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目的:优选荆三棱中三棱内酯B和三棱双苯内酯的提取工艺。方法:采用HPLC测定三棱内酯B和三棱双苯内酯含量,色谱条件为汉邦色谱柱(4.6 mm×250 mm,5μm),流动相甲醇-1%冰醋酸(65∶35),流速1.0 mL·min-1,柱温30℃,检测波长385 nm,进样量10μL。以三棱内酯B和三棱双苯内酯提取量为指标,通过正交试验考察乙醇体积分数、乙醇用量、提取时间及提取次数对提取工艺的影响。结果:各因素对三棱内酯B提取量的影响顺序依次为提取次数>乙醇体积分数>乙醇用量>提取时间,各因素对三棱双苯内酯提取量的影响大小依次为乙醇体积分数>提取次数>提取时间>乙醇用量。优选的提取工艺为加10倍量70%乙醇水浴加热2次,每次1.5 h,三棱内酯B、三棱双苯内酯平均提取量分别为13.95,5.95μg·g-1。结论:优选的工艺稳定可行,提取效率高;建立的HPLC测定方法灵敏、准确、重复性好。
OBJECTIVE: To optimize the extraction process of Trialeptolide B and Tribenurpin in Jing Triangular prism. Methods: The HPLC method was used to determine the content of trimellolactone B and tribenuron diphenyl lactone. The chromatographic conditions were as follows: Hanbang column (4.6 mm × 250 mm, 5 μm), mobile phase methanol-1% glacial acetic acid (65:35) Flow rate 1.0 mL · min-1, column temperature 30 ℃, detection wavelength 385 nm, injection volume 10μL. The effects of ethanol volume fraction, ethanol amount, extraction time and extraction times on the extraction process were investigated by orthogonal test. Results: The order of the effect of each factor on the extraction yield of trigeminal lactone B were order of extraction> volume fraction of ethanol> amount of ethanol> extraction time, and the influence of various factors on the extraction yield of tribenurpin was as follows: ethanol volume fraction> Extraction times> Extraction time> Ethanol consumption. The optimal extraction process was heating twice with 10 times amount of 70% ethanol in water bath for 1.5 h each. The average extraction yield of the trigeminal lactone B and the trigeminobiphenyl lactone was 13.95 and 5.95 μg · g -1, respectively. Conclusion: The optimal process is stable and feasible, and the extraction efficiency is high. The established HPLC method is sensitive, accurate and reproducible.