Munns R K, Roybal J E, Shimoda W, Hurlbut J A
Animal Drug Research Center, Food and Drug Administration, Denver Federal Center, CO 80225.
J Chromatogr. 1988 Jun 17;442:209-18. doi: 10.1016/s0021-9673(00)94469-8.
A method is presented for the derivatization and determination of carboxylic acids by high-performance liquid chromatography with electrochemical and ultraviolet detection. The derivatizing reagents used in this study were synthesized, and their suitability was investigated for determination of drugs and metabolites with carboxylic acid groups. Quinoxaline-2-carboxylic, benzoic and salicylic acids each labeled with 1-(4-hydroxyphenyl)-, 1-(2,4-dihydroxyphenyl)- and 1-(2,5-dihydroxyphenyl)-2-bromoethanone were the principal esters studied; in addition, some antibiotics and their salts were also esterified. Conditions of derivatization are relatively mild at 60 degrees C for 60 min or less, and the reaction is 76% complete. The detection limits are as low as 1 pmol for some acids. Clean-up steps are not required to remove excess derivatizing reagent.
本文介绍了一种通过高效液相色谱结合电化学和紫外检测对羧酸进行衍生化和测定的方法。本研究中使用的衍生化试剂是合成的，并研究了它们对于测定含羧酸基团的药物和代谢物的适用性。喹喔啉 - 2 - 羧酸、苯甲酸和水杨酸分别与1 - （4 - 羟基苯基） - 、1 - （2,4 - 二羟基苯基） - 和1 - （2,5 - 二羟基苯基） - 2 - 溴乙酮标记的酯是主要研究对象；此外，一些抗生素及其盐也进行了酯化。衍生化条件相对温和，在60℃下进行60分钟或更短时间，反应完成度达76%。某些酸的检测限低至1皮摩尔。无需进行净化步骤以去除过量的衍生化试剂。
