摘要
目的建立测定裸鼠肝组织中6'-羟基爵床定A浓度的LC-MS/MS法,并用于裸鼠的组织分布研究。方法色谱柱为Agilent Zorbax SB-C18柱;流动相为水(含0.1%甲酸)-乙腈(含0.1%甲酸),梯度洗脱,流速0.5 ml.min-1,柱温为室温。采用ESI源,以多反应监测方式分别监测离子对m/z 410.8→136.9(6'-羟基爵床定A)和m/z 386.1→122.0(内标丁螺环酮)。肝组织匀浆后采用蛋白沉淀法进行预处理。结果 6'-羟基爵床定A在裸鼠肝组织中的线性范围为1.0～2000ng.ml-1,日内精密度RSD小于8.61%;日间精密度RSD小于8.15%,回收率在89.3%～98.3%范围内。结论该方法简单、灵敏、准确,适用于裸鼠肝组织中6'-羟基爵床定A的浓度测定及其组织分布研究。
Objective To develop an LC-MS/MS method for the determination of 6＇-Hydroxy Justicidin A in the liver of Nu/Nu mice. Method An Agilent Zorbax SB-C18 column （50 mm x 2.1 ram,3.5 μm） was used with water （0.1% formic acid）-acetonitrile （0.1% formic acid） as the mobile phase at a flow rate of 0.5 ml ·min-1 The column temperature was set at room temperature LC-MS/MS was performed in the multiple reaction monito- ring mode using target ions at m/z 410.8→136.9 （6＇-Hydroxy Justicidin A） and m/z 386.1→122.0 （ Buspirone, IS）. The Nu/Nu mice liver homogenates were treated using protein precipitation method. Result The calibration curve of 6＇-hydroxy justicidin A was linear within the range of 1.0-2000 ng ·ml^-1 in liver homogenates. Inter-day RSD was less than 8.15% and intra-day RSD was less than 8.61%. The recovery was calculated to be 89.3%- 98.3% in the liver. Conclusion This method is simple, sensitive and accurate for content determination and tissue distribution of 6＇-hydroxy justicidin A in Nu/Nu mice livers.
出处
《解放军药学学报》
CAS
2013年第1期20-22,25,共4页
Pharmaceutical Journal of Chinese People's Liberation Army
基金
北京市自然科学基金
No.7112092
2011年度高等学校博士学科点专项科研基金
No.20111106110034
科技部重大新药创制专项
No.2009ZX09502-025
2012ZX09301-002-001
中国医学科学院硕士研究生科研创新项目
No.2011106001007M10
