【摘要】：目的:通過正交試驗與三步沉淀法優(yōu)選地榆總皂苷的提取與純化工藝條件。方法:采用HPLC-ELSD測定地榆皂苷-Ⅰ的含量,流動相[甲醇-乙腈(1∶1)]-水梯度洗脫,蒸發(fā)光散射檢測器的漂移溫度100℃,氣體流速3.0 L·min-1。以地榆皂苷-Ⅰ轉(zhuǎn)移率為指標,通過正交試驗優(yōu)選地榆總皂苷的提取工藝;采用三步堿沉法,以鞣質(zhì)清除率與地榆皂苷-Ⅰ含量為評價指標,通過單因素試驗優(yōu)選純化工藝。結(jié)果:地榆總皂苷最佳工藝條件為加8倍量70%乙醇回流提取2次,每次1.5 h,提取液加10%氫氧化鈉溶液調(diào)p H 12~14,靜置12 h,離心去沉淀,上清液用10%氫氧化鈉溶液調(diào)p H 12~13,靜置24 h,離心,沉淀于70℃減壓干燥至干,用30倍量無水乙醇回流30 min,減壓回收乙醇至有固形物析出,固形物減壓干燥12 h。地榆總皂苷純度91.32%。結(jié)論:優(yōu)選的地榆總皂苷提取純化工藝路線簡單、穩(wěn)定,制備的地榆總皂苷得率、純度高,適合工業(yè)化生產(chǎn)。
[Abstract]:OBJECTIVE:To optimize the extraction and purification conditions of total saponins from Sanguisorba officinalis by orthogonal test and three-step precipitation method.METHODS:The content of saponins from Sanguisorba officinalis was determined by HPLC-ELSD,the mobile phase was gradient elution with methanol-acetonitrile(1:1)-water,the drift temperature of evaporative light scattering detector was 100 C,the gas flow rate was 3.0 L.min-1.The transfer rate of saponins from Sanguisorba officinalis- The extraction process of total saponins from Sanguisorba officinalis was optimized by orthogonal test, and the tannin removal rate and the content of saponins from Sanguisorba officinalis L. were used as evaluation indexes. The purification process was optimized by single factor test. The supernatant was adjusted by 10% NaOH solution for 24 hours, centrifuged and dried at 70 C for 30 minutes. The ethanol was recovered by 30 times of anhydrous ethanol for 30 minutes. The purity of total saponins was 91.32%. The extraction and purification process of total saponins is simple and stable, and the yield of total saponins is high. It is suitable for industrial production.
【作者單位】： 成都中醫(yī)藥大學(xué)藥學(xué)院中藥材標準化教育部重點實驗室四川省中藥資源系統(tǒng)研究與開發(fā)利用重點實驗室——省部共建國家重點實驗室培育基地;江西中醫(yī)藥大學(xué)現(xiàn)代中藥制劑教育部重點實驗室;
【基金】：國家自然科學(xué)基金項目(81373976) 國家“重大新藥創(chuàng)制”科技重大專項(2013ZX09103002-013)
【分類號】：R283.6

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