Abstract:
A simple HPLC method was developed for the determination of antiplatelet drug ticagrelor (TCG) in blood. Sample preparation and extraction conditions were investigated and optimized. The preparation of blood plasma was investigated by protein precipitation using perchloric acid, methanol, acetonitrile (ACN), and trifluoroacetic acid. Protein precipitation using ACN was found to be the most suitable. Chromatographic separation of TCG was performed on a C18 column with a mobile phase consisting of ACN and 15 mM ammonium acetate buffered at pH 8.0. The method was applied to determine TCG in blood plasma of patients who had a heart attack. Blood samples were collected 1.5 h after the administration of the initial loading dose of the antiplatelet drug. The average concentration of TCG was found to be 0.97 ± 0.53 μg/ml. The developed method proved to be very selective, without interferences from other endogenous substances and the influences of possible coadministered drugs. The limits of detection and quantification estimated by the signal-to-noise ratio in real samples were 0.24 and 0.4 μg/ml, respectively. The developed method is simple and can be easily applied in clinics and emergency cardiac situations after the initial loading dose of TCG in the first few hours of a heart attack.
摘要:
已开发出一种简单的HPLC法测定血液中抗血小板药物替格瑞洛的方法。研究并优化了样品制备和提取条件。通过使用高氯酸的蛋白质沉淀法研究了血浆的制备,甲醇,乙腈和三氟乙酸。发现用乙腈沉淀蛋白质是最合适的。替格瑞洛的色谱分离在C18柱上进行,流动相由乙腈和在pH8.0缓冲的15mM乙酸铵组成。该方法用于测定心脏病发作患者血浆中的替格瑞洛。在施用初始负荷剂量的抗血小板药物后1.5小时收集血样。替格瑞洛的平均浓度为0.97±0.53μg/mL。开发的方法被证明是非常有选择性的,没有其他内源性物质的干扰和可能的共同给药的影响。实际样品中通过信噪比估计的检测限和定量限分别为0.24μg/mL和0.4μg/mL。所开发的方法简单,在心脏病发作的最初几个小时内服用初始负荷剂量的替格瑞洛后,可以轻松地应用于临床状况和紧急心脏情况。