Senyuva Hamide Z, Gilbert John, Stroka Joerg, Biselli S, De Girolamo A, De Rijk T, De Saeger S, Köppen R, MacDonald S, Neumann G, Patel S, Seefelder W, Tibet U, Trucksess M W, van Osenbruggen W A, Zachariásová M
TUBITAK, Ankara Test and Analysis Laboratory, Konya Yolu No. 67, Besevler, 06530 Ankara, Turkey.
J AOAC Int. 2010 Mar-Apr;93(2):611-21.
An interlaboratory validation study was conducted to establish the method performance characteristics of an immunoaffinity column (IAC) cleanup procedure followed by LC/MS for the determination of fumonisins B1 (FB1) and B2 (FB2) and combined FB1 + FB2 in corn. The test portion is extracted with acetonitrile-methanol-water (25 + 25 + 50). The extract is filtered, diluted with phosphate-buffered saline solution, and applied to an IAC. FB1 and FB2 are removed with methanol, followed by water, then directly determined by RPLC with MS detection using selected-ion monitoring of two characteristic ions in each case. Naturally contaminated corn samples were milled to a fine powder and mixed to produce three samples with target levels of combined FB1 + FB2 ranging from 350 to 4000 microg/kg. Of 15 initially participating laboratories, two failed to report results and another did not follow the prescribed method. Thus, valid results were obtained from 12 participants located in 11 countries. Statistical analysis of the results produced RSDr values of 4.6-11.9, 1.9-12.6, and 1.4-11.5% for FB1, FB2, and combined FB1 + FB2, respectively; the corresponding RSDR values were 19.8-23.8, 18.2-25.5, and 18.8-23.2%. The three concentration levels of combined FB1 + FB2 were 534, 1194, and 1954 microg/kg. HorRat values for r and R were all < 2.0, indicating that the method is suitable as a regulatory method for the enforcement of European Union limits for fumonisins in corn.
开展了一项实验室间验证研究，以确定免疫亲和柱（IAC）净化程序结合液相色谱/质谱法测定玉米中伏马菌素B1（FB1）、B2（FB2）以及FB1与FB2总量的方法性能特征。称取试验份，用乙腈 - 甲醇 - 水（25 + 25 + 50）进行提取。提取物经过过滤，用磷酸盐缓冲盐溶液稀释后，加至IAC上。先用甲醇洗脱，再用水洗脱，去除FB1和FB2，然后直接采用反相液相色谱 - 质谱联用仪，通过选择离子监测每种伏马菌素的两个特征离子进行测定。将天然污染的玉米样品磨成细粉并混匀，制备出3个样品，其FB1与FB2总量的目标水平在350至4000 μg/kg之间。最初参与的15个实验室中，2个未报告结果，另1个未遵循规定方法。因此，从位于11个国家的12个参与者处获得了有效结果。结果的统计分析表明，FB1、FB2以及FB1与FB2总量的相对标准偏差（RSDr）值分别为4.6 - 11.9%、1.9 - 12.6%和1.4 - 11.5%；相应的相对标准偏差（RSDR）值分别为19.8 - 23.8%、18.2 - 25.5%和18.8 - 23.2%。FB1与FB2总量的3个浓度水平分别为534、1194和1954 μg/kg。r和R的HorRat值均< 2.0，表明该方法适合作为执行欧盟玉米中伏马菌素限量规定的监管方法。
