Ferguson-Foos J, Warren J D
J Assoc Off Anal Chem. 1984 Nov-Dec;67(6):1111-4.
A rapid method is described for extraction and cleanup of raw and processed milk for determination of aflatoxins M1 and M2 by using a C18 Sep-Pak/silica gel cleanup column combination. Aflatoxins are separated by normal phase liquid chromatography and their concentrations are determined by fluorescence detection in a silica gel-packed flow cell. Recoveries ranged from 99 to 103% with coefficients of variation less than 2% for M1 levels of 0.117-1.17 ng/mL added to raw milk. Similar recoveries were obtained for M2. The coefficient of variation for analysis of 5 subsamples of naturally contaminated milk was less than 1%. Agreement with the official method is satisfactory. Each sample requires less than 25 mL solvent and 10 min actual handling time. Sample chromatograms show no interferences in the M1-M2 elution region and no late-eluting peaks, which permits spacing injections at 13-20 min intervals. Aflatoxin levels as low as 0.03 ppb may be determined by this procedure. Extracts have also been analyzed by thin layer chromatography.
描述了一种快速方法，用于通过使用C18 Sep - Pak/硅胶净化柱组合来提取和净化生乳和加工乳，以测定黄曲霉毒素M1和M2。黄曲霉毒素通过正相液相色谱法分离，并在硅胶填充的流通池中通过荧光检测来测定其浓度。对于添加到生乳中浓度为0.117 - 1.17 ng/mL的M1水平，回收率范围为99%至103%，变异系数小于2%。M2也获得了类似的回收率。对5个天然污染乳子样分析的变异系数小于1%。与官方方法的一致性令人满意。每个样品所需溶剂少于25 mL，实际处理时间为10分钟。样品色谱图显示在M1 - M2洗脱区域无干扰，也无晚洗脱峰，这允许以13 - 20分钟的间隔进样。通过该方法可测定低至0.03 ppb的黄曲霉毒素水平。提取物也已通过薄层色谱法进行分析。
