Mitakos A, Panderi I
School of Pharmacy, Division of Pharmaceutical Chemistry, University of Athens, Panepistimiopolis, Zografou, 157 71, Athens, Greece.
J Pharm Biomed Anal. 2002 May 15;28(3-4):431-8. doi: 10.1016/s0731-7085(01)00620-3.
A stability indicating, reversed-phase high-performance liquid chromatographic method was developed and validated for the determination of clopidogrel in pharmaceutical dosage forms. The determination was performed on a semi-micro column, BDS C8 (250 x 2.1 mm i.d., 5 microm particle size); the mobile phase consisted of a mixture of 0.010 M sodium dihydrogen phosphate (pH 3.0) and acetonitrile (35:65, v/v), pumped at a flow rate 0.30 ml min(-1). The UV detector was operated at 235 nm. The retention times for clopidogrel and naproxen, which was used as internal standard, were 3.08 and 6.28 min, respectively. Calibration graphs are linear (r better than 0.9991, n=6), in concentration range 1.00-3.00 microg ml(-1) for clopidogrel. The intra- and inter-day RSD values were less than 1.96%, while the relative percentage error E(r) was less than 2.0% (n=5). Detection and quantitation limits were 0.12 and 0.39 micro ml(-1), respectively. The method was applied in the quality control of commercial tablets and content uniformity test and proved to be suitable for rapid and reliable quality control.
建立了一种用于测定药物剂型中氯吡格雷的稳定性指示反相高效液相色谱法并进行了验证。测定在半微柱BDS C8（内径250×2.1mm，粒径5μm）上进行；流动相由0.010M磷酸二氢钠（pH 3.0）和乙腈（35:65，v/v）的混合物组成，以0.30ml min⁻¹的流速泵送。紫外检测器在235nm波长下运行。氯吡格雷和用作内标的萘普生的保留时间分别为3.08分钟和6.28分钟。校准曲线在氯吡格雷浓度范围1.00 - 3.00μg ml⁻¹内呈线性（r优于0.9991，n = 6）。日内和日间相对标准偏差值小于1.96%，而相对百分比误差E(r)小于2.0%（n = 5）。检测限和定量限分别为0.12和0.39μg ml⁻¹。该方法应用于市售片剂的质量控制和含量均匀度测试，证明适用于快速可靠的质量控制。
