Leite Fátima da Silva, Pereira Valéria Adriana, Omosako Célia Etsuco, Carmona Maria José Carvalho, Auler José Otávio Costa, Santos Silvia Regina Cavani Jorge
School of Pharmaceutical Sciences University of Sao Paulo, São Paulo, Brazil.
Ther Drug Monit. 2006 Apr;28(2):237-44. doi: 10.1097/01.ftd.0000198647.39751.f5.
A simple, rapid, selective, and sensitive analytical method was developed for the quantification of atenolol in small volumes of plasma, by high-performance liquid chromatography with fluorescence detection. Only 200 microL of plasma was used for chromatographic analysis. Separation was performed on a C18 reverse-phase column (4 microm) using a binary mobile phase consisting of 0.05 M of phosphate buffer, pH 5.5, and methanol (80:20, vol/vol) at a flow rate of 0.7 mL/minute. The retention times of atenolol and of the internal standard (sotalol) were 12.7 and 10.4 minutes, respectively. Validation of this analytical method showed a good linear correlation (8-2000 ng/mL), high sensitivity (quantification limit: 8 ng/ml and detection limit: 4 ng/mL), accuracy of 99.3%, and intraday and interday precision of 5.3% and 6.9%, respectively. Absolute recovery was 93.7%. The method was found to be robust, with acceptable stability. The analytical method was validated by the quantification of atenolol in plasma obtained from 2 patients with unstable angina, scheduled for myocardium revascularization surgery, who were chronically treated with 50 mg of atenolol administered per os once a day. The method developed was found to be adequate for use in pharmacokinetic studies and in adjusted dose pharmacotherapy.
建立了一种简单、快速、选择性好且灵敏的分析方法,用于通过高效液相色谱-荧光检测法定量测定少量血浆中的阿替洛尔。仅200微升血浆用于色谱分析。在C18反相柱(4微米)上进行分离,使用由0.05 M磷酸盐缓冲液(pH 5.5)和甲醇(80:20,体积/体积)组成的二元流动相,流速为0.7毫升/分钟。阿替洛尔和内标(索他洛尔)的保留时间分别为12.7分钟和10.4分钟。该分析方法的验证表明具有良好的线性相关性(8 - 2000纳克/毫升)、高灵敏度(定量限:8纳克/毫升,检测限:4纳克/毫升)、准确度为99.3%,日内和日间精密度分别为5.3%和6.9%。绝对回收率为93.7%。该方法被发现具有稳健性和可接受的稳定性。通过对2例不稳定型心绞痛患者血浆中的阿替洛尔进行定量验证了该分析方法,这2例患者计划进行心肌血运重建手术,长期口服每日一次50毫克阿替洛尔进行治疗。所建立的方法被发现适用于药代动力学研究和调整剂量的药物治疗。