论文部分内容阅读
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 establish a method for simultaneous determination of Schizandrin A, Schisandrin A and Schisandrin B in rat tissues by HPLC-MS, and to study the tissue distribution of three lignans in rats. Methods: Testosterone was used as an internal standard. The samples were separated by acetonitrile and analyzed by HPLC-MS. The elution was performed on the ODS-C18 column (250 mm × 4.6 mm, 5 μm) ) As mobile phase and gradient elution. In the mode of positive ion selective detection (SIM), the m / z ratios of schisandrin A 433.2, schisandrin A 401.0, schisandrin B 417.0 and testosterone 289.0 were selected. Results: The linearity of three lignan components in different tissues of rats was linear (r≥0.9951). The precision and stability RSD were less than 15% and the recoveries were 81.11% ~ 99.49 %, RSD less than 15%, in line with non-clinical pharmacokinetic study of technical guidelines. Three lignans were widely distributed in rats, mainly in liver and lung tissues, with the lowest concentration in the spleen. Conclusion: The established method is simple, accurate and reliable. It is applied to the tissue distribution of lignan in rats and the satisfactory results are obtained.