Trucksess M W, Stoloff L
J Assoc Off Anal Chem. 1984 Mar-Apr;67(2):317-20.
Procedures from 2 methods, one for aflatoxins B1 and M1 in eggs and one for aflatoxicol in milk, blood, and liver, have been combined to determine the 3 toxins in eggs. The sample is blended with sodium chloride-saturated water and this mixture is then blended with acetone. After separation from the solid residue, the aqueous acetone extract is defatted with petroleum ether. The toxins are next partitioned into chloroform and separated from interferences on a silica gel column. Aflatoxicol is determined by fluorescence measurement after separation on a C18 reverse phase liquid chromatographic column, and aflatoxins B1 and M1 are determined by fluorescence densitometry after separation on a silica gel thin layer chromatographic plate. In a recovery study with eggs, mean recoveries of aflatoxicol added at levels of 0.1, 0.05, and 0.025 ng/g were 87, 77, and 78%, respectively. Mean recoveries of aflatoxins B1 and M1 added at a level of 0.1 ng/g were 75 and 87%, respectively, and at an added level of 0.05 ng/g were 86 and 75%. The within-laboratory precision (repeatability) ranged from 2 to 13%.
已将两种方法的步骤相结合来测定鸡蛋中的三种毒素,其中一种方法用于检测鸡蛋中的黄曲霉毒素B1和M1,另一种方法用于检测牛奶、血液和肝脏中的黄曲霉毒素醇。将样品与饱和氯化钠水溶液混合,然后将此混合物与丙酮混合。从固体残渣中分离后,用石油醚对丙酮水提取物进行脱脂。接下来将毒素分配到氯仿中,并在硅胶柱上与干扰物分离。黄曲霉毒素醇在C18反相液相色谱柱上分离后通过荧光测量进行测定,黄曲霉毒素B1和M1在硅胶薄层色谱板上分离后通过荧光密度测定法进行测定。在一项针对鸡蛋的回收率研究中,添加水平为0.1、0.05和0.025 ng/g的黄曲霉毒素醇的平均回收率分别为87%、77%和78%。添加水平为0.1 ng/g的黄曲霉毒素B1和M1的平均回收率分别为75%和87%,添加水平为0.05 ng/g时分别为86%和75%。实验室内精密度(重复性)范围为2%至13%。