Kumar Rajinish, Suresh P S, Rudresh G, Zainuddin Mohd, Dewang Purushottam, Kethiri Ragahava Reddy, Rajagopal Sriram, Mullangi Ramesh
Jubilant Biosys Ltd., Industrial Suburb, Yeshwanthpur, Bangalore 560 022, India.
Medicinal Chemistry, Jubilant Biosys Ltd., Industrial Suburb, Yeshwanthpur, Bangalore 560 022, India.
J Pharm Biomed Anal. 2016 Jun 5;125:140-4. doi: 10.1016/j.jpba.2016.03.036. Epub 2016 Mar 17.
A sensitive, specific and rapid LC-ESI-MS/MS method has been developed and validated for the quantification of ulixertinib in mice plasma using phenacetin as an internal standard (I.S.) as per regulatory guidelines. Sample preparation was accomplished through a protein precipitation procedure with acetonitrile:methanol mixture. Chromatographic separation was performed on Atlantis dC18 column using a binary gradient using mobile phase A (0.2% formic acid in water) and B (acetonitrile) at a flow rate of 0.60mL/min. Elution of ulixertinib and I.S. occurred at ∼1.07 and 1.20min, respectively. The total chromatographic run time was 2.5min. A linear response function was established in the concentration range of 1.58-2054ng/mL. The intra- and inter-day accuracy and precisions were in the range of 2.11-11.8 and 5.80-11.4%, respectively. This novel method has been applied to a pharmacokinetic study in mice.
根据监管指南，已开发并验证了一种灵敏、特异且快速的液相色谱-电喷雾串联质谱（LC-ESI-MS/MS）方法，用于以非那西丁作为内标（I.S.）对小鼠血浆中的乌利西替尼进行定量分析。样品制备通过用乙腈：甲醇混合物进行蛋白沉淀程序来完成。色谱分离在Atlantis dC18柱上进行，使用二元梯度，流动相A（0.2%甲酸水溶液）和B（乙腈），流速为0.60mL/min。乌利西替尼和内标的洗脱时间分别约为1.07分钟和1.20分钟。总色谱运行时间为2.5分钟。在1.58 - 2054ng/mL的浓度范围内建立了线性响应函数。日内和日间准确度及精密度分别在2.11 - 11.8%和5.80 - 11.4%的范围内。这种新方法已应用于小鼠的药代动力学研究。
