Croitoru Octavian, Spiridon Adela-Maria, Belu Ionela, Turcu-Ştiolică Adina, Neamţu Johny
Faculty of Pharmacy, Department I of Pharmacy, University of Medicine and Pharmacy, Petru Rares Street, 200349 Craiova, Romania.
Faculty of Pharmacy, Doctoral School, University of Medicine and Pharmacy, Petru Rares Street, 200349 Craiova, Romania.
J Anal Methods Chem. 2015;2015:892470. doi: 10.1155/2015/892470. Epub 2015 Dec 29.
A simple, sensitive, and specific reversed phase liquid chromatographic method was developed and validated for simultaneous quantification of clopidogrel, its carboxylic acid metabolite, and atorvastatin in human serum. Plasma samples were deproteinized with acetonitrile and ibuprofen was chosen as internal standard. Chromatographic separation was performed on an BDS Hypersil C18 column (250 × 4.6 mm; 5 μm) via gradient elution with mobile phase consisting of 10 mM phosphoric acid (sodium) buffer solution (pH = 2.6 adjusted with 85% orthophosphoric acid) : acetonitrile : methanol with flow rate of 1 mL·min(-1). Detection was achieved with PDA detector at 220 nm. The method was validated in terms of linearity, sensitivity, precision, accuracy, limit of quantification, and stability tests. Calibration curves of the analytes were found to be linear in the range of 0.008-2 μg·mL(-1) for clopidogrel, 0.01-4 μg·mL(-1) for its carboxylic acid metabolite, and 0.005-2.5 μg·mL(-1) for atorvastatin. The results of accuracy (as recovery) with ibuprofen as internal standard were in the range of 96-98% for clopidogrel, 94-98% for its carboxylic acid metabolite, and 90-99% for atorvastatin, respectively.
建立了一种简单、灵敏且特异的反相液相色谱法，并对其进行了验证，用于同时定量测定人血清中的氯吡格雷、其羧酸代谢物和阿托伐他汀。血浆样品用乙腈进行脱蛋白处理，并选用布洛芬作为内标。色谱分离在BDS Hypersil C18柱（250×4.6 mm；5 μm）上进行，采用梯度洗脱，流动相由10 mM磷酸（钠）缓冲溶液（用85%正磷酸调节pH = 2.6）：乙腈：甲醇组成，流速为1 mL·min(-1)。使用PDA检测器在220 nm波长处进行检测。该方法在线性、灵敏度、精密度、准确度、定量限和稳定性测试等方面进行了验证。发现各分析物的校准曲线在氯吡格雷0.008 - 2 μg·mL(-1)、其羧酸代谢物0.01 - 4 μg·mL(-1)、阿托伐他汀0.005 - 2.5 μg·mL(-1)范围内呈线性。以布洛芬作为内标时，氯吡格雷、其羧酸代谢物和阿托伐他汀的准确度（以回收率表示）结果分别在96 - 98%、94 - 98%和90 - 99%范围内。
