Solfrizzo Michele, De Girolamo Annalisa, Gambacorta Lucia, Visconti Angelo, Stroka Joerg, Van Egmond Hans P
Institute of Sciences of Food Production, National Research Council of Italy, Via Amendola, 122/0-70126 Bari, Italy.
J AOAC Int. 2011 May-Jun;94(3):900-8.
A liquid chromatographic method for the determination of fumonisins B1 (FB1) and B2 (FB2) in corn-based foods for infants and young children was subjected to an interlaboratory validation study involving 11 laboratories. Five blind duplicate sample pairs of each matrix were analyzed to establish the accuracy, repeatability, and reproducibility of the method. Mass fractions in the baby food samples ranged from 89.1 to 384.4 microg/kg FB1 and from 22.5 to 73.6 microg/kg FB2. The method involved a warm extraction with citrate phosphate buffer-methanol-acetonitrile (50 + 25 + 25, v/v/v), a cleanup through an immunoaffinity column, and an end-determination of fumonisins by LC after automated precolumn derivatization with o-phthaldialdehyde reagent. RSDs for within-laboratory repeatability (RSDr) ranged from 6.8 to 23.5% for FB1 and 7.6 to 22.9% for FB2. RSDs for between-laboratory reproducibility (RSDR) ranged from 15.4 to 26.2% for FB1 and 21.6 to 36.3% for FB2. Mean FB1 recoveries from baby foods spiked at 100.0 and 250.0 microg/kg were 89 and 96%, respectively; for FB2 spiked foods at 25.0 and 62.5 microg/kg recoveries were 90 and 85%, respectively. HorRat values ranged from 0.8 to 1.2 for FB1, whereas for FB2 they ranged from 0.9 to 1.4 when calculated according to Horwitz, and from 1.0 to 1.7 when calculated according to Thompson, indicating an acceptable among-laboratory precision for all matrixes (HorRat values <2).
一种用于测定婴幼儿玉米基食品中伏马毒素B1（FB1）和B2（FB2）的液相色谱法，接受了一项由11个实验室参与的实验室间验证研究。对每种基质的5对盲法重复样品进行分析，以确定该方法的准确性、重复性和再现性。婴儿食品样品中的质量分数范围为FB1 89.1至384.4微克/千克，FB2 22.5至73.6微克/千克。该方法包括用柠檬酸磷酸盐缓冲液 - 甲醇 - 乙腈（50 + 25 + 25，v/v/v）进行温热萃取，通过免疫亲和柱净化，以及在用邻苯二甲醛试剂进行自动柱前衍生化后通过液相色谱法对伏马毒素进行最终测定。FB1的实验室内重复性相对标准偏差（RSDr）范围为6.8%至23.5%，FB2为7.6%至22.9%。实验室间再现性相对标准偏差（RSDR）范围为FB1 15.4%至26.2%，FB2为21.6%至36.3%。在100.0和250.0微克/千克加标的婴儿食品中，FB1的平均回收率分别为89%和96%；在25.0和62.5微克/千克加标的FB2食品中，回收率分别为90%和85%。根据Horwitz计算时，FB1的HorRat值范围为0.8至1.2，而FB2为0.9至1.4；根据Thompson计算时，FB2的HorRat值范围为1.0至1.7，这表明所有基质的实验室间精密度均可接受（HorRat值<2）。
