Nakano Yukitaka, Nohta Hitoshi, Yoshida Hideyuki, Todoroki Kenichiro, Saita Tetsuya, Fujito Hiroshi, Mori Masato, Yamaguchi Masatoshi
Department of Pharmacy, Saga University Hospital, 5-1-1 Nabeshima, Saga 849-8501, Japan.
Anal Sci. 2004 Mar;20(3):489-93. doi: 10.2116/analsci.20.489.
A selective liquid chromatographic method has been developed for the assay of ethambutol in serum samples. The assay involves intramolecular excimer-forming derivatization with 4-(1-pyrene)butanoyl chloride (PBC) and isocratic reversed-phase chromatography with fluorescence detection. After acetonitrile-deproteinization of the serum sample, the derivatization reaction of ethambutol with PBC was completed within 30 min at 50 degrees C. N,N'-Diethylethylenediamine was used as an internal standard. The detection limit of ethambutol was 23 ng/ml serum, corresponding to 180 fmol on column at a signal-to-noise ratio of 3. The present method was selective enough to analyze ethambutol in rabbit serum without any tedious sample clean-up procedure because biogenic monoamines gave no peak in the chromatogram. The method was applicable to drug monitoring in rabbit serum.
已开发出一种用于测定血清样品中乙胺丁醇的选择性液相色谱法。该测定方法包括用4-(1-芘)丁酰氯(PBC)进行分子内准分子形成衍生化以及采用荧光检测的等度反相色谱法。血清样品经乙腈脱蛋白后，乙胺丁醇与PBC的衍生化反应在50℃下30分钟内完成。使用N,N'-二乙基乙二胺作为内标。乙胺丁醇的检测限为23 ng/ml血清，在信噪比为3时相当于柱上180 fmol。由于生物源性单胺在色谱图中无峰，本方法具有足够的选择性，无需任何繁琐的样品净化程序即可分析兔血清中的乙胺丁醇。该方法适用于兔血清中的药物监测。
