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目的建立高速逆流色谱(HSCCC)法从裂叶独活根中分离制备高质量分数的香豆素类成分。方法利用高效液相色谱-二极管阵列检测器分析优化溶剂体系,选择正己烷-醋酸乙酯-甲醇-水(1.5∶2.5∶2∶1.5)为HSCCC溶剂系统,上相为固定相,下相为流动相,主机转速为850 r/min,体积流量为3 m L/min,检测波长为323 nm。所接收馏份在50℃减压浓缩,静置得到蛇床子素晶体、二氢欧山芹醇乙酸酯晶体和二氢欧山芹醇当归酸酯晶体,应用核磁共振氢谱、碳谱、质谱、红外光谱等进行鉴定,并用HPLC测定质量分数。结果进样量为300 mg浸膏,得到二氢欧山芹醇乙酸酯6.3 mg、蛇床子素10.6 mg、二氢欧山芹醇当归酸酯6.4 mg,三者的质量分数均达到96.0%以上。结论 HSCCC法可用于裂叶独活中高质量分数香豆素类成分的快速分离制备。
OBJECTIVE To establish a high-speed countercurrent chromatography (HSCCC) method for the separation and preparation of high-quality coumarins from the root of Ligustrum lucidum. Methods The optimized solvent system was analyzed by high performance liquid chromatography with diode array detector. The solvent system was n-hexane-ethyl acetate-methanol-water (1.5: 2.5: Mobile phase, the host speed of 850 r / min, the volume flow of 3 m L / min, the detection wavelength of 323 nm. The received fraction was concentrated under reduced pressure at 50 ° C and allowed to stand for the solution of osthole crystals, octahydrin, and achyl alcohol dihydrochloride angelices, and the products were characterized by 1H-NMR, GC, MS and FTIR Etc., and the mass fraction was determined by HPLC. Results The injection volume was 300 mg, and the yield of dihydro octapeptane acetate 6.3 mg, osthole 10.6 mg, and dihydroalpinechlorethylene angelate 6.4 mg was obtained, and the mass fractions of the three reached more than 96.0%. Conclusion The HSCCC method can be used for the rapid separation and preparation of high-quality coumarin components in Cleopatra.