荆三棱中有效成分的提取工艺优选

Optimization of Extraction Technology of Active Components from Scirpus yagara

摘要:

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,5 μm),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10 μL。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13.95,5.95 μg·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。

Abstract:

Objective: To optimize extracting technology of sparstolonin B and sanleng diphenyllactone from Scirpus yagara. Method: Contents of sparstolonin B and sanleng diphenyllactone were determined by HPLC,chromatographic conditions were as follows:Hanbang column(4.6 mm×250 mm,5 μm),mobile phase of methanol-1% acetic acid(65:35),flow rate 1.0 mL·min^-1,column temperature 30℃,detection wavelength 385 nm,injection volume 10 μL.With extracting amounts of sparstolonin B and sanleng diphenyllactone as indexes,orthogonal test was adopted to investigate effects of the concentration and dosage of enthanol,extraction time,extraction times on technology. Result: Order of effects of each factors on yield of sparstolonin B was extraction times>ethanol concentration>ethanol consumption>extraction time,but effects of each factor on yield of sanleng diphenyllactone was in order of ethanol concentration>extraction times>extraction time>ethanol consumption.Optimum extraction technology was as following:reflux extracted 2 times with 10 times the amount of 70% ethanol,1.5 h per time;Average extracting amounts of sparstolonin B and sanleng diphenyllactone were 13.95,5.95 μg·g^-1,respectively. Conclusion: Optimized extraction technology was stable and feasible with high extraction efficiency;This established determination method was sensitive,accurate and reproducible.