Phillips T D, Stein A F, Ivie G W, Kubena L F, Hayes A W, Heidelbaugh N D
J Assoc Off Anal Chem. 1983 May;66(3):570-6.
The mycotoxin ochratoxin A (OA) was derivatized to an O-methyl,methyl ester (Me2) with diazomethane and then determined by high pressure liquid chromatography (HPLC). Both OA and OA-Me2 were chromatographed by reverse phase HPLC with a mobile phase of acetonitrile-water (60 + 40). An increase in retention time of 309 s was observed with OA-Me2 which was detectable at 254 nm at levels as low as 3 ng. Recovery of OA as OA-Me2 from chicken kidney homogenates and human plasma was quantitative following simple extraction and cleanup procedures, reaction with diazomethane, and HPLC analysis. The novel method described should prove useful for measuring and confirming OA in tissues and in further studies on the biological fate of this mycotoxin.
霉菌毒素赭曲霉毒素A(OA)用重氮甲烷衍生化为O-甲基甲酯(Me2),然后通过高压液相色谱法(HPLC)进行测定。OA和OA-Me2均采用反相HPLC进行色谱分析,流动相为乙腈-水(60 + 40)。观察到OA-Me2的保留时间增加了309秒,在254nm处可检测到低至3ng的水平。经过简单的提取和净化程序、与重氮甲烷反应以及HPLC分析后,从鸡肾匀浆和人血浆中以OA-Me2形式回收的OA是定量的。所描述的新方法对于测量和确认组织中的OA以及对这种霉菌毒素的生物归宿进行进一步研究应该是有用的。