Russel F G, van Uum S, Tan Y, Smits P
Department of Pharmacology 233, Faculty of Medical Sciences, University of Nijmegen, The Netherlands.
J Chromatogr B Biomed Sci Appl. 1998 Jun 12;710(1-2):223-6. doi: 10.1016/s0378-4347(98)00141-8.
A new method is described for the solid-phase extraction of 18beta-glycyrrhetinic acid from plasma or serum, with subsequent analysis by HPLC. New aspects of the method include the use of commercially available 18alpha-glycyrrhetinic acid as the internal standard and the use of a Bond Elut C2 (ethyl) extraction column, to avoid the need to use large volumes of organic solvent to elute the isolates from the columns. Separation was achieved on a Shandon Hypersil BDS C18 analytical column, with a mobile phase consisting of acetonitrile-0.02 M phosphate buffer, pH 5.7 (55:45, v/v). The column effluent was monitored at 248 nm. Compared with previous methods, the procedure is much easier to carry out, whereas the sensitivity (limit of detection, 10 ng/ml, and limit of quantitation, 50 ng/ml), the precision (0.3-6.2%) and the accuracy (97.2-101.9%) are of the same order of magnitude.
本文描述了一种从血浆或血清中固相萃取18β-甘草次酸的新方法,随后通过高效液相色谱法进行分析。该方法的新特点包括使用市售的18α-甘草次酸作为内标,以及使用Bond Elut C2(乙基)萃取柱,从而避免了使用大量有机溶剂从柱上洗脱分离物的需要。在Shandon Hypersil BDS C18分析柱上实现分离,流动相由乙腈-0.02 M磷酸盐缓冲液(pH 5.7,55:45,v/v)组成。在248 nm处监测柱流出物。与以前的方法相比,该程序更易于实施,而灵敏度(检测限为10 ng/ml,定量限为50 ng/ml)、精密度(0.3 - 6.2%)和准确度(97.2 - 101.9%)处于相同的数量级。