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目的:建立UPLC-MS同时测定小鼠组织中芦丁、野黄芩苷和半枝莲碱B的分析方法,并对该3种成分在小鼠体内的组织分布进行研究。方法:以2-氰基-3,12-二氧代齐墩果烷~(-1),9(11)-二烯-28-酸甲酯(CDDO-Me)为内标,通过甲醇沉淀组织样品蛋白,使用LC-MS技术进行定量分析,采用ACQUITY UPLC BEH-C18色谱柱(100 mm×2.1 mm,1.7μm),以0.1%甲酸水溶液-乙腈为流动相,梯度洗脱,正、负离子检测模式,检测离子质荷比(m/z)为芦丁609.2、野黄芩苷463.3、半枝莲碱B 558.4和CDDO-Me 506.7。结果:在小鼠肝脏、心脏、脾脏、肺脏、肾脏等组织中,芦丁、野黄芩苷、半枝莲碱B分别在0.005 0~0.160 0、0.004 0~0.133 0、0.0033~0.106 7μg·m L~(-1)的线性范围内线性关系良好(r≥0.9913);方法的精密度和稳定性RSD均小于15%;回收率为90.0%~98.4%,RSD小于15%,符合化学药物非临床药代动力学研究技术指导原则。芦丁等3个成分在小鼠体内分布比较广泛,其中在肝脏和肾脏中分布较多,在肺脏中分布含量最低。结论:本方法经方法学验证,可对小鼠组织中的芦丁、野黄芩苷、半枝莲碱B含量进行测定;在用于小鼠体内化学成分的组织分布研究中,芦丁在肾脏中含量多、脾脏中最少,野黄芩苷在心脏中含量最多、肺脏中最少,半枝莲碱B在肝脏中含量最多、肾脏中最少。
OBJECTIVE: To establish a method for the simultaneous determination of rutin, scutellarin and barbataeine B in mouse tissues by UPLC-MS, and to study the tissue distribution of the three components in mice. Methods: CDDO-Me was used as internal standard for 2-cyano-3,12-dioxo-oleanane-1 and 9 (11) -diene-28- Tissue sample proteins were quantified by LC-MS. The mobile phases were eluted with ACQUITY UPLC BEH-C18 column (100 mm × 2.1 mm, 1.7 μm) using 0.1% formic acid in acetonitrile as mobile phase. Positive and negative ions The detection mode, ion mass to charge ratio (m / z) of rutin 609.2, wild baicalin 463.3, Scutellarin B 558.4 and CDDO-Me 506.7. Results: Rutin, Scutellaria baicalensis and Scutellaria B in the liver, heart, spleen, lungs and kidneys of mice were 0.005-0 0.160 0,0.004 0-0,133 0,0.0033-0.106 7 μg · m The linearity of L ~ (-1) was linear (r≥0.9913). The precision and stability of the method were all less than 15%. The recoveries ranged from 90.0% to 98.4% with a RSD of less than 15% Clinical pharmacokinetic study of technical guidelines. Rutin and other three components are widely distributed in mice, which are more distributed in the liver and kidney, the distribution of the content in the lungs the lowest. Conclusion: This method was validated by methodology, rutin, Scutellaria baicalensis and Scutellaria B were determined in mouse tissues. In the study of the tissue distribution of chemical components in mice, In the content of the spleen in the least, wild baicalin content in the heart most, the least in the lungs, Scutellaria B content in the liver most, the least in the kidneys.