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 Ⅰ of A. macrocephala by supercritical extraction is simple, sensitive, and reliable.