Department of Chemistry, Saurashtra University, Rajkot 360 005, Gujarat, India.
Saudi Pharm J. 2011 Jul;19(3):159-64. doi: 10.1016/j.jsps.2011.03.005. Epub 2011 Mar 21.
The objective of the current study was the development of a simple, precise and accurate isocratic reversed-phase stability indicating Ultra Performance Liquid Chromatography [UPLC] assay method and validated for determination of ticlopidine hydrochloride in solid pharmaceutical dosage forms. Isocratic separation was achieved on a Zorbax SB-C18 (50 mm × 4.6 mm, 1.8 μm) column using mobile phase of methanol-0.01 M ammonium acetate buffer, pH 5.0 (80:20, v/v) at a flow rate of 0.8 ml min(-1), the injection volume was 4.0 μl and the detection was carried out at 235 nm by using photo-diode array detector. The drug was subjected to oxidation, hydrolysis, photolysis and heat to apply stress condition. The method was validated for specificity, linearity, precision, accuracy, robustness and solution stability. The method was linear in the drug concentration range of 62.5-375 μg ml(-1) with a correlation coefficient of 0.9999. The precision (relative standard deviation - RSD) of six samples was 1.31% for repeatability and the intermediate precision [RSD] among six-sample preparation was 0.77%. The accuracy (recovery) was between 98.80% and 101.50%. Degradation products produced as a result of stress studies did not interfere with detection of ticlopidine hydrochloride and the assay can thus be considered stability indicating.
本研究的目的是开发一种简单、精确和准确的等度反相稳定性指示超高效液相色谱[UPLC]分析方法，并对其进行验证，以测定固体制剂中盐酸噻氯匹定的含量。等度分离在 Zorbax SB-C18（50mm×4.6mm，1.8μm）柱上实现，流动相为甲醇-0.01M 乙酸铵缓冲液，pH5.0（80:20，v/v），流速为 0.8ml/min，进样体积为 4.0μl，检测波长为 235nm，采用光电二极管阵列检测器。药物经氧化、水解、光解和热解处理，以施加应条件。该方法经过专属性、线性、精密度、准确度、耐用性和溶液稳定性验证。该方法在药物浓度范围为 62.5-375μg/ml 时具有线性，相关系数为 0.9999。六个样品的精密度（相对标准偏差-RSD）为 1.31%，重复性良好，六个样品制备的中间精密度[RSD]为 0.77%。准确度（回收率）在 98.80%和 101.50%之间。在应激研究中产生的降解产物不会干扰盐酸噻氯匹定的检测，因此可以认为该测定方法具有稳定性指示作用。
