Ji Shengnan, Liu Xiaomeng, Ha Jing, Ai Lianfeng, Li Zheng
College of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, 050018 Shijiazhuang, China.
Shijiazhuang Customs Technology Center, 050051 Shijiazhuang, China; College of Public Health, Hebei Medical University, 050017 Shijiazhuang, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2023 Apr 15;1221:123680. doi: 10.1016/j.jchromb.2023.123680. Epub 2023 Mar 20.
A sensitive and simple method was developed to determine orelabrutinib in human plasma and cerebrospinal fluid by liquid chromatography tandem mass spectrometry (LC-MS/MS). The samples were prepared by simple protein precipitation with by 0.1% formic acid acetonitrile solution and efficient separations were performed on the Thermo Hypersll GOLD C18 column (2.1 mm × 150 mm, 5 μm) under a gradient program in a total run time of 9 min. The orelabrutinib was detected by electrospray ionization in positive ion mode with selective reaction monitoring (SRM) and mass spectrometric conditions were optimized in order to increase selectivity and sensitivity. The developed method was validated in terms of its accuracy, precision, selectivity, linearity, recovery, matrix effect, stability, and limits of quantification (LOQ). The lower limit of quantification is 0.50 ng/mL, the intraday and interday precision RSD are both less than 15%, and the recovery rate is 85.7%-92.9%. Finally, the method was successfully applied for the quantitation of orelabrutinib in human plasma and cerebrospinal fluid of clinical patients treated with orelabrutinib.
建立了一种灵敏且简便的液相色谱串联质谱法（LC-MS/MS）测定人血浆和脑脊液中的奥雷巴替尼。样品采用0.1%甲酸乙腈溶液进行简单的蛋白沉淀法制备，并在Thermo Hypersll GOLD C18柱（2.1 mm×150 mm，5μm）上按照梯度程序进行高效分离，总运行时间为9分钟。奥雷巴替尼采用电喷雾电离正离子模式下的选择性反应监测（SRM）进行检测，并对质谱条件进行了优化以提高选择性和灵敏度。所建立的方法在准确性、精密度、选择性、线性、回收率、基质效应、稳定性和定量限（LOQ）方面进行了验证。定量下限为0.50 ng/mL，日内和日间精密度RSD均小于15%，回收率为85.7%-92.9%。最后，该方法成功应用于接受奥雷巴替尼治疗的临床患者人血浆和脑脊液中奥雷巴替尼的定量分析。
