德丽达·木拉提别克, 古丽美克热依·吐尼亚孜, 阿来·海拉希, 迪里努尔·马力克, 李茵萍. 新疆多花蔷薇根中熊果酸的提取及分离纯化工艺研究[J]. 云南大学学报(自然科学版), 2019, 41(3): 572-582. doi: 10.7540/j.ynu.20180694
引用本文: 德丽达·木拉提别克, 古丽美克热依·吐尼亚孜, 阿来·海拉希, 迪里努尔·马力克, 李茵萍. 新疆多花蔷薇根中熊果酸的提取及分离纯化工艺研究[J]. 云南大学学报(自然科学版), 2019, 41(3): 572-582. doi: 10.7540/j.ynu.20180694
Delida·Mulatibieke, Gulimeikereyi·Tuniyazi, Alai·Hailaxi, Dilnur·Malik, Li Yin-ping. Extraction, separation and purification of ursolic acid from Rosa multiflora Thunb root of Xinjiang[J]. Journal of Yunnan University: Natural Sciences Edition, 2019, 41(3): 572-582. DOI: 10.7540/j.ynu.20180694
Citation: Delida·Mulatibieke, Gulimeikereyi·Tuniyazi, Alai·Hailaxi, Dilnur·Malik, Li Yin-ping. Extraction, separation and purification of ursolic acid from Rosa multiflora Thunb root of Xinjiang[J]. Journal of Yunnan University: Natural Sciences Edition, 2019, 41(3): 572-582. DOI: 10.7540/j.ynu.20180694

新疆多花蔷薇根中熊果酸的提取及分离纯化工艺研究

Extraction, separation and purification of ursolic acid from Rosa multiflora Thunb root of Xinjiang

  • 摘要: 通过超声−微波辅助法提取了多花蔷薇根中的熊果酸,并对其进行分离、纯化,确定了最优提取及分离纯化条件. 采用响应面法优化熊果酸的提取工艺,经脱脂、脱色、酸碱沉淀、凝胶柱层析等方法得到了分离纯化熊果酸的最佳条件,用紫外光谱(UV),红外光谱(IR),核磁共振氢谱(1H NMR),核磁共振碳谱(13C NMR)对产品进行鉴定. 结果表明:在超声功率50 W,微波功率310 W,提取时间2.4 min,液固比20:1 mL/g,微波浸提时间15 min,浸提温度55 ℃的提取条件下,熊果酸的得率可达2.64%. 当石油醚用量为提取液体积的0.2倍,脱脂2次,活性炭用量0.04 g/mL,脱色3次,碱沉淀pH值为12,酸沉淀pH值为4,熊果酸粗品用葡聚糖凝胶LH-20分离洗脱2次时,重结晶后的熊果酸纯度在97%以上,达到较好的分离效果.

     

    Abstract: In this paper, ursolic acid was extracted from the roots of Rosa multiflora Thunb by ultrasonic−microwave−assisted extraction, and the optimum extraction and purification conditions were determined. The extraction process of ursolic acid was optimized by response surface methodology. The best conditions for separation and purification of ursolic acid were obtained by defatting, decolorizing, acid base precipitation and gel column chromatography. The products were identified by ultraviolet spectroscopy (UV), infrared spectroscopy (IR), 1H NMR and 13C NMR. The results showed that the yield of ursolic acid could reach 2.64% under the conditions of ultrasonic power 50 W, microwave power 310 W, extraction time 2.4 min, liquid−solid ratio 20∶1 mL/g, microwave extraction time 15 min and extraction temperature 55℃. When the amount of petroleum ether was 0.2 times of the volume of extract, 2 times of degreasing, 0.04 g/mL of active carbon, 3 times of decolorization; the pH value of alkali precipitation was 12; the acid precipitation pH value was 4; when ursolic acid crude product was separated from dextran gel LH-20 for two times, the purity of ursolic acid after recrystallization was over 97%, achieving a better separation effect.

     

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