Marti L R, Wilson D M, Evans B D
J Assoc Off Anal Chem. 1978 Nov;61(6):1353-8.
A method is described for determining citrinin in corn and barley. The initial extraction uses an aqueous acidified acetonitrile solution, and the resulting solution is partially purified by several partition steps. Citrinin is determined by using either high pressure liquid chromatography (HPLC) or thin layer chromatography (TLC). For HPLC, the extract is injected on a reverse phase column, eluted with either 0.25N H3PO4-methanol (45 + 55) or 0.25N H3PO4-acetonitrile (50 + 50), and detected by fluorescence (excitation 325--385 nm, emission above 451 nm). Recovery of added citrinin from corn by this method is 60--87% at levels of 50--4000 microgram/kg. For TLC, the chromatographic plates are impregnated with oxalic acid by dipping them in an oxalic acid-methanol solution before spotting and development. Recovery of added citrinin from corn, using TLC, is 40--100% at levels of 50--40000 microgram-kg.
描述了一种测定玉米和大麦中桔霉素的方法。初始提取使用酸化乙腈水溶液,所得溶液通过几个分配步骤进行部分纯化。桔霉素通过高压液相色谱法(HPLC)或薄层色谱法(TLC)测定。对于HPLC,提取物注入反相柱,用0.25N H3PO4-甲醇(45 + 55)或0.25N H3PO4-乙腈(50 + 50)洗脱,并通过荧光检测(激发波长325 - 385nm,发射波长高于451nm)。用该方法从玉米中添加桔霉素的回收率在50 - 4000微克/千克水平时为60 - 87%。对于TLC,在点样和展开前,将色谱板浸入草酸-甲醇溶液中用草酸浸渍。使用TLC从玉米中添加桔霉素的回收率在50 - 40000微克/千克水平时为40 - 100%。