Rouan M C, Souppart C, Alif L, Moes D, Lecaillon J B, Godbillon J
Laboratories Ciba-Geigy, Centre de Bioanalyse et Pharmacocinétique, Rueil-Malmaison, France.
J Chromatogr B Biomed Appl. 1995 May 19;667(2):307-13. doi: 10.1016/0378-4347(95)00026-f.
Automated procedures for the determination of CGP 33,101 in plasma and the simultaneous determination of CGP 33,101 and its carboxylic acid metabolite, CGP 47,292, in urine are described. Plasma was diluted with water and urine with a pH 2 buffer prior to extraction. The compounds were automatically extracted on reversed-phase extraction columns and injected onto an HPLC system by the automatic sample preparation with extraction columns (ASPEC) automate. A Superlosil LC-18 (5 microns) column was used for chromatography. The mobile phase was a mixture of an aqueous solution of potassium dihydrogen phosphate, acetonitrile and methanol for the assay in plasma, and of an aqueous solution of tetrabutylammonium hydrogen sulfate, tripotassium phosphate and phosphoric acid and of acetonitrile for the assay in urine. The compounds were detected at 230 nm. The limit of quantitation was 0.11 mumol/l (25 ng/ml) for the assay of CGP 33,101 in plasma, 11 mumol/l (2.5 micrograms/ml) for its assay in urine and 21 mumol/l (5 micrograms/ml) for the assay of CGP 47,292 in urine.
本文描述了血浆中CGP 33,101的自动测定方法以及尿液中CGP 33,101及其羧酸代谢物CGP 47,292的同时测定方法。提取前，血浆用水稀释，尿液用pH 2缓冲液稀释。通过自动样品制备萃取柱（ASPEC）自动进样器，将化合物在反相萃取柱上自动萃取并注入高效液相色谱系统。采用Superlosil LC-18（5微米）柱进行色谱分析。血浆分析的流动相是磷酸二氢钾水溶液、乙腈和甲醇的混合物，尿液分析的流动相是硫酸氢四丁铵、磷酸三钾和磷酸的水溶液与乙腈的混合物。化合物在230纳米处检测。血浆中CGP 33,101测定的定量限为0.11微摩尔/升（25纳克/毫升），尿液中其测定的定量限为11微摩尔/升（2.5微克/毫升），尿液中CGP 47,292测定的定量限为21微摩尔/升（5微克/毫升）。
