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目的:利用高速逆流色谱法分离何首乌中的游离蒽醌与二苯乙烯苷。方法:以不同溶剂系统分离纯化何首乌提取液,分别以紫外分光光度法测定其游离蒽醌含量,高效液相色谱法测定其二苯乙烯苷含量,同时以单因素试验考察高速逆流萃取流速、转速、萃取温度对游离蒽醌与二苯乙烯提取率的影响,在此基础上通过响应曲面法优化试验、优选最佳工艺。结果:以正己烷-乙酸乙酯-甲醇-水(9∶1∶5∶5)作为溶剂系统时,何首乌中游离蒽醌的分离度最高。以甲酸乙酯-甲醇-水(10∶0.5∶10)作为溶剂系统时,何首乌中二苯乙烯苷的分离度最高。何首乌游离蒽醌萃取工艺流程为:溶剂流速1.5 mL/min,转速735 r/min,萃取柱温度27℃;二苯乙烯苷萃取工艺流程为:溶剂流速1.5 mL/min,转速738 r/min,萃取柱温度26℃;此工艺条件下何首乌中游离蒽醌的质量分数达68.60%,二苯乙烯苷的质量分数达73.77%。结论:利用高速逆流色谱法富集何首乌中游离蒽醌、二苯乙烯苷,快速、简单、分离度好。
OBJECTIVE: To separate free anthraquinone and stilbene glycoside from Radix Polygoni multiflori by high speed countercurrent chromatography. Methods: The Polygonum multiflorum Thunb extract was isolated and purified with different solvent systems. The content of free anthraquinone was determined by UV spectrophotometry. The content of stilbene glycoside was determined by high performance liquid chromatography. The effects of high speed countercurrent extraction, flow rate, , The extraction temperature on the free anthraquinone and stilbene extraction rate, on the basis of response surface methodology to optimize the experiment, the best optimization process. Results: When n-hexane-ethyl acetate-methanol-water (9:1:5:5) was used as the solvent system, the separation of free anthraquinones from Polygonum multiflorum was the highest. When ethyl formate-methanol-water (10: 0.5: 10) was used as the solvent system, the concentration of stilbene glycoside in Polygonum multiflorum was the highest. Polygonum multiflorum anthraquinone extraction process: solvent flow rate 1.5 mL / min, speed 735 r / min, extraction temperature 27 ° C; stilbene glycoside extraction process: solvent flow rate 1.5 mL / min, speed 738 r / min, The temperature of the extraction column was 26 ℃. The mass fraction of anthraquinone in Radix Polygoni multiflori was 68.60% and the mass fraction of stilbene glucoside was 73.77%. Conclusion: The enrichment of free anthraquinone and stilbene in Polygonum multiflorum by high-speed countercurrent chromatography is rapid, simple and has good resolution.