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引用本文:陈光宇,葛发欢,何群,谢梦洲.工业色谱法纯化山银花中绿原酸的工艺研究[J].中国现代应用药学,2018,35(5):698-703.
CHEN Guangyu,GE Fahuan,HE Qun,XIE Mengzhou.Study of the New Process of the Purification by Industrial Chromatography of Chlorogenic Acid in Lonicera Macranthoides[J].Chin J Mod Appl Pharm(中国现代应用药学),2018,35(5):698-703.
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工业色谱法纯化山银花中绿原酸的工艺研究
陈光宇1,2, 葛发欢2, 何群3,4, 谢梦洲1
1.湖南中医药大学-湖南省药食同源功能性食品工程技术研究中心, 长沙 410208;2.中山大学生命科学学院, 广州 510275;3.中药成药性与制剂制备湖南省重点实验室, 长沙 410208;4.湖南省药学“十二五”重点学科, 长沙 410208
摘要:
目的 探索工业色谱法纯化山银花中绿原酸的最优工艺参数。方法 以绿原酸的转移率为评价指标,以山银花水提液过大孔树脂后的20%乙醇洗脱液为原料液,采用单因素及响应面设计试验,对采用工业色谱纯化山银花中绿原酸工艺中的原料液浓缩程度、固定相类型、流动相乙醇浓度、乙醇流速、进样量等主要工艺参数进行优化,确定了最优工业色谱纯化山银花中绿原酸的工艺条件。结果 工业色谱纯化山银花中绿原酸的最优工艺条件:以60℃,-0.1 MPa为浓缩条件,将原料液浓缩至原体积的0.166 7(1/6),工业色谱UV检测波长为230 nm,以PIPO-02色谱填料为固定相,以18.54%乙醇作为流动相,流速为14.57 mL·min-1,进样量为13.15 mg。该工艺绿原酸的平均转移率为95.49%,RSD=1.91%,绿原酸产品纯度为97.45%,RSD=3.30%。结论 经过工艺优化与验证,创立了一条工业色谱纯化山银花中绿原酸工艺路线,该工艺制备的绿原酸产品纯度>97%,绿原酸转移率高,工艺简单、无毒,溶剂易于回收,适合于山银花中绿原酸纯化的工业化生产。
关键词:  山银花  绿原酸  工业色谱纯化  PIPO-02  CT-25  CT-36
DOI:10.13748/j.cnki.issn1007-7693.2018.05.017
分类号:R284.2
基金项目:
Study of the New Process of the Purification by Industrial Chromatography of Chlorogenic Acid in Lonicera Macranthoides
CHEN Guangyu1,2, GE Fahuan2, HE Qun3,4, XIE Mengzhou1
1.Engineering Center of Medicinal and Edible Functional Food, Hunan University of Chinese Medicine, Changsha 410208, China;2.College of Life Science, Sun Yat-Sen University, Guangzhou 510275, China;3.Druggability of Traditional Chinese Medicine and Preparations, Key Laboratory of Hunan Province, Changsha 410208, China;4.Key Disciplinary of "The 12th Five-Year Plan" of Pharmacy in Hunan Province, Changsha 410208, China
Abstract:
OBJECTIVE To explore the optimal process of the purification by industrial chromatography of chlorogenic acid in Lonicera macranthoides.METHODS The transport rate of chlorogenic acid was used as main assessment index, the eluent of 20% ethanol solution of macroporous resin, which first gained from the water extract solution of Lonicera macranthoides, was used as raw material, single factor and response surface test was adopt to design this test, these main factors, which have effect on the process of the purification by industrial chromatography of chlorogenic acid in Lonicera macranthoides, such as the type of stationary phase, the concentration of ethanol in mobile phase, the flow rate of mobile phase, the sample amount, were optimized. The optimum condition of the process of the purification by industrial chromatography of chlorogenic acid in Lonicera macranthoides was determined.RESULTS The optimum conditions of the process of the purification by industrial chromatography of chlorogenic acid in Lonicera macranthoides were as follows:the condense condition was 60,℃ -0.1 MPa, the volume of raw material should be concentrated to one-sixth of its original volume, the UV determine wavelength of industrial chromatography was 230 nm, the chromatography packing of PIPO-02 was used as the stationary phase, 18.54% ethanol was used as the mobile phase, the flow rate of mobile phase was 14.5 mL·min-1, the sample amount was 13.15 mg. In this process the average data-transfer rate of chlorogenic acid was 95.49% (RSD=1.91%), the purity of product was 97.45% (RSD=3.30%).CONCLUSION A new route of the process of the purification by industrial chromatography of chlorogenic acid from Lonicera macranthoides has been established through optimization and verification experiment. The process, with a high transport rate of chlorogenic acid, is simple, healthy, the solvent is easy to recycle, and the process is suitable for industrialize production of the purification by industrial chromatography of chlorogenic acid in Lonicera macranthoides.
Key words:  Lonicera macranthoides  chlorogenic acid  purification by industrial chromatography  PIPO-02  CT-25  CT-36
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