藤黄中藤黄酸两种异构体的hplc含量测定.docVIP

藤黄中藤黄酸两种异构体的HPLC含量测定 张俊艳1, 2，夏广萍1，赵娜夏1，常允平1, 2，韩英梅1* 1. 天津药物研究院 天津市新药设计与发现重点实验室，天津 300193 2. 天津中医药大学 天津 300193 mm×150mm，μm)，流动相为乙腈-甲醇-0.3%三氟乙酸(36:37:27)，检测波长为360 nm，流速为0.3 mL·min-1，柱温为28℃。结果：R-藤黄酸，S-藤黄酸线性关系方程分别为Y=-2.24×105+2.87×106X，R=0.9999； Y=-144×105+3.31×106X，R=0.9999。 关键词：R-藤黄酸；S-藤黄酸；高相液相色谱法；含量测定 Quantitative analysis of two gambogic acids in Garcinia hanburyi Hook.f. by HPLC ZHANG Jun-yan1,2, XIA Guang-ping1, Zhao Na-xia1, CHANG Yun-ping1,2, HAN Ying-mei1* 1. Tianjin Key Laboratory of Molecular Design and Drug Discovery, Tianjin Institute of Pharmaceutical Research, Tianjin 300193, China 2. Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China Abstract: Object: To establish a method for the determination of two gambogic acids by HPLC. Methods: Analytical column was SunFire(Waters) C8 (2.1mm×150mm，3.5 μm), the mobile phase consisted of acetonitrile -methanol-0.3% trifluoroacetic acid(36:37:27), the detection wavelength was 360 nm, the flow rate was 0.3 mL·min-1, the column temperature was 28℃.Results: The linear regression equation of R-gambogic acid is Y=-223658+2868721X, R=0.9999. The linear regression equation of S-gambogic acid is Y=-143551+3310250X,R=0.9999. The average recoveries were 100.0% and 100.9%, and RSD were 2.1% and 2.5% (n=6). The average contents of two gambogic acid in Garcinia hanburyi Hook.f. were 30.06% and 21.45%, respectively. Conclusion: The method was proved to be convenient and reliable, so it can be used for quantitative analysis and assay of R-gambogic acid and S-gambogic acid. Key words: R-gambogic acid, S-gambogic acid, HPLC, determination 笼状呫吨酮类化合物是药用藤黄(Garcinia hanburyi Hook.f.)中特征性成分类群，藤黄酸（gambogic acid）为其中最具代表性的成分，因具有抗肿瘤活性受到业界关注。藤黄酸在原药材中含量最高，早在1955年Amorosa通过吡啶盐结晶的方法得到，并在1965年确定了分子结构[1,2]。后续的研究发现该化合物存在C-2位R、S异购现象，以吡啶盐结晶法得到的是R构型，在原药材中是以R、S异构体混合物的形式存在。Quanbin Han[3] 等首次分离得到藤黄酸R、S异构体，并发现在肿瘤细胞上这两种异构体具有同等强度的细胞毒性，而在对人肝微粒体P-450酶系的抑制试验中S型对CYP2C9显示了很强的抑制作用，作用强度为R型的20倍，由此推测S构型有可能对R构型或其他联合用药的药代动力学过程产生影响。因此，建立藤黄酸R、