Czerwiecki L
Zakład Analizy Zywności, Instytut Biotechnologii Przemysłu Rolno-Spozywczego, Warszawa.
Rocz Panstw Zakl Hig. 1998;49(1):1-11.
The aim of this study was to perform a optimized method for determination of aflatoxin M1 in milk. The manner of extraction and clean-up of milk extracts as well conditions of reaction of aflatoxin M1 with TFA and HPLC was described. The main steps of optimized method were: extraction of samples with chloroform, clean-up of extracts on SPE C18 columns and by means of extraction with n-hexane, derivatisation of aflatoxin M1 with TFA (60 degrees C, 6 minutes) to acetal form--aflatoxin M2a and determination of aflatoxin by means of the RP-HPLC technique. The mobile phase was a mixture of methanol, isopropanol and water (18 + 7 + 75). Fluorometric detection was made at 370/418-700 nm. The mean recovery of aflatoxin M1 dependent on fortification level was 62-67%, limit of detection was 0.01 microgram/1 of milk.
本研究的目的是建立一种测定牛奶中黄曲霉毒素M1的优化方法。文中描述了牛奶提取物的提取和净化方式以及黄曲霉毒素M1与三氟乙酸（TFA）反应和高效液相色谱（HPLC）的条件。优化方法的主要步骤如下：用氯仿提取样品，在固相萃取C18柱上净化提取物并通过正己烷萃取，用三氟乙酸（60℃，6分钟）将黄曲霉毒素M1衍生化为缩醛形式——黄曲霉毒素M2a，并用反相高效液相色谱（RP-HPLC）技术测定黄曲霉毒素。流动相为甲醇、异丙醇和水的混合物（18 + 7 + 75）。荧光检测在370/418 - 700nm下进行。黄曲霉毒素M1的平均回收率取决于强化水平，为62 - 67%，检测限为0.01微克/1毫升牛奶。
