大孔吸附树脂同时纯化雪松松针中的莽草酸和总黄酮
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摘要
目的优选大孔吸附树脂同时纯化雪松松针中莽草酸和总黄酮的最佳工艺。方法以雪松松针中莽草酸和总黄酮的质量分数为评价指标,考察了6种树脂的纯化效果;以上样质量浓度、上样体积流量、上样量、水洗脱用量、乙醇质量浓度和乙醇洗脱用量考察了最佳树脂的纯化能力;在单因素实验的基础上,采用正交试验法,通过综合评分优选最佳的纯化工艺。结果 XAD 7HP树脂对雪松松针中莽草酸和总黄酮的纯化效果最佳,水洗脱部分为莽草酸,乙醇洗脱部分为总黄酮,其最佳的纯化工艺为上样液中莽草酸的质量浓度11.59 mg/m L和总黄酮的质量浓度6.96 mg/m L、上样体积流量8 BV/h、上样量2.0 m L/g;水洗脱用量为上样液加4 BV的水洗液、70%的乙醇洗脱4 BV。纯化后莽草酸的质量分数由19.25%提升到28.98%,总黄酮的质量分数由11.92%提升到54.45%。结论优选的纯化工艺稳定、可行,为工业化生产雪松松针中莽草酸和总黄酮提供参考。
Objective To research the simultaneous purification process of shikimic acid and total flavonoids from pine needles of Cedrusdeodara(Roxb.) G. Don. Methods Taking the purity of shikimic acid and total flavonoids as the evaluation indicator, the purification effect of six macroporous resins were evaluated. Orthogonal design L9(34) and single factor experiments were employed to optimize the purification conditions by comprehensive scoring. The purification capacity of the best resin was investigated by the sample mass concentration, the volume flow of the sample, the ratio of the resin to the drug, the amount of water for washing, the concentration of ethanol, and the elution of ethanol. Results XAD 7 HP macrophous resin offered better purification effect of shikimic acid and total flavonoids from pine needles of C. deodara than other macrophous resins. The optimum purification condition was confirmed as follows: The concentration of shikimic acid in the sample was 11.59 mg/m L, and total flavonoids concentration was 6.9 mg/m L; The flow rate was 8 BV/h, and the sample volume was 2.0 m L/g; The shikimic acid was eluted with loading capacity and 4 BV of water; The total flavonoids was eluted with 4 BV of 70% ethanol successively. The purity of shikimic acid can be increased from 19.25% to 28.98%, and the purity of total flavonoids can be increased from 11.92% to 54.45%. Conclusion The optimized purification process is stable, feasible and suitable for pilot enrichment of shikimic acid and total flavonoids from pine needles of C. deodara.
Objective To research the simultaneous purification process of shikimic acid and total flavonoids from pine needles of Cedrusdeodara(Roxb.) G. Don. Methods Taking the purity of shikimic acid and total flavonoids as the evaluation indicator, the purification effect of six macroporous resins were evaluated. Orthogonal design L9(34) and single factor experiments were employed to optimize the purification conditions by comprehensive scoring. The purification capacity of the best resin was investigated by the sample mass concentration, the volume flow of the sample, the ratio of the resin to the drug, the amount of water for washing, the concentration of ethanol, and the elution of ethanol. Results XAD 7 HP macrophous resin offered better purification effect of shikimic acid and total flavonoids from pine needles of C. deodara than other macrophous resins. The optimum purification condition was confirmed as follows: The concentration of shikimic acid in the sample was 11.59 mg/m L, and total flavonoids concentration was 6.9 mg/m L; The flow rate was 8 BV/h, and the sample volume was 2.0 m L/g; The shikimic acid was eluted with loading capacity and 4 BV of water; The total flavonoids was eluted with 4 BV of 70% ethanol successively. The purity of shikimic acid can be increased from 19.25% to 28.98%, and the purity of total flavonoids can be increased from 11.92% to 54.45%. Conclusion The optimized purification process is stable, feasible and suitable for pilot enrichment of shikimic acid and total flavonoids from pine needles of C. deodara.
引文
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[13]吴方,余陈欢,俞文英,等.基于micro RNAs的石荠苧总黄酮抗流感病毒性肺炎作用机制研究[J].中草药,2016,47(7):1149-1154.
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[15]刘东彦,石晓峰,胡鹏斌,等.大孔吸附树脂富集纯化雪松松针总黄酮工艺的优化[J].中成药,2017,39(2):308-311.
[16]刘东彦,张莉霞,石晓峰,等.雪松松针中莽草酸和多糖的提取工艺研究[J].中药材,2017,40(8):1915-1917.
[17]胡鹏斌,韩涛,刘东彦,等.雪松松针中总黄酮及4种指标成分的含量测定方法研究[J].中国药房,2015,26(3):381-383.
