氢化松香酯键合硅胶制备柱的研制及性能研究  

Preparation and Properties of Hydrogenated Rosin Ester Bonded Silica Gel Column

作　　者：姜利娟 吴惠莹 曾磊 苏宇萍 雷福厚 李浩 JIANG Lijuan;WU Huiying;ZENG Lei;SU Yuping;LEI Fuhou;LI Hao(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》2024年第2期1-8,共8页Chemistry and Industry of Forest Products

基　　金：国家自然科学基金资助项目(32060325);广西民族大学科研基金资助项目(2022KJQD16)。

摘　　要：将氢化松香丙烯酸乙二醇酯(EGHRA)通过点击化学反应键合到巯基化硅胶(SH@SiO_(2))表面,制备了一种新型的氢化松香丙烯酸乙二醇酯键合硅胶(EGHRA@SiO_(2))固定相。对合成的固定相进行元素分析、红外光谱、热失重分析、N 2吸附-脱附实验和粒径分布测试,结果显示:EGHRA@SiO_(2)固定相中的C元素较SiO_(2)增加了10.72个百分点,比表面积270.06 m 2/g,平均孔径6.16 nm,平均粒径10μm。使用匀浆法填装了250 mm×30 mm制备柱并对其进行了一系列色谱评价,证明EGHRA@SiO_(2)制备柱具有较好的流通性和典型的反相色谱特性,且表现出良好的稳定性和可重复性。Tanaka测试表明:由于键合单体具有类菲环骨架,使得EGHRA@SiO_(2)柱的空间选择性优于C18柱。反相色谱模式下,EGHRA@SiO_(2)制备柱对红豆杉树皮粗提物有较理想的分离效果,筛选出乙腈/水(体积比47∶53),在流速15 mL/min时进样1.0 mL,一次纯化将粗提物中紫杉醇的纯度提高了91.52个百分点,10-去乙酰基紫杉醇的纯度提高了83.24个百分点,7-木糖-10-去乙酰基紫杉醇的纯度提高了62.99个百分点,三尖杉宁碱的纯度提高了55.85个百分点。Hydrogenated rosin glycol acrylate(EGHRA)was bonded to the surface of thioglycolated silica gel(SH@SiO_(2))by click chemical reaction to prepare a novel hydrogenated rosin acrylate ethylene glycol ester bonded silica gel(EGHRA@SiO_(2))stationary phase.The synthesized stationary phase was characterized by elemental analysis,infrared spectroscopy,thermogravimetric analysis,N 2 adsorption-desorption experiments,and particle size distribution tests.The results showed that the EGHRA@SiO_(2)stationary phase had an increased C content of 10.72 percentage points compared to SiO_(2),a specific surface area of 270.06 m 2/g,an average pore diameter of 6.16 nm,and an average particle size of 10μm.A 250 mm×30 mm preparation column was filled by homogenization method,and a series of chromatographic evaluations were performed,demonstrating good flowability typical reversed-phase chromatographic characteristic as well as excellent stability and reproducibility of the EGHRA@SiO_(2)preparation column.Tanaka tests showed that the spatial selectivity of EGHRA@SiO_(2)column was superior to that of C18 column owing to the phenanthrene-like skeleton of the bonding monomer.Under reversed-phase chromatographic mode,EGHRA@SiO_(2)preparation column exhibited ideal separation performance for the crude extracts of Taxus bark.Using the screened acetonitrile-water(volume ratio of 47∶53)mobile phase at a flow rate of 15 mL/min,the purity of paclitaxel(PTX),10-deacetylbaccatin III(10-DAT),7-xylosyl-10-deacetylbaccatin III(7-xyl-10-DAT)and cephalomannine(CEP)in the crude extract were increased by 91.52,83.24,62.99 and 55.85 percentage points after a single purification step of 1.0 mL injection sample,respectively.

关 键 词：松香 制备型高效液相色谱 紫杉醇 制备柱 

分 类 号：TQ35[化学工程]