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目的建立检测大鼠全血中ASC-J9的高效液相色谱-质谱联用(HPLC-MS/MS)。方法方法全血样本经液液萃取提取分离,色谱柱为Symmetry C18(4.6 mm×150 mm,5μm),流动相为纯水(含0.1%甲酸和10 mmol·L-1甲酸铵)-乙腈,流速为1.0 m L·min-1,质谱分流0.4 m L·min-1,柱温35℃,大气压电喷雾离子源(ESI),正离子模式多重反应选择离子检测(MRM)。结果 ASC-J9线性范围为3.54~1 180 ng·m L-1,提取回收率在83.19%~87.27%,日内、日间RSD均小于8.89%。结论本方法专属性强,灵敏度高,适用于ASC-J9药动学研究。
Objective To establish a high performance liquid chromatography-mass spectrometry (HPLC-MS / MS) system for the detection of ASC-J9 in rat whole blood. Methods Blood samples were separated by liquid-liquid extraction. The chromatographic column was Symmetry C18 (4.6 mm × 150 mm, 5 μm). The mobile phase consisted of pure water (containing 0.1% formic acid and 10 mmol·L -1 ammonium formate) The flow rate was 1.0 m L · min-1, mass spectrometry split 0.4 m L · min-1, column temperature 35 ℃, atmospheric pressure electrospray ionization (ESI) and positive ion mode multiple reaction selective ion detection (MRM). Results The linear range of ASC-J9 was 3.54-1 180 ng · m L-1. The recoveries ranged from 83.19% to 87.27%. The intra-day and inter-day RSD were less than 8.89%. Conclusion The method is highly specific and sensitive, suitable for ASC-J9 pharmacokinetic studies.