高效液相色谱法测定小鼠肝组织中两种甲氧基补骨脂素  

Determination of two kinds of methoxypsoralen in mouseliver tissue by high performance liquid chromatography

作　　者：吴天伟[1] 崔蓉[1] 张宝旭[1] WU Tian-wei CUI Rong ZHANG Bao-xu(School of Public Health, Peking University, Beijing 100191)

机构地区：[1]北京大学公共卫生学院,北京100191

出　　处：《分析试验室》2017年第10期1215-1218,共4页Chinese Journal of Analysis Laboratory

摘　　要：建立小鼠肝组织中8-甲氧基补骨脂素(8-MOP)与5-甲氧基补骨脂素(5-MOP)的高效液相色谱测定方法。采用正交试验设计对样品的前处理方法进行优化,Waters Symmetry C_(18)柱(250 mm×4.6 mm,5μm)分离,流动相为甲醇-水(55:45,V/V),流速为1.0 m L/min,荧光检测器激发与发射波长分别为334 nm与484 nm。小鼠肝组织中8-MOP与5-MOP在0.10~25μg/m L范围内线性良好,r值分别为0.9998与0.9994;8-MOP与5-MOP的定量限分别为4.0 ng/g和1.0 ng/g;8-MOP与5-MOP的加标回收率分别为101.1%~102.0%与94.2%~103.2%;提取回收率分别为96.6%~98.6%与92.6%~98.4%;基质效应分别为95.6%~98.2%与91.4%~99.6%;日内精密度分别为2.7%~3.3%与5.2%~5.5%;日间精密度分别为1.4%~2.4%与0.3%~1.6%。给药后小鼠肝组织中8-MOP含量为23.1~48.7 ng/g。方法适用于小鼠肝组织中8-MOP与5-MOP的同时测定。A method for the determination of 8-methoxypsoralen （8-MOP） and 5-methoxypsoralen （5- MOP） in mouse liver tissue using high performance liquid chromatography was developed. Orthogonal experiment design was applied for the optimization of sample preparation conditions. 8-MOP and 5- MOP were separated on a Waters Symmetry Cls column （250 mm x 4. 6 mm, 5 p^m ）. The mobile phase consisted of methanol-water （55：45, V/V） at a flow rate of 1.0 mL/min, and the excitation and emission wavelengths of fluorescence detector were set at 334 nm and 484 nm respectively. The calibration curves were linear with correlation coefficients of 0. 9998 for 8-MOP and 0. 9994 for 5-MOP over the concentration range of 0. 10- 25 μg/mL. The limits of quantitation were 4. 0 ng/g for 8-MOP, and 1.0 ng/g for 5-MOP, respectively. The recoveries of 8-MOP and 5-MOP ranged from 101.1% to 102. 0% and from 94. 2% to 103.2% , respectively. The extraction recoveries of 8-MOP and 5-MOP were 96.6% ~ 98.6% and 92. 6% - 98.4%, respectively. And the matrix effects were 95.6% -98.2% for 8-MOP, and 91.4% ~ 99.6% for 5-MOP. The intra-day precisions of 8-MOP and 5-MOP was 2.7% -3.3% and 5.2% -5.5% , respectively, while the inter-day precisions were 1.4% - 2. 4% and 0. 3% - 1. 6%, respectively. The contents of 8-MOP in mice liver after administration were from 23. 1 to 48.7 ng/g. This method was suitable for simultaneous determination of 8-MOP and 5-MOP in mouse liver tissue.

关 键 词：高效液相色谱 8-甲氧基补骨脂素 5-甲氧基补骨脂素 小鼠 肝组织 

分 类 号：R917[医药卫生—药物分析学]