THE DETERMINATION OF HYDROXYLATED NATURAL PRODUCTS

7-[(氯甲酰基)甲氧基]-4-甲基香豆素(CMMC)是一种荧光物质 液体中羟基化合物的柱前衍生化试剂 层析法。酰氯的合成涉及到使用 亚硫酰氯，后来被证明无一例外地 引入由于氯化而产生的高荧光杂质 形成了酰氯。一种改进的衍生化试剂 使用反应性酰基咪唑，而不是酰氯， 提供更纯净的产品，同时保持所需的试剂 具有易于处理、衍生条件温和、 等。7-[(imidazolemethanoyl)methoxy]-4-methylcoumarin的反应。 与各种羟基化合物产生的酯很容易 可在反相高效液相色谱条件下分离与检测兼容 用热喷雾质谱仪测定。当被阳离子观察时 热喷雾质谱仪，这些化合物给出[M+H]+离子作为 它们的质谱图的基峰没有明显的碎裂。在……里面 这些化合物的负离子热喷雾质谱图，质子- 7-羟基-4-甲基香豆素的抽提阴离子(出现在m/z 175)是， 无一例外，基峰。

7-[(Chlorocarbonyl)methoxy]-4-methylcoumarin (CMMC) is a fluorescent reagent for precolumn derivatization of hydroxy compounds in liquid chromatography. The synthesis of the acyl chloride involves the use of thionyl chloride, which has been subsequently shown to unexceptably introduce highly fluorescent impurities due to chlorination in addition to formation of the acyl chloride. An improved derivatization reagent utilizes a reactive acyl imidazole, instead of the acyl chloride, offerring a purer product while maintaining desirable reagent characteristics such as ease of handling, mild derivatization conditions, etc. Reaction of 7-[(imidazolemethanoyl)methoxy]-4-methylcoumarin (IMMC) with various hydroxy compounds produces esters which are readily separable under reversed-phase HPLC conditions compatible with detection by thermospray mass spectrometry. When observed by positive ion thermospray mass spectrometry, these compounds give [M+H]+ ions as the base peak of their mass spectra with no discernible fragmentation. In the negative ion thermospray mass spectra of these compounds, the proton- abstracted anion of 7-hydroxy-4-methylcoumarin (appearing at m/z 175) is, without exception, the base peak.