摘要
目的:建立HPLC-MS同时测定大鼠组织中五味子醇甲、五味子甲素和五味子乙素的分析方法,并应用于3个木脂素成分在大鼠体内的组织分布研究。方法:以睾丸酮为内标,组织样品经乙腈沉淀蛋白后进行HPLC-MS分析,采用依利特ODS-C18色谱柱(250 mm×4.6 mm,5μm),乙腈(A)-0.05%甲酸水溶液(B)为流动相,梯度洗脱;正离子选择性检测(SIM)模式,选择的检测离子质荷比(m/z)为五味子醇甲433.2、五味子甲素401.0、五味子乙素417.0和睾丸酮289.0。结果:在大鼠不同组织中,3个木脂素成分在测定的线性范围内线性关系良好(r≥0.9951);方法的精密度和稳定性RSD均小于15%;回收率为81.11%～99.49%,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。3个木脂素成分在大鼠体内分布比较广泛,主要分布在肝和肺组织中,在脾中的分布浓度最低。结论:建立的方法简便易行、准确可靠,应用于大鼠体内木脂素成分的组织分布研究,获得了满意的结果。
Objective： To develop an HPLC-MS method for simultaneous determination of schisandrin,deoxyschisandrin and schisandrin B in rat tissues,and apply the method to tissue distribution study of three studied lignans.Methods： The tissue samples were precipitated with acetonitrile and analyzed by HPLC-MS with acetonitrile-0.05% formic acid solution as a gradient elution mobile phase.Testosterone was used as an internal standard.The mass spectrometer was operated in selected reaction monitoring（SIM） mode with positive electrospray ionization,the transition m / z 433.2,m / z 401.0,m / z 417.0 and m / z 289.0 was used for schisandrin,deoxyschisandrin,schisandrin B and testosterone,respectively.Results： Excellent linearity（r≥0.9951） was observed in all three studied lignans in their linear range.The RSD of precision and stability of the developed method was less than 15%.The recovery of the method was 81.11%-99.49% with RSD less than 15%.Schisandrin,deoxyschisandrin and schisandrin B were widely distributed in rat tissues.Majority was found in liver and lung,and lowest in spleen.Conclusion： The established method is simple and accurate.Satisfactory results are obtained applying this method to the tissue distribution study of schisandrin,deoxyschisandrin and schisandrin B.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2013年第7期1121-1126,共6页
Chinese Journal of Pharmaceutical Analysis
基金
国家科技重大专项项目(No.2009ZX09308-004)
江苏省教育厅重大项目(NO.09KJA360001)
江苏省针灸结合重点实验室课题(No.KJA200906)
江苏省优秀学科开放课题(NO.2011ZYX2-003)
