Inter-Laboratory Study of an LC-MS/MS Method for Simultaneous Determination of Fumonisin B_1,B_2 and B_3 in Corn

摘要

トウモロコシに含まれるフモニシンB_1(FB_1)フモニシンB_2(FB_2)およびフモニシンB_3(FB3)のLC-MS/MSを用いた同時分析法を評価するために，9機関の共同試験を実施した.試験には添加試料3種，自然汚染試料2種と陰性試料1種を用いた.FB_1, FB_2およびFB_3の回収率はそれぞれ79〜87%, 79〜103%および80〜93%であり， 室内再現性および室間再現性の相対標準偏差は3種のフモニシンいずれについてもそれぞれ20%および30%以下であり，HorRat値は0.2〜0.9の範囲であった.本分析法を用いて，国内で入手したコーングリッッ中に含まれるフモニシンを分析した.以上の結果より，本法はトウモロコシにおけるフモニシンの汚染実態調査に有用であることが示された.%Tovalidate an LC-MS/MS method using a strong anion exchange cartridge for simultaneous determination of fumonisin B_1, B_2 and B_3 in corn, an inter-laboratory study was performed in 9 laboratories using one fumonisin-negative corn sample, three spiked corn samples (FB_1 100-1,000 μg/kg, FB_2 and FB_3: 10-100 μg/kg) and two naturally contaminated corn samples. The recoveries were in the ranges of 79.7-87.2% for FB_1 78.6-103.2% for FB_2 and 80.1-92.8% for FB_3. The relative standard deviations for repeatability (RSDr) ranged from 3.7 to 8.0% for FB_1 from 2.6 to 15.3% for FB_2 and from 4.3 to 9.7% for FB_3. The relative standard deviations for reproducibility (RSDr) for FB_1， FB_2 and FB_3 were in the ranges of 6.3-10.1%, 5.9-18.7% and 9.3-16.0%, respectively. The HorRat values for all analytes ranged from 0.2 to 0.9. The difference of the trueness between the two kinds of commercially available anion exchange cartridges used in this study was not significant (p＞0.05). Surveillance for fumonisins in corn grits was performed using the validated method. All of the samples were contaminated with fumonisins and the mean concentrations for FB_1,FB_2 and FB_3were 118.1, 37.3 and 17.9 (μg/kg, respectively. These results indicated that the method for simultaneous determination of FB_1 FB_2 and FB_3 in corn was successfully developed and validated.