连翘与陈皮混合挥发油提取与包合工艺优化

Optimization of Extraction and Inclusion Processes of Mixed Volatile Oils from Forsythiae Fructus and Citri Reticulatae Pericarpium

目的优选保和颗粒组方中连翘、陈皮混合挥发油提取工艺及β-环糊精(β-CD)包合工艺。方法以饮片粉碎粒度、提取时间、加水倍数为考察因素,挥发油收率为评价指标,采用L_(9)(3^(4))正交试验法优选。以β-CD与挥发油比例(g∶m L)、包合时间、包合温度为考察因素,挥发油包合率、包合物收率、包合物含油量的综合评分为评价指标,同上法优选包合工艺并验证。结果最佳提取工艺,将饮片粉碎至20目,加10倍水提取3 h。最佳包合工艺,β-CD∶挥发油为7∶1(g∶m L),45℃下包合反应3 h;紫外光谱扫描、X射线衍射、扫描电镜、薄层色谱等结果均证明形成了稳定的包合物。制成的包合物中连翘及陈皮混合挥发油的包合率为95.13%,包合物收率为87.84%,包合物含油量为10.29%,综合评分为76.70分。结论优化后的连翘及陈皮混合挥发油提取、包合工艺稳定可行。

Objective To optimize the extraction process of mixed volatile oils from Forsythiae Fructus and Citri Reticulatae Pericarpium in the Baohe Granules and the inclusion process ofβ-cyclodextrin(β-CD).Methods The extraction process of mixed volatile oils from Forsythiae Fructus and Citri Reticulatae Pericarpium was optimized by the L_(9)(3^(4))orthogonal test,with the granule size of crushed decoction pieces,extraction time and water addition amount as the investigation factors,and with the volatile oil yield as the evaluation indicator.The inclusion process was optimized by the L_(9)(3^(4))orthogonal test,with the ratio ofβ-CD to volatile oil(g∶mL),inclusion time and inclusion temperature as the investigation factors,and with the comprehensive score of volatile oil inclusion rate,inclusion yield,and oil content of inclusions as the evaluation indicator,and then the verification test was conducted.Results The optimal extraction process was that crushing decoction pieces to a size of 20 mesh and extracting with 10 times the amount of water for 3 h.The optimal inclusion process was as follows:the ratio ofβ-CD to volatile oil was 7∶1(g∶mL),and the inclusion reaction lasted for 3 h at 45℃.The stable inclusions were proved by the ultraviolet(UV)spectral scanning,X-ray diffraction,scanning electron microscope(SEM),and thin layer chromatography(TLC).The inclusion rate of the mixed volatile oils from Forsythiae Fructus and Citri Reticulatae Pericarpium in the preparative inclusions was 95.13%,the inclusion yield was 87.84%,and the oil content of the inclusions was 10.29%,with the comprehensive score of 76.70 points.Conclusion The optimal extraction and inclusion processes of mixed volatile oils from Forsythiae Fructus and Citri Reticulatae Pericarpium is stable and feasible.