摘要
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 an HPLC-MS / MS method for determination of ASC-J9 in rat blood. METHODS After liquid-liquid extraction,ASC-J9 was separated on a Symmetry C18 colume,with mobile phase of acetonitrile-water containing 0. 1% formic acid and 10 mmol·L- 1ammonium formate. The flow rate was 1. 0 m L·min- 1,mass shunt was 0. 4 m L·min- 1,and column temperature was main tained at 35 ℃. Quantification was performed in positive ion multiple-reaction-monitoring（ MRM） mode. RESULTS The calibration curve of ASC-J9 had good linearity in the concentration range of 3. 54- 1 180 ng·m L- 1. The extraction recovery rate was within 83. 19% to 87. 27%,and the intra-day and inter-day RSDs were both less than 8. 89%. CONCLUSION This method is specific,sensitive and suitable for determination of ASC-J9 in rat blood.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2015年第22期1996-1999,共4页
Chinese Pharmaceutical Journal
