差（RSDR）= 11%；FB2的重复性和再现性水平为：RSDr = 11%，相对标准偏差（RDSR）= 13%。大多数参与者获得的回收率较低（FB1为70%，FB2为69%），且受提取方式的影响很大。采用混合方式的实验室，FB1和FB2的平均回收率分别为62%和60%；而采用振荡方式的实验室，FB1和FB2的平均回收率分别为85%和86%。日常数据表明，所有实验室FB1的日内实验室内部重复性均低于15%（变异系数< 15%），而只有三个实验室FB2的日内实验室内部再现性高于15%（变异系数> 15%）。