[18]何春喜,余泽义,何毓敏,等.竹节参总皂苷的大孔吸附树脂纯化与离子交换树脂脱色工艺研究[J].中草药,2017,48(6):1146-1152.
[19]罗春梅,黄志芳,汤依娜,等.附子水溶性生物碱提取纯化工艺研究[J].中草药,2017,48(12):2415-2424.
[20]孙静,刘洁琼,黎伟华,等.陕产黄花油点草总黄酮部位纯化工艺研究[J].中草药,2013,44(10):1275-1279.
[21]于鹤云,刘汉清,刘嘉,等.D-101型大孔吸附树脂纯化黄蜀葵花总黄酮的工艺研究[J].中成药,2014,36(3):520-525.
[22]钟方丽,金龙哲,王晓林,等.大孔吸附树脂纯化黄芪茎总黄酮的工艺及其抗氧化性[J].河南工业大学学报:自然科学版,2017,38(2):88-94.
[23]董双双,袁悦,杨志伟.大孔吸附树脂在黄酮类化合物分离纯化中的应用[J].精细与专用化学品,2016,24(11):29-32.
[2]白朝辉,石晓峰,刘东彦,等.雪松松针的化学成分及药理作用研究进展[J].中国药师,2012,15(12):1791-1793.
[3]雷艳萍,石晓峰,白朝晖,等.雪松不同部位中莽草酸的含量分析[J].中国药房,2015,26(6):803-805.
[4]李师,刘东彦,石晓峰,等.雪松松针正丁醇部位化学成分的研究[J].中草药,2014,45(18):2602-2606.
[5]王东东,石晓峰,李冲,等.7种松柏科植物中莽草酸的含量测定[J].中国药房,2011,22(7):616-618.
[6]刘东彦,石晓峰,李冲,等.雪松松针中莽草酸的分离及其纯度检查[J].中国现代应用药学杂志,2011,28(7):637-640.
[7]刘东彦,石晓峰,王东东,等.雪松松针黄酮类化学成分的研究[J].中草药,2011,42(4):631-633.
[8]Liu D Y,Shi X F,Wang D D,et al.A new flavonoid in pine needles of Cedrus deodara[J].Chin Herb Med,2011,3(1):5-6.
[9]Liu D Y,Shi X F,Wang D D,et al.Two new myricetin glycosides from pine needles of Cedrus deodara[J].CNC,2011,47(5):704-707.
[10]刘东彦,石晓峰,李冲,等.雪松松针醋酸乙酯部位化学成分研究[J].中草药,2011,42(10):1921-1924.
[11]张军民,石晓峰.天然产物莽草酸的研究进展[J].中国中医药信息杂志,2011,18(2):109-112.
[12]李湘洲,栾芳菲,张胜,等.黄酮类化合物的抗肿瘤和抗血管生成作用研究进展[J].食品与机械,2016,32(1):199-201.
[13]吴方,余陈欢,俞文英,等.基于micro RNAs的石荠苧总黄酮抗流感病毒性肺炎作用机制研究[J].中草药,2016,47(7):1149-1154.
[14]Shi X F,Liu D Y,Zhang J M,et al.Extraction and purification of total flavonoids from pine needles of Cedrus deodara contribute to anti-tumor in vitro[J].BMC Complem Altern M,2016,16(1):245-253.
[15]刘东彦,石晓峰,胡鹏斌,等.大孔吸附树脂富集纯化雪松松针总黄酮工艺的优化[J].中成药,2017,39(2):308-311.
[16]刘东彦,张莉霞,石晓峰,等.雪松松针中莽草酸和多糖的提取工艺研究[J].中药材,2017,40(8):1915-1917.
[17]胡鹏斌,韩涛,刘东彦,等.雪松松针中总黄酮及4种指标成分的含量测定方法研究[J].中国药房,2015,26(3):381-383.
[18]何春喜,余泽义,何毓敏,等.竹节参总皂苷的大孔吸附树脂纯化与离子交换树脂脱色工艺研究[J].中草药,2017,48(6):1146-1152.
[19]罗春梅,黄志芳,汤依娜,等.附子水溶性生物碱提取纯化工艺研究[J].中草药,2017,48(12):2415-2424.
[20]孙静,刘洁琼,黎伟华,等.陕产黄花油点草总黄酮部位纯化工艺研究[J].中草药,2013,44(10):1275-1279.
[21]于鹤云,刘汉清,刘嘉,等.D-101型大孔吸附树脂纯化黄蜀葵花总黄酮的工艺研究[J].中成药,2014,36(3):520-525.
[22]钟方丽,金龙哲,王晓林,等.大孔吸附树脂纯化黄芪茎总黄酮的工艺及其抗氧化性[J].河南工业大学学报:自然科学版,2017,38(2):88-94.
[23]董双双,袁悦,杨志伟.大孔吸附树脂在黄酮类化合物分离纯化中的应用[J].精细与专用化学品,2016,24(11):29-32.