■Nintedanib(NTB)是一种多种酪氨酸激酶抑制剂,被调查了许多疾病,如特发性肺纤维化(IPF),系统性硬化症间质性肺病(SSc-ILD)和非小细胞肺癌(NSCLC)。NTB可作为口服胶囊配方,但是它能够检测通过氧化形成的降解物,光解和水解过程使其难以量化。在目前的工作中,开发并验证了一种新的反相高效液相色谱(RP-HPLC)方法。
■开发的方法很简单,精确,可重复,稳定和准确。使用提出的分析方法方法评估了NTB的固有稳定性,并进行了力降解研究。NTB在ShimadzuC18色谱柱上作为固定相(250×4.6mm,5µm)使用等度洗脱方法,在HPLC级水和乙腈(ACN)中使用0.1%v/v的三乙胺(TEA),比例为35:65%v/v。流动相以1.0ml/min的恒定流速泵送,洗脱剂在390nm波长处检测。
■NTB在保留时间(tR)为6.77±0.00min时洗脱,相关系数为0.999,所开发的方法在0.5µg/ml至4.5µg/ml的浓度范围内呈线性。发现对于1.5µg/ml浓度,回收率在99.391±0.468%的范围内。六个重复标准品被确定为具有0.04的%RSD。
■配方辅料不会干扰NTB的测定,证明了所开发方法的特异性。所开发的分析方法的建议方法可用于量化原料药和药物制剂中存在的NTB的量。
UNASSIGNED: Nintedanib (NTB) is a multiple tyrosine kinase inhibitor, been investigated for many disease conditions like idiopathic pulmonary fibrosis (IPF), systemic sclerosis interstitial lung disease (SSc-ILD) and non-small cell lung cancer (NSCLC). NTB is available as oral capsule formulation, but its ability to detect degradants formed through oxidative, photolytic and hydrolytic processes makes it difficult to quantify. In the current work, a novel reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated.
UNASSIGNED: The developed method is simple, precise, reproducible, stable and accurate. The inherent stability of NTB was evaluated using the proposed analytical method approach and force degradation studies were carried out. NTB was separated chromatographically on the Shimadzu C 18 column as stationary phase (250 ×4.6 mm, 5 µm) using an isocratic elution method with 0.1% v/v triethyl amine (TEA) in HPLC grade water and acetonitrile (ACN) in the ratio 35:65% v/v. The mobile phase was pumped at a constant flow rate of 1.0 ml/min, and the eluent was detected at 390 nm wavelength.
UNASSIGNED: NTB was eluted at 6.77±0.00 min of retention time (t R) with a correlation coefficient of 0.999, the developed method was linear in the concentration range of 0.5 µg/ml to 4.5 µg/ml. The recovery rate was found to be in the range of 99.391±0.468% for 1.5 µg/ml concentration. Six replicate standards were determined to have an % RSD of 0.04.
UNASSIGNED: The formulation excipients didn\'t interfere with the determination of NTB, demonstrating the specificity of the developed method. The proposed approach of the analytical method developed can be used to quantify the amount of NTB present in bulk drugs and pharmaceutical formulations.