Chiap P, Ceccato A, Miralles Buraglia B, Boulanger B, Hubert P, Crommen J
Department of Analytical Pharmaceutical Chemistry, Institute of Pharmacy, University of Liège, CHU, B36, B-4000 Liège 1, Belgium.
J Pharm Biomed Anal. 2001 Mar;24(5-6):801-14. doi: 10.1016/s0731-7085(00)00547-1.
A fully automated method for the determination of sotalol in human plasma was developed, involving dialysis through a cellulose acetate membrane, clean-up and enrichment of the dialysate on a strong cation-exchange pre-column and subsequent liquid chromatographic (LC) analysis with UV detection. All sample handling operations were carried out by means of an ASTED system. Before starting dialysis, the trace enrichment column (TEC) was conditioned. The plasma sample, to which the internal standard (atenolol) was automatically added, was then loaded in the donor channel and was kept static while the dialysis liquid, consisting of 0.017 M acetic acid, was passed through the acceptor channel in successive pulses. After each pulse, the dialysate was dispensed onto the TEC. When dialysis was discontinued, the analytes were eluted from the TEC by the LC mobile phase by rotation of a switching valve and transferred to the analytical column packed with octyl silica. The LC mobile phase was a mixture of methanol and pH 7.0 phosphate buffer containing 1-octanesulfonate at a concentration of 7.5 x 10(-4) M (19:81; v/v). The UV detection was performed at 230 nm. The influence of several parameters of the dialysis and trace enrichment processes on analyte recovery and method selectivity was investigated. The method was then validated. The mean absolute recovery for sotalol was about 60%. The limit of quantitation was 25 ng/ml and R.S.D. for repeatability and intermediate precision obtained at a concentration level of 50 ng/ml were 4.3 and 5.8%, respectively.
建立了一种全自动测定人血浆中索他洛尔的方法，该方法包括通过醋酸纤维素膜进行透析、在强阳离子交换预柱上对透析液进行净化和富集，以及随后采用紫外检测的液相色谱（LC）分析。所有样品处理操作均通过ASTED系统进行。在开始透析前，对微量富集柱（TEC）进行预处理。然后将自动加入内标（阿替洛尔）的血浆样品加载到供体通道中，并保持静止，同时由0.017 M醋酸组成的透析液以连续脉冲的方式通过受体通道。每次脉冲后，将透析液分配到TEC上。透析停止后，通过切换阀的旋转，用LC流动相将分析物从TEC上洗脱下来，并转移到填充有辛基硅胶的分析柱上。LC流动相是甲醇和pH 7.0的磷酸盐缓冲液的混合物，其中含有浓度为7.5×10(-4) M的1-辛烷磺酸盐（19:81；v/v）。在230 nm处进行紫外检测。研究了透析和微量富集过程的几个参数对分析物回收率和方法选择性的影响。然后对该方法进行了验证。索他洛尔的平均绝对回收率约为60%。定量限为25 ng/ml，在50 ng/ml浓度水平下获得的重复性和中间精密度的相对标准偏差分别为4.3%和5.8%。
