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
姜利娟 1吴惠莹 1曾磊 1苏宇萍 1雷福厚 1李浩1
作者信息
- 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
- 折叠
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@SiO2)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@SiO2)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、N2 吸附-脱附实验和粒径分布测试,结果显示:EGHRA@SiO2固定相中的C元素较SiO2 增加了 10.72 个百分点,比表面积 270.06 m2/g,平均孔径 6.16 nm,平均粒径10 μm.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@SiO2 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@SiO2柱的空间选择性优于C18 柱.反相色谱模式下,EGHRA@SiO2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.
Abstract
Hydrogenated rosin glycol acrylate(EGHRA)was bonded to the surface of thioglycolated silica gel(SH@SiO2)by click chemical reaction to prepare a novel hydrogenated rosin acrylate ethylene glycol ester bonded silica gel(EGHRA@SiO2)stationary phase.The synthesized stationary phase was characterized by elemental analysis,infrared spectroscopy,thermogravimetric analysis,N2 adsorption-desorption experiments,and particle size distribution tests.The results showed that the EGHRA@SiO2 stationary phase had an increased C content of 10.72 percentage points compared to SiO2,a specific surface area of 270.06 m2/g,an average pore diameter of 6.16 nm,and an average particle size of 10 μm.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@SiO2 preparation column.Tanaka tests showed that the spatial selectivity of EGHRA@SiO2 column was superior to that of C18 column owing to the phenanthrene-like skeleton of the bonding monomer.Under reversed-phase chromatographic mode,EGHRA@SiO2 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Key words
rosin/preparative liquid chromatography/paclitaxel/preparation column引用本文复制引用
基金项目
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)
出版年
2024
国家科技期刊平台
NSTL
万方数据