Shukla Snehal K, Kadry Hossam, Bhatt Jayshil A, Elbatanony Rasha, Ahsan Fakhrul, Gupta Vivek
Department of Pharmaceutical Sciences, College of Pharmacy & Health Sciences, St. John's University, Queens, NY 11432, USA.
School of Pharmacy, Texas Tech University Health Sciences Center, 1300 S Coulter, Amarillo, TX 79106, USA.
Bioanalysis. 2020 Feb;12(3):159-174. doi: 10.4155/bio-2019-0284. Epub 2020 Feb 13.
A high throughput ultra-performance liquid chromatography (UPLC)-ultraviolet method for quantification of nintedanib in rat and human plasma was developed and optimized using chemometrical approach. Design of experiment and multivariate statistical approach was used for definition of optimized method. Final separation was performed using protein precipitation method on ACQUITY HSS T3 C18 column in isocratic mode using potassium phosphate buffer (pH 7.5): acetonitrile. Method was validated as per US-FDA guidelines linearly from 15-750 ng/ml. All quality control samples showed <15% relative standard deviation for precision and 85-115% accuracy along with >98% extraction recovery. The developed method is easily applicable in determining pharmacokinetic parameters in preclinical subjects along with successful implementation for quantification in human plasma samples.
采用化学计量学方法开发并优化了一种用于定量大鼠和人血浆中尼达尼布的高通量超高效液相色谱（UPLC）-紫外方法。实验设计和多变量统计方法用于确定优化方法。最终分离采用蛋白沉淀法，在ACQUITY HSS T3 C18柱上以等度模式使用磷酸钾缓冲液（pH 7.5）：乙腈进行。该方法按照美国食品药品监督管理局（US-FDA）指南进行验证，线性范围为15 - 750 ng/ml。所有质量控制样品的精密度相对标准偏差<15%，准确度为85 - 115%，提取回收率>98%。所开发的方法易于应用于确定临床前受试者的药代动力学参数，并成功用于人血浆样品的定量分析。
