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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。
To establish a method for the determination of 8-methoxy psoralen (8-MOP) and 5-methoxy psoralen (5-MOP) in mouse liver tissue by high performance liquid chromatography. The orthogonal experimental design was used to optimize the sample pretreatment. The separation was performed on a Waters Symmetry C_ (18) column (250 mm × 4.6 mm, 5 μm) using methanol-water (55:45, V / V) 1.0 m L / min. Fluorescence detector excitation and emission wavelengths were 334 nm and 484 nm, respectively. The linearity of 8-MOP and 5-MOP was found in the range of 0.10 ~ 25μg / mL in mouse liver with r values of 0.9998 and 0.9994, respectively. The limits of quantitation of 8-MOP and 5-MOP were 4.0 ng / g and 1.0 The recoveries of 8-MOP and 5-MOP were 101.1% ~ 102.0% and 94.2% ~ 103.2%, respectively. The recoveries were 96.6% ~ 98.6% and 92.6% ~ 98.4%, respectively. Were 95.6% -98.2% and 91.4% -99.6% respectively. The intra-day precision was 2.7% -3.3% and 5.2% -5.5%, respectively. The intra-day precision was 1.4% -2.4% and 0.3% -1.6%, respectively. The 8-MOP content in liver tissue of mice after administration was 23.1-48.7 ng / g. The method is suitable for the simultaneous determination of 8-MOP and 5-MOP in mouse liver tissue.