Saadat Ebrahim, Dehghan Kelishady Pooya, Ravar Fatemeh, Kobarfard Farzad, Dorkoosh Farid A
Department of Pharmaceutics, Faculty of Pharmacy, Tehran University of Medical Sciences, P.O. Box 14155-645, Tehran, Iran.
Department of Medicinal Chemistry, School of Pharmacy, Shahid Beheshtee University of Medical Sciences, Tehran, Iran.
J Chromatogr Sci. 2015 Jul;53(6):932-9. doi: 10.1093/chromsci/bmu150. Epub 2014 Dec 9.
A rapid, simple and stability-indicating high-performance liquid chromatography assay method was developed and validated for quantitative analysis of lapatinib (LPT) in bulk pharmaceuticals. The newly developed method was assessed using a C18 MZ-Analytical column (5 µm, 150 × 4.6 mm, OSD-3), which was protected by a (5 µm, 4.0 × 4.6 mm, OSD-3) pre-column with mobile phase that was composed of acetonitrile and water (70/30, v/v) and a detection wave length of 227 nm. The method was validated according to the ICH guidelines with respect to precision, accuracy, linearity, robustness, specificity and system suitability. Forced degradation studies were also performed for LPT to determine the stability-indicating aspect of developed method. The method was found to be specific for LPT in the presence of degradation products. The retention time of LPT was ∼4 min. Accuracy of the method was found to be 2.20% bias for all tested samples. The inter- and intra-day precision of the novel method were found to be 2.84 and 2.78%, respectively. The calibration curve was linear over the concentration range of 5-80 µg/mL with a regression coefficient of 0.9990. The limits of detection and quantification were also found to be 1 and 5 µg/mL, respectively. Mass spectrometry analysis was performed in order to better characterize degraded products.
建立并验证了一种快速、简单且具有稳定性指示功能的高效液相色谱分析方法，用于原料药中拉帕替尼（LPT）的定量分析。使用C18 MZ - Analytical色谱柱（5 µm，150×4.6 mm，OSD - 3）对新开发的方法进行评估，该色谱柱由（5 µm，4.0×4.6 mm，OSD - 3）保护柱保护，流动相由乙腈和水（70/30，v/v）组成，检测波长为227 nm。根据ICH指南，对该方法的精密度、准确度、线性、稳健性、特异性和系统适用性进行了验证。还对LPT进行了强制降解研究，以确定所开发方法的稳定性指示方面。结果发现该方法在存在降解产物的情况下对LPT具有特异性。LPT的保留时间约为4分钟。所有测试样品的方法准确度偏差为2.20%。新方法的日间和日内精密度分别为2.84%和2.78%。校准曲线在5 - 80 µg/mL的浓度范围内呈线性，回归系数为0.9990。检测限和定量限分别为1和5 µg/mL。进行了质谱分析以更好地表征降解产物。
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