大孔吸附树脂富集纯化番泻豆荚中番泻苷的工艺研究
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摘要
探究大孔吸附树脂富集纯化番泻豆荚中番泻苷的最佳工艺。以番泻豆荚为原料,采用高效液相测定番泻苷A、B含量,以吸附率及解吸率为指标,采用静态吸附试验对5种大孔树脂进行筛选,优选出吸附解吸性能最佳的大孔树脂,并对纯化条件进行优化,确定最佳工艺参数。结果表明:AB-8型树脂对番泻豆荚中番泻苷有较好的吸附及解吸附效果,其最佳工艺为:树脂饱和吸附量按生药计为0.21 g/g,径高比为1∶8,上样流速为1 BV/h,洗脱流速为2 BV/h,以3 BV水除杂,3 BV 30%乙醇洗脱,纯化后产品中番泻苷A、B总含量高达26.05%。结论:AB-8型树脂适合富集纯化番泻豆荚中番泻苷。
To explore the optimal technology for enrichment and purification of sennoside from senna pod with macroporous resin. Methods: The content of sennaside A and B were determined by the HPLC. By using adsorption rate and desorption rate as the indices, five kinds of macroporous resins were screened by the static adsorption test. The best macroporous resin with better adsorption and desorption properties, and the optimal purification conditions of resin were obtained based on static adsorption. Results: Experiment results showed that AB-8 resin possessed high absorption capacity. The best technical parameters were obtained as follows: saturation adsorption capacity of resins 0.21 g/g(equivalent as crude drug), the ratio of diameter to height 1∶8, absorption flow rate 1 BV/h, desorption flow rate 2 BV/h, 3 BV water impurity, eluent with 3 BV 30% ethanol. The total content of sennoside A and B in the purified product were as high as 26.04%. Conclusion: The AB-8 macroporous adsorption resin has the best enrichment and purification efficiency for sennoside from senna pod.
To explore the optimal technology for enrichment and purification of sennoside from senna pod with macroporous resin. Methods: The content of sennaside A and B were determined by the HPLC. By using adsorption rate and desorption rate as the indices, five kinds of macroporous resins were screened by the static adsorption test. The best macroporous resin with better adsorption and desorption properties, and the optimal purification conditions of resin were obtained based on static adsorption. Results: Experiment results showed that AB-8 resin possessed high absorption capacity. The best technical parameters were obtained as follows: saturation adsorption capacity of resins 0.21 g/g(equivalent as crude drug), the ratio of diameter to height 1∶8, absorption flow rate 1 BV/h, desorption flow rate 2 BV/h, 3 BV water impurity, eluent with 3 BV 30% ethanol. The total content of sennoside A and B in the purified product were as high as 26.04%. Conclusion: The AB-8 macroporous adsorption resin has the best enrichment and purification efficiency for sennoside from senna pod.
引文
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[11] 李静,车景超,曲佳,等.寿国香.HPLC法测定番泻豆荚中番泻苷A和番泻苷B[J].中草药,2007(12):1897-1898.
[12] CHEN Y,ZHANG W,ZHAO T,et al.Adsorption properties of macroporous adsorbent resins for separation of anthocyanins from mulberry[J].Food Chemistry,2016,194(1):712-722.
[13] 张阳.大孔吸附树脂分离番泻叶中二蒽酮类化合物的研究[D].天津:天津大学,2006.
[14] 顾燕,薛明,刘萌,等.番泻总苷的纯化工艺研究[J].中成药,2010,32(11):1986-1988.
[15] 仲冉,何珺,徐洋,等.大孔吸附树脂富集纯化罗汉果茎叶中山奈苷的工艺研究[J].食品科技,2018,43 (3):196-200.
[2] DEQUEKERR.Some aspects of the chemical determination of the anthracene constituents of senna leaf and tincture[J].Boll Chim Farm,1962,10(1):290.
[3] 孙森凤,张颖颖.番泻叶成分及药理作用研究进展[J].山东化工,2017,46(13):44-45.
[4] LEMLI J,TOPPET S,CUVEELE J,et al.Naphthalene glycosides in Cassia senna and Cassia angustifolia[J].Planta Medica,1981,43(1):11.
[5] 毕海林,肖裕章,胡军,等.番泻叶的研究概况[J].中国兽医杂志,2017,53(4):108-111.
[6] 张苗,顾燕.HPLC法在测定番泻总苷胶囊中番泻苷AB含量中的应用[J].现代医药卫生,2015,31(21):3235-3237.
[7] 韩雯雯.番泻叶抑菌成分的提取分离与抑菌作用研究[D].呼和浩特:内蒙古农业大学,2012.
[8] 黄娟,张靖,徐文,等.番泻叶提取液中番泻苷A、番泻苷B的稳定性考察[J].中国医院药学杂志,2014,34(10):794-797.
[9] 邵峰,陈慧娟,刘荣华,等.黑顺片总生物碱对番泻叶致小鼠腹泻及大鼠离体小肠平滑肌运动的影响[J].中药材,2013,36(11):1805-1809.
[10] 金施施,牛换云,丁辉,等.正交实验法优化番泻叶的提取工艺[J].天津中医药大学学报,2016,35(2):122-125.
[11] 李静,车景超,曲佳,等.寿国香.HPLC法测定番泻豆荚中番泻苷A和番泻苷B[J].中草药,2007(12):1897-1898.
[12] CHEN Y,ZHANG W,ZHAO T,et al.Adsorption properties of macroporous adsorbent resins for separation of anthocyanins from mulberry[J].Food Chemistry,2016,194(1):712-722.
[13] 张阳.大孔吸附树脂分离番泻叶中二蒽酮类化合物的研究[D].天津:天津大学,2006.
[14] 顾燕,薛明,刘萌,等.番泻总苷的纯化工艺研究[J].中成药,2010,32(11):1986-1988.
[15] 仲冉,何珺,徐洋,等.大孔吸附树脂富集纯化罗汉果茎叶中山奈苷的工艺研究[J].食品科技,2018,43 (3):196-200.