核壳型松香基高分子键合硅胶液相色谱固定相高效分离紫杉醇  

Highly Effective Separation of Paclitaxel by Using Core-shell Rosin-based Polymer Bonded Silica as Liquid Chromatography Stationary Phase

作　　者：李浩 谢文博 曾磊 易柳钰 李文 雷福厚 LI Hao;XIE Wenbo;ZENG Lei;YI Liuyu;LI Wen;LEI Fuhou(School of Chemistry and Chemical Engineering,Guangxi Minzu University,Key Laboratory of Chemistry and Engineering of Forest Products,State Ethnic Affairs Commission,Guangxi Key Laboratory of Chemistry and Engineering of Forest Products,Guangxi Collaborative Innovation Center for Chemistry and Engineering of Forest Products,Nanning 530006,China)

机构地区：[1]广西民族大学化学化工学院,林产化学与工程国家民委重点实验室,广西林产化学与工程重点实验室,广西林产化学与工程协同创新中心,广西南宁530006

出　　处：《林产化学与工业》2023年第1期34-42,共9页Chemistry and Industry of Forest Products

基　　金：国家自然科学基金资助项目(32060325)。

摘　　要：将富马海松酸三(β-丙烯酰氧基乙基)酯(FATE)通过自由基聚合反应键合到烷基化硅胶(TPM-SiO_(2))表面,制备了核壳型松香基高分子键合硅胶(RP@SiO_(2))固定相,对RP@SiO_(2)固定相进行了一系列表征和评价,探讨了RP@SiO_(2)柱对紫杉醇(PTX)及其类似物的分离性能和分离机理,并将其用于红豆杉树皮粗提物中PTX的分离纯化。结果表明:FATE成功键合在硅胶表面,核壳型结构材料成功制备,RP@SiO_(2)的平均粒径约为5μm;RP@SiO_(2)柱是类似于C18柱的典型反相色谱柱,表现出优异的色谱性能、良好的重现性和典型的反相色谱行为;采用RP@SiO_(2)柱分离紫杉醇类似物,连续洗脱样品的分离度均超过6.6。计量置换保留理论(SDT-R)和van’t Hoff热力学分析结果表明:疏水相互作用决定了分析物的保留,在RP@SiO_(2)柱上分离紫杉醇类似物是一个焓驱动的放热过程,SDT-R可用于解释其保留机理。采用RP@SiO_(2)柱从红豆杉树皮粗提物中分离纯化紫杉醇,紫杉醇的纯度由6%提高到81%。A rosin-based core-shell polymer bonded silica(RP@SiO_(2))stationary phase was prepared by the radical polymerization of fumaropimaric acid tri(β-acryloxyl ethyl)ester(FATE)onto alkylated silica(TPM-SiO_(2)).The RP@SiO_(2)stationary phase was characterized and evaluated,the separation performance and mechanism of RP@SiO_(2)column for paclitaxel(PTX)and its analogs were discussed,and it was used for the separation and purification of PTX from crude yew-bark extract.The results showed that FATE was successfully bonded to the surface of silica,the core-shell structure material was successfully prepared,and the average particle size of RP@SiO_(2)was about 5μm.The RP@SiO_(2)column was a typical reversed-phase column similar to C18 column,showing excellent chromatographic performance,satisfactory performance reproducibility,and typical reversed-phase chromatographic behavior.The RP@SiO_(2)column was used to separate paclitaxel analogs,and the separation degree of continuous elution samples was more than 6.6.Stoichiometric displacement theory for retention(SDT-R)and van’t Hoff thermodynamic analysis showed that hydrophobic interactions determined the analyte retention,and the separation of paclitaxel analogs on RP@SiO_(2)column was an exothermic process driven by enthalpy.Furthermore,SDT-R could be used to explain its retention mechanism.The RP@SiO_(2)column was employed to separate and purify paclitaxel from crude yew-bark extract,increasing paclitaxel purity from 6%to 81%.

关 键 词：松香基固定相 高效液相色谱 保留机理 紫杉醇 

分 类 号：TQ35[化学工程] O658[理学—分析化学]