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林产化学与工业 ›› 2014, Vol. 34 ›› Issue (4): 37-41.doi: 10.3969/j.issn.0253-2417.2014.04.007

• 研究报告 • 上一篇    下一篇

中心复合设计法优化熊果酸和齐墩果酸的HPLC测试条件

邢雅丽1, 毕良武1,2, 赵振东1,2, 韩路路1, 夏田娟1   

  1. 1. 中国林业科学研究院 林产化学工业研究所;生物质化学利用国家工程实验室;国家林业局 林产化学工程重点开放性实验室;江苏省生物质能源与材料重点实验室, 江苏 南京 210042;
    2. 中国林业科学研究院 林业新技术研究所, 北京 100091
  • 收稿日期:2013-05-16 出版日期:2014-08-25 发布日期:2015-08-18
  • 作者简介:邢雅丽(1987-),女,河南南阳人,硕士生,从事天然产物化学与利用研究;E-mail:xyl0416@126.com
  • 基金资助:
    国家林业局948技术引进项目(2011-4-01)

Optimization of the HPLC Condition of Ursolic Acid and Oleanolic Acid by Central Composite Design

XING Ya-li1, BI Liang-wu1,2, ZHAO Zhen-dong1,2, HAN Lu-lu1, XIA Tian-juan1   

  1. 1. Institute of Chemical Industry of Forest Products, CAF;National Engineering Lab. for Biomass Chemical Utilization;Key and Open Lab. of Forest Chemical Engineering, SFA;Key Lab. of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China;
    2. Research Institute of Forestry New Technology, CAF, Beijing 100091, China
  • Received:2013-05-16 Online:2014-08-25 Published:2015-08-18
  • Contact: 毕良武,研究员,博士生导师,从事天然产物化学与利用研究;E-mail:biliangwu@126.com。 E-mail:biliangwu@126.com

摘要: 在考察HPLC流动相体系和色谱柱对熊果酸、齐墩果酸分离测定影响的基础上,采用中心复合设计,以分离度和分析时间为响应值,对熊果酸和齐墩果酸HPLC分离测定的主要影响因素(甲醇与水相的体积比、水相中磷酸的体积分数、流动相流速及柱温)进行多重响应优化,建立了有效、快速的分离测定熊果酸和齐墩果酸的HPLC方法。结果表明,在 210 nm 的检测波长下,用Shim-pack ODS-CLC(M)色谱柱,流动相为甲醇/磷酸水溶液体系,甲醇与水体积比为91.7:8.3,磷酸体积分数为 0.05%,流速为 0.6 mL/min,柱温为 21℃,齐墩果酸和熊果酸可以在 23 min 内得到有效分离,分离度达到1.739。

关键词: 中心复合设计, 高效液相色谱, 熊果酸, 齐墩果酸

Abstract: Effects of HPLC mobile phase and column on the separation and determination of ursolic acid and oleanolic acid were in vestigated. By using the resolution and the analysis time as response values, the main influencing factors of HPLC(the volumetric ratio of methanol and aqueous phase in the mobile phase, the volume fraction of phosphoric acid in the aqueous phase, as well as the flow rate of the mobile phase and the column temperature) were optimized by central composite design. An effective and fast method for the separation and determination of ursolic acid and oleanolic acid by HPLC was established. The results showed that oleanolic acid and ursolic acid were effectively separated within 23 min with the resolution of 1.739, when the chromatographic separation was performed on a Shim-pack ODS-CLC (M) column kept at 21℃, using the methanol and aqueous phase containing 0.05% phosphoric acid with the volumetric ratio of 91.7:8.3 as the mobile phase at a flow rate of 0.6 mL/min, and the detection wavelength was set at 210 nm.

Key words: central composite design, HPLC, ursolic acid, oleanolic acid

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