白术中白术内酯Ⅰ的超临界CO_2萃取工艺研究

Supercritical CO_2 extraction of atractylenolide Ⅰ from Atractylodes macrocephala

目的探讨超临界CO2流体萃取白术中白术内酯Ⅰ的方法,并建立白术内酯Ⅰ高效液相色谱测定方法。方法考察了萃取压力、解析压力等7个因素对白术中白术内酯Ⅰ的超临界CO2流体萃取的影响。采用高效液相色谱法对白术内酯Ⅰ进行HPLC分析。色谱柱HypersilODS2,流动相甲醇-水(70∶30),体积流量1.0mL/min;检测波长220nm。结果以10%乙醇为携带剂,药材粒度60目,萃取压力25MPa,解析压力5MPa,萃取温度40℃,解析温度30℃的条件下萃取4h为最佳工艺。结论超临界萃取法提取白术中白术内酯Ⅰ耗时少、准确、效率高,可用于工业化大生产和小规模试验。建立的白术超临界提取物中白术内酯Ⅰ的测定方法简单、灵敏、结果可靠。

Objective To investigate the extraction technique for atractylenolide I in Atractylodes macrocephala by supercritical CO2 fluid extraction and develop a method used for determining the content of atractylenolide I in the extract by HPLC. Methods The effects of seven facters, such as the extracting pressure, resolving pressure etc, to the extraction rate of atractylenolide I in A. macrocephala by supercritical CO2 extraction were investigated. RP-HPLC was used to determine the content of atractylenolide I in extraction of A. macrocephala. The separation was performed on Hypersil ODS2 column with methanol-water （70 ： 30） as mobile phase. The flow rate was 1.0 mL/min and the wavelength of UV detector was 220 nm. Results The optimal extracting conditions ： taking 10% alcohol as entraiter, the particle size of medicinal substances was 60 screen meshes, extracting pressure 25 MPa, resolving pressure 5 MPa, extracting temperature 40℃, resolving temperature 30℃, and the extracting time 4 h. Conclusion Supercritical extraction is time-shorter and efficient in extracting atractylenolide Ⅰ from A. macrocephala. It is suitable to both trial and industrialized production. The method established to determine the content of atractylenolide Ⅰof A. macrocephala by supercritical extraction is simple, sensitive, and reliable.