高速逆流色谱法分离制备化橘红中的柚皮苷、橙皮内酯水合物和异橙皮内酯

目的: 采用超临界流体萃取技术提取紫苏叶挥发油,并用GC-MS对挥发油进行化学成分分析。 方法: 通过单因素实验和正交实验法确定超临界CO₂流体萃取紫苏叶挥发油的最佳条件,考察萃取压力、温度、动态萃取时间及CO₂流量对挥发油得率的影响;利用GC-MS分析最佳萃取条件下所得挥发油的化学成分,面积归一化法测定其百分含量。 结果: 紫苏叶超临界CO₂萃取最佳条件为:萃取压力20 MPa,温度35 ℃,萃取时间150 min,CO₂流量10 kg·h^-1;挥发油的得率3.2%,从中鉴定出了16个化合物,其含量占出峰物质总量的97.68%。 结论: 紫苏叶挥发油中富含醚、萜类化合物、酯、酮和醇等组分。

Objective: To establish a high-speed counter-current chromatography(HSCCC) method for preparation and separation of the components of Exocarpium Citri Grandis. Methods: Naringin was obtained with two phase solvent system composed of ethyl acetate-n-butanol-water(4∶ 1∶ 5), meranzin hydrate was obtained with n-hexane-ethyl acetate-methanol-water (1∶ 2∶ 1∶ 2.5), isomeranzin was obtained with n-hexane-ethyl acetate-methanol-water (1∶ 1∶ 1∶ 1) by HSCCC, while the apparatus rotated at 857 r·min^-1 at 30 ℃. Results: The purities of naringin and meranzin hydrate were over 98.0%, the purity of isomeranzin was over 95.0% analysed by HPLC. Conclusion: HSCCC is a simple, high-performance method for the separation of naringin, meranzin hydrate and isomeranzin from Exocarpium Citri Grandis.