摘要
目的建立HPLC-MS的方法测定大鼠血浆中白杨素含量。方法以柚皮素为内标;采用Waters Xtera C18色谱柱(150 mm×4.6 mm,5μm)分离,柱温设定为30℃;梯度洗脱:A相为乙腈,B相为0.05%甲酸;流速为0.8 ml·min-1,使用分流器将0.2 ml·min-1的洗脱液注入离子源;选择离子监测检测(SIM):白杨素m/z 255[M+H]+,内标柚皮素m/z 273[M+H]+。结果本研究所采用的方法检测限为1.5 ng·ml-1,定量限为4.0 ng·ml-1,且精密度、稳定性及回收率满足测定要求,并成功用于白杨素在大鼠体内的药动学评价。结论本研究建立了快速、准确的HPLC-MS法用于测定大鼠血浆中的白杨素含量,并成功拟合其药动学参数,白杨素在大鼠体内的药动学特性符合二室开放模型含量。
Objective To establish an HPLC-MS method to analyze the concentration of chrysin in rat plas- ma. Methods Naringenin was used as the internal standard. The separations was performed on a Waters Xtera C18 column （150 mm ×4.6 ram,5 μm）. The column temperature was set at 30 ℃ ;the mobile phase was composed of acetonitrile （A） and 0.05 % formic acid solution. A linear gradient elution was used, and the flow rate was 0.8 ml · min-1.0.2 ml·min-1 elution buffer was transferred into the ion source by a solvent splitter,the ion monitor mode was chosen and the selected ions were m/z 255 [ M ＋ H ] ＋for chrysin and m/z 273 [ M ＋ H ] ＋ for naringenin. Re- sults The limit of detection （LOD） and limit of quantitation （LOQ） were 1.5 and 4.0 ng·m1-1 respectively,with satisfactory precision, stability and recovery. This method was also applied to evaluate the Pharmacokinetics profile of chrysin. Conclusion A quick and accurate HPLC-MS method has been established to analyze the concentration of chrysin in rat plasma. Pharmacokinetics parameters are estimated accurately, and the data are fitted to a two-com- partment model with first-order absorption.
出处
《解放军药学学报》
CAS
2014年第1期37-39,51,共4页
Pharmaceutical Journal of Chinese People's Liberation Army
