Saini P K, Jain C L, Singh R M, Mathur S C, Singh G N
Research and Development Division, Indian Pharmacopoeia Commission, Sector-23, Rajnagar Ghaziabad-201 001, India.
Indian J Pharm Sci. 2010 Jul;72(4):494-7. doi: 10.4103/0250-474X.73925.
A simple, very fast, precise and accurate reverse phase ultra performance liquid chromatographic method was developed for the determination and validation of topotecan hydrochloride in bulk and injection dosage form. A Waters BEH C18, 50×2.1 mm, 1.7 μm particle size column in gradient mode was used with mobile phase comprising of 0.1% v/v orthophosphoric acid in water and acetonitrile. The analytical column was thermostated at 50° and flow rate was set at 0.4 ml per min, with photo diode array detection at 260 nm. The retention time of topotecan was found 1.38 min. The method was validated in terms of linearity, accuracy, precision and specificity. The calibration curve was found linear between 20 to 60 μg/ml. The limit of detection and limit of quantification were found 0.2353 and 0.7131 μg/ml, respectively. Percentage recoveries were obtained in the range of 98.91% and 99.17%. The proposed method is precise, accurate, selective and reproducible. The ultra performance liquid chromatographic assay procedure, which proved superior because of its greater sensitivity and relatively shorter (4 min) run time, should be an important tool for speedy future analysis of topotecan hydrochloride in bulk and its injection dosage form.
建立了一种简单、快速、精确且准确的反相超高效液相色谱法，用于测定和验证原料药及注射剂剂型中的盐酸拓扑替康。采用Waters BEH C18柱（50×2.1 mm，粒径1.7μm），以梯度模式运行，流动相由0.1%（v/v）的磷酸水溶液和乙腈组成。分析柱温度设定为50℃，流速设定为每分钟0.4 ml，采用光电二极管阵列检测器，检测波长为260 nm。测得盐酸拓扑替康的保留时间为1.38分钟。该方法在线性、准确度、精密度和特异性方面均得到验证。校准曲线在20至60μg/ml范围内呈线性。检测限和定量限分别为0.2353和0.7131μg/ml。回收率在98.91%至99.17%之间。所提出的方法精确、准确、具有选择性且可重现。超高效液相色谱测定法因其更高的灵敏度和相对较短（4分钟）的运行时间而表现出色，应成为未来快速分析盐酸拓扑替康原料药及其注射剂剂型的重要工具。
