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采用高速逆流色谱技术从马比木粗提物中快速分离制备喜树碱类化学成分。通过高效液相色谱测定各溶剂系统的分配系数,获得较好的分离条件。溶剂体系为:V(氯仿):V(正己烷):V(甲醇):V(水)=6:6:5:4,上相(水相)为固定相,下相(有机相)为流动相,正相洗脱;进样质量浓度:2.25 mg/mL;进样体积:20 mL;流速:2.0 mL/min;转速:800 r/min,从马比木粗提物中一次分离制备出3种单体成分。其结构经HPLC,UV,IR,ESI-MS和NMR确认和分析,分别为10-羟基脱氧喜树碱(1)、10-甲氧基喜树碱(2)和喜树碱(3),纯度分别为98.3%,99.3%,99.0%。
High-speed countercurrent chromatography technique was used to separate camptothecin from the crude extracts of the wood. The partition coefficient of each solvent system was determined by high performance liquid chromatography to obtain better separation conditions. The solvent system is as follows: V (n-hexane): V (methanol): V (water) = 6: 6: 5: 4; the upper phase Mobile phase, normal phase elution; injection mass concentration: 2.25 mg / mL; injection volume: 20 mL; flow rate: 2.0 mL / min; rotation speed: 800 r / min, Three kinds of monomer composition. Their structures were confirmed and analyzed by HPLC, UV, IR, ESI-MS and NMR, which were 10-hydroxydeoxycamptothecin (1), 10-methoxycamptothecin (2) and camptothecin Purities were 98.3%, 99.3%, 99.0%, respectively.