Park D L, Nesheim S, Trucksess M W, Stack M E, Newell R F
Food and Drug Administration, Division of Contaminants Chemistry, Washington, DC 20204.
J Assoc Off Anal Chem. 1990 Mar-Apr;73(2):260-6.
A collaborative study of a liquid chromatographic method for the determination of aflatoxins B1, B2, G1, and G2 was conducted in laboratories located in the United States, Canada, South Africa, and Switzerland. Twenty-one artificially contaminated raw peanuts, peanut butter, and corn samples containing varying amounts of aflatoxins B1, B2, G1, and G2 were distributed to participating laboratories. The test portion was extracted with methanol-0.1N HCl (4 + 1), filtered, defatted with hexane, and then partitioned with methylene chloride. The concentrated extract was passed through a silica gel column. Aflatoxins B1 and G1 were derivatized with trifluoroacetic acid, and the individual aflatoxins were determined by reverse-phase liquid chromatography with fluorescence detection. Statistical analysis of the data was performed to determine or confirm outliers, and to compute repeatability and reproducibility of the method. For corn, relative standard deviations for repeatability (RSDr) for aflatoxin B1 ranged from 27.2 to 8.3% for contamination levels from 5 through 50 ng/g. For raw peanuts and peanut butter, RSDr values for aflatoxin B1 were 35.0 to 41.2% and 11.2 to 19.1%, respectively, for contamination levels from 5 through 25 ng/g. RSDr values for aflatoxins B2, G1, and G2 were similar. Relative standard deviations for reproducibility (RSDr) for aflatoxin B1 ranged from 15.8 to 38.4%, 24.4 to 33.4%, and 43.9 to 54.0% for corn, peanut butter, and raw peanuts, respectively. The method has been adopted official first action for the determination of aflatoxins B1, B2, G1, and G2 in peanut butter and corn at concentrations greater than or equal to 13 ng total aflatoxins/g.
美国、加拿大、南非和瑞士的实验室共同开展了一项用于测定黄曲霉毒素B1、B2、G1和G2的液相色谱法的研究。向参与研究的实验室分发了21份人工污染的生花生、花生酱和玉米样品,这些样品含有不同含量的黄曲霉毒素B1、B2、G1和G2。将测试部分用甲醇 - 0.1N盐酸(4 + 1)萃取,过滤,用己烷脱脂,然后用二氯甲烷分配。浓缩提取物通过硅胶柱。黄曲霉毒素B1和G1用三氟乙酸衍生化,各黄曲霉毒素通过带荧光检测的反相液相色谱法测定。对数据进行统计分析以确定或确认异常值,并计算该方法的重复性和再现性。对于玉米,黄曲霉毒素B1重复性(RSDr)的相对标准偏差在污染水平为5至50 ng/g时,范围为27.2%至8.3%。对于生花生和花生酱,黄曲霉毒素B1的RSDr值在污染水平为5至25 ng/g时,分别为35.0%至41.2%和11.2%至19.1%。黄曲霉毒素B2、G1和G2的RSDr值相似。黄曲霉毒素B1再现性(RSDr)的相对标准偏差对于玉米、花生酱和生花生分别为15.8%至38.4%、24.4%至33.4%和43.9%至54.0%。该方法已被正式首次采用,用于测定花生酱和玉米中总黄曲霉毒素含量大于或等于13 ng/g时的黄曲霉毒素B1、B2、G1和G2。