Medina Angel, Valle-Algarra Francisco M, Gimeno-Adelantado José V, Mateo Rufino, Mateo Fernando, Jiménez Misericordia
Departamento de Microbiologia y Ecologia, Facultad de Biología, Universitat de València, Dr. Moliner 50, E-46100 Burjassot, Valencia, Spain.
J Chromatogr A. 2006 Jul 21;1121(2):178-83. doi: 10.1016/j.chroma.2006.04.034. Epub 2006 May 11.
A new method for the determination of ochratoxin A (OTA) in beer has been developed. The new method has been compared with a reference method currently accepted as AOAC official first action. The limits of detection and quantification of the proposed method were 0.0008 and 0.0025 ng/ml, respectively, while they were 0.0025 and 0.0075 ng/ml, respectively, in the AOAC method used as reference. The recovery levels in the 0.025-0.40 ng OTA/ml spiking range for the proposed and the reference methods were 80.6-87.6% and 78.2-83.8%, respectively. The relative standard deviations of recoveries were 2.6-7.5% for the proposed method and 0.7-6.1% for the reference method. Passing and Bablok regression analysis of recovery data obtained by the proposed method versus data obtained by the reference method on an OTA-spiked beer sample showed good correlation (r2 = 0.9993), while the slope and intercept were 1.049 and -0.0013, respectively. The advantage of the proposed method is the low cost of the materials used in sample preparation because expensive immunoaffinity columns are not needed to clean-up samples while it maintains or even increases the good performance of the reference method. The proposed method was applied to 69 beer samples from different geographic origins (national and imported) but purchased in the Spanish market. They were found to be contaminated with OTA in the range from 0.008 to 0.498 ng/ml (average: 0.070 ng/ml). Five samples surpassed the limit recommended by the European Union (0.2 ng OTA/g).
已开发出一种测定啤酒中赭曲霉毒素A（OTA）的新方法。该新方法已与目前被AOAC官方首次采用的参考方法进行了比较。所提出方法的检测限和定量限分别为0.0008和0.0025 ng/ml，而用作参考的AOAC方法的检测限和定量限分别为0.0025和0.0075 ng/ml。在所提出方法和参考方法的0.025 - 0.40 ng OTA/ml加标范围内，回收率分别为80.6 - 87.6%和78.2 - 83.8%。所提出方法回收率的相对标准偏差为2.6 - 7.5%，参考方法为0.7 - 6.1%。对OTA加标啤酒样品上所提出方法获得的回收率数据与参考方法获得的数据进行的Passing和Bablok回归分析显示出良好的相关性（r2 = 0.9993），而斜率和截距分别为1.049和 -0.0013。所提出方法的优点是样品制备中使用的材料成本低，因为无需昂贵的免疫亲和柱来净化样品，同时它保持甚至提高了参考方法的良好性能。所提出的方法应用于从西班牙市场购买的69个来自不同地理来源（国内和进口）的啤酒样品。发现它们被OTA污染，污染范围为0.008至0.498 ng/ml（平均：0.070 ng/ml）。有5个样品超过了欧盟推荐的限量（0.2 ng OTA/g）。
