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作 者:李凤[1] 亢静静[1] 李爱峰[1] 孙爱玲[1] 柳仁民[1] LI Feng;KANG Jing-jing;LI Ai-feng;SUN Ai-ling;LIU Ren-min(College of Chemistry and Chemical Engineering,Liaocheng University,Liaocheng 252059,China)
机构地区:[1]聊城大学化学化工学院
出 处:《高校化学工程学报》2019年第6期1437-1443,共7页Journal of Chemical Engineering of Chinese Universities
基 金:国家自然科学基金(21675071);山东省重点研发计划(2016GSF202007)
摘 要:建立超临界流体色谱(SFC)分离纯化补骨脂中异补骨脂素和补骨脂素的工艺方法。采用YMC-C18、YMC-Diol和YMC-NH2等3种色谱柱,甲醇、乙腈、乙醇、异丙醇等4种改性剂,流动相流速2~6 mL×min^-1、温度300~325 K、压力10~14 MPa条件下,考察了异补骨脂素和补骨脂素的纯化效果。放大得到制备型SFC条件为:色谱柱YMC-Diol;流动相为含有j=2%甲醇的超临界二氧化碳,流速14.0 mL×min^-1;分离温度313 K;压力12 MPa。结果表明,分离得到的异补骨脂素和补骨脂素的纯度均大于98%,由Van’t Hoff曲线可知实验条件下SFC分离过程为焓控过程。A supercritical fluid chromatography(SFC) method was established for the separation and purification of isopsoralen and psoralen from Psoralea corylifolia L. The analytical conditions were: three columns including YMC-C18, YMC-Diol and YMC-NH2, four modifiers including methanol, acetonitrile, ethanol and isopropanol, flow rate of mobile phase 2~6 m L×min^-1, separation temperature 300~325 K and separation pressure 10~14 MPa. Moreover, the conditions for preparative SFC were: column = YMC-Diol, mobile phase = supercritical carbon dioxide containing 2%(v/v) methanol at a flow rate of 14.0 mL×min^-1, separation temperature = 313 K and separation pressure = 12 MPa. The result shows that the purities of isopsoralen and psoralen are both above 98%. The Van’t Hoff curve shows that the SFC separation is an enthalpy control process under the experimental conditions.
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