Fujino H, Goya S
Faculty of Pharmaceutical Sciences, Kumamoto University, Japan.
Yakugaku Zasshi. 1991 Aug;111(8):463-7. doi: 10.1248/yakushi1947.111.8_463.
Pyrene-1-carbonyl fluoride (PCF) was synthesized as a precolumn fluorescent labeling reagent for alcohols and amines for use in high performance liquid chromatography (HPLC). PCF reacted with primary and phenolic hydroxyl groups in dichloromethane at 100 degrees C for 30 min in the presence of 4-dimethylaminopyridine (DMAP) to give the corresponding fluorescent pyrene esters and also reacted with primary amines in acetonitrile at room temperature for 2 min in the presence of DMAP to give the amides. The PCF esters of corticosteroids were separated by normal-phase chromatography on a Cosmosil 5 SL column with hexane-ethyl acetate (6:5, v/v) and the PCF amides of primary amines were separated by reversed-phase chromatography on a TSK gel ODS-80 TM column with methanol-water (10:3, v/v). The detection limits (S/N = 3) of cortisone and 2-phenylethylamine were 600 fmol and 800 fmol for an injection volume of 10 microliters, respectively.
芘-1-羰基氟化物（PCF）被合成为一种用于高效液相色谱（HPLC）的醇类和胺类的柱前荧光标记试剂。PCF在4-二甲氨基吡啶（DMAP）存在下，于100℃在二氯甲烷中与伯羟基和酚羟基反应30分钟，生成相应的荧光芘酯，并且在DMAP存在下于室温在乙腈中与伯胺反应2分钟，生成酰胺。皮质类固醇的PCF酯在Cosmosil 5 SL柱上用己烷-乙酸乙酯（6:5，v/v）通过正相色谱法分离，伯胺的PCF酰胺在TSK凝胶ODS-80 TM柱上用甲醇-水（10:3，v/v）通过反相色谱法分离。对于10微升的进样体积，可的松和2-苯乙胺的检测限（S/N = 3）分别为600飞摩尔和800飞摩尔。
