目的 研究细梗香草总皂苷壳聚糖絮凝纯化工艺，为继续纯化三萜皂苷B(LC-B)和三萜皂苷C(LC-C)奠定基础。方法 用可见分光光度法、高效液相色谱-蒸发光散射检测法(HPLC-ELSD)，分别测定总皂苷中间体水溶液絮凝率、总皂苷损失率，以絮凝率和总皂苷损失率为指标，用正交实验优选壳聚糖絮凝纯化最佳工艺条件。结果 最佳工艺条件为总皂苷质量浓度为0.6 mg·mL-1， 每100 mL总皂苷水溶液加入壳聚糖溶液30 mL，絮凝温度60 ℃，絮凝时间4 h。验证结果表明，总皂苷中间体水溶液澄清率为47.81%，总皂苷损失率为9.53%。结论 与传统除鞣质工艺相比，壳聚糖絮凝纯化工艺能有效保留有效成分，工艺稳定性好，适合工业化生产。
Abstract
OBJECTIVE To study the flocculation process of the total saponins intermediate solution of Lysimachia capillipes Hemsl. with chitosan and lay the foundation for separation of the total saponins monomer components by medium pressure column. METHODS Visible spectrophotometry and HPLC-ELSD were used to respectively determine the flocculation rate and total saponins loss rate as two main parameters to estimate the effects of influencing factors on flocculation. The optimum conditions of chitosan flocculation were determined by orthogonal test. RESULTS The optimum conditions were as follows: aqueous solution concentration of 0.6 mg·mL-1, chitosan solution volume of 30 mL per 100 mL intermediate solution, flocculation temperature of 60 ℃, and flocculation time of 4 h. Under these conditions, a flocculation rate of 47.81% and a total saponins loss rate of 9.53% were achieved. CONCLUSION Compared with traditional tannin removing process, chitosan flocculation purification process can effectively retain the active ingredients in the solution and has good process stability, which is suitable for industrial production.
关键词
细梗香草 /
总皂苷 /
三萜皂苷B /
三萜皂苷C /
壳聚糖 /
高效液相色谱-蒸发光散射检测法
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Key words
Lysimachia capillipes Hemsl. /
total saponin /
capilliposide B /
capilliposide C /
chitosan /
HPLC-ELSD
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中图分类号：
R284
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参考文献
TIAN J K,ZOU Z M,XU L Z,et al. Studies on chemical constituents of Lysimachia cgoillipes. Chin Pharm J(中国中药杂志),2006,31(3):171-173. XIE C,XU L Z,ZHAO B H,et al. Studies on chemical constituents of hairystalk loosestrife (Lysimachia cgoillipes). Chin Tradit Herb Drugs(中草药),2000,32(2):81-83. YING H M. Study on the extraction and purification process of total saponins in Lysimachia cgoillipes Hemsl. and the establishment of quality standards.Hangzhou;Zhejiang University,2011:20-51. XU Y, RONG Y M,LIU X B,et al.Experimental studies on anti-tumor effects of Capilliposide.Chin Pharmacol Bull(中国药理学通报),2012,28(4):545-548. XIE J,LIU X J,ZHU X Y,et al. Application of chitosan flocculation method in clarification of water extract from Stevia rebaudiana Bertoni leaves and flocculation mechanism analysis.Food Sci(食品科学),2011,20(1):1-5. ZHANG J W ,FAN H W. Purification extraction of water-extraction solution of Ginkgo leaves with chitosan. Chin Tradit Pat Med (中成药),2008,30(4) : 511-515. WANG J,XU Z S,MAO H L. Explore the traditional Chinese medicine injection tannin removal method. Primary J Chin Mater Med(基层中药杂志) ,2001,15(5):51-52. WANG J F,LI H,ZHANG Z W. Study on chitosan coagulation method used in clarifying decoction of Radix et Caulis Acanthopanacis Senticosi. Chin Tradit Pat Med (中成药),2001,23(10) : 707-710. ZHANG Z G, KANG Y,FENG Y,et al. Application of flocculation technology in the purification of chinese traditional medicine.Chem Ind Eng(化学工业与工程),2003,20(6):377-384.
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脚注
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基金
新药创制国家科技重大专项资助(2012ZX09102201-10)
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