Mangoni P, Sioufi A, Godbillon J
Ciba-Geigy Laboratories, Reuil-Malmaison, France.
J Chromatogr B Biomed Appl. 1995 Feb 17;664(2):393-400. doi: 10.1016/0378-4347(94)00471-g.
The simultaneous determination of CGP 50 068, S(-)-enantiomer (I), its (-)-carboxylic acid metabolite CGP 55 461 (II) and the related (+)-enantiomer CGP 54 228 (III) by stereospecific high-performance liquid chromatography, in human plasma, is described. The three compounds and racemic acebutolol, used as internal standard, were isolated from plasma by liquid-solid extraction on disposable C18 columns. The resolution and determination of I and the two carboxylic acid enantiomers were achieved by direct chromatography using a Chiral-AGP column refrigerated at 5 degrees C. The mobile phase was tetrabutylammonium iodide in a pH 7 phosphate buffer solution used at a constant flow-rate of 0.5 ml/min. The UV detection wavelength was set at 270 nm. The reproducibility and accuracy of the method were found to be suitable over the concentration range 0.56-28.0 mumol/l for II and III and 2.0-26.7 mumol/l for I.
本文描述了采用立体特异性高效液相色谱法同时测定人血浆中CGP 50 068的S(-)-对映体（I）、其(-)-羧酸代谢物CGP 55 461（II）以及相关的(+)-对映体CGP 54 228（III）。使用一次性C18柱通过液固萃取从血浆中分离出这三种化合物以及用作内标的外消旋醋丁洛尔。通过使用在5℃冷藏的Chiral-AGP柱直接色谱法实现了I与两种羧酸对映体的分离和测定。流动相为碘化四丁铵，其在pH 7的磷酸盐缓冲溶液中以0.5 ml/min的恒定流速使用。紫外检测波长设定为270 nm。结果发现，该方法在II和III的浓度范围为0.56 - 28.0 μmol/l以及I的浓度范围为2.0 - 26.7 μmol/l时，重现性和准确性均合适。
