漆酚酯键合SiO_(2)色谱柱分离纯化天麻素及其热力学研究  

Separation and Purification of Gastrodin by Urushiol Methacrylate Bonded SiO_(2) Column and Its Thermodynamic Study

作　　者：曾磊 易冯梅 曹宇 史伯安 雷福厚 ZENG Lei;YI Fengmei;CAO Yu;SHI Bo'an;LEI Fuhou(College of Chemistry and Chemical Engineering,Guangxi Minzu University,Guangxi Key Laboratory of Chemistry and Engineering of Forest Products,Key Laboratory of Chemistry and Engineering of Forest Products,State Ethnic Affairs Commission,Guangxi Collaborative Innovation Center for Chemistry and Engineering of Forest Products,Nanning 530006,China;School of Chemical and Environmental Engineering,Hubei Minzu Unirensity,Enshi 445000,China)

机构地区：[1]广西民族大学化学化工学院,广西林产化学与工程重点实验室,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协同创新中心,广西南宁530006 [2]湖北民族大学化学与环境工程学院,湖北恩施445000

出　　处：《林产化学与工业》2022年第5期30-36,共7页Chemistry and Industry of Forest Products

基　　金：国家自然科学基金资助项目(31460172);广西科技基地和人才专项(AD18126005);广西林产化学与工程重点实验室开放项目(GXFC2004)。

摘　　要：利用天麻素(GAS)的结构类似物苯基-β-D-吡喃葡萄糖苷(PGL)和4-甲氧基苯基-β-D-吡喃葡萄糖苷(MGL)作为竞争分子,考察漆酚酯键合SiO_(2)色谱柱对天麻素的分离性能,并对其分离过程进行热力学分析。研究发现:漆酚酯键合SiO_(2)色谱柱分离天麻素的最佳色谱条件为以乙腈-0.05%磷酸水溶液(体积比3∶97)为流动相,流速0.4 mL/min,柱温25℃,检测波长220 nm,进样量20 mL。在该色谱条件下,漆酚酯键合SiO_(2)色谱柱对PGL-GAS的分离度达到7.8,对MGL-GAS的分离度达到14.0。热力学研究发现:分离过程中PGL-GAS和MGL-GAS的ΔH、ΔΔH和ΔΔG均小于0,ΔΔS均大于0,表明漆酚酯键合SiO_(2)色谱柱对天麻素及其结构类似物的分离过程是一个自发的放热过程,分离既受熵驱动又受焓驱动;随着柱温的升高,分析物的保留因子与分离度均有所下降。天麻粗提物经漆酚酯键合SiO_(2)色谱柱纯化后,杂质明显降低,天麻素的纯度由粗提物中的17.06%提升至93.45%,纯化过程中漆酚酯键合SiO_(2)色谱柱表现出良好的分离性能和稳定性。Using phenyl-β-D-glucopyranoside(PGL)and 4-methoxyphenyl-β-D-glucopyranoside(MGL)as the competitive molecules owing to its structural analogues of gastrodin(GAS),the separation performance of GAS by usurushiol methacrylate bonded SiO_(2) column was investigated,and its thermodynamics behavior was also analyzed.The result showed that the optimum separation conditions of urushiol methacrylate bonded SiO_(2) chromatographic column were as follows:0.05%phosphoric acid water solution(3∶97,volume ratio),flow rate 0.4 mL/min,column temperature 25℃,detection wavelength 220 nm and injection volume 20 L.Under this chromatographic condition,the resolution of urushiol methacrylate bonded SiO_(2) chromatographic column to PGL-GAS and MGL-GAS was 7.8 and 14.0,respectively.The thermodynamic studies revealed that theΔH,ΔΔH andΔΔG values of both PGL-GAS and MGL-GAS were negative,and theΔΔS values were greater than zero,during the process of separation.It indicated that the separation of GAS and its structural analogues on urushiol methacrylate bonded SiO_(2) column was a thermodynamic spontaneous process,which was driven both by the entropy and enthalpy.The retention and resolution of analytes decrease with the increasing column temperature.After the crude extract was purified by usurushiol methacrylate bonded SiO_(2) column,the impurities were significatly reduced,and the purity of gastrodin increased from 17.06%to 93.45%.The urushiol methacrylate bonded SiO_(2) column exhibited good separation performance and stability during the separation process.

关 键 词：漆酚酯键合SiO_(2)色谱柱 天麻素 分离 纯化 热力学 

分 类 号：TQ35[化学工程]