天然产物研究与开发 ›› 2017, Vol. 29 ›› Issue (8): 1333-1338.doi: 10.16333/j.1001-6880.2017.8.013

• 研究简报 • 上一篇    下一篇

不同采收期水栀子果实中西红花苷I、西红花苷Ⅱ和栀子苷含量变化研究

刘和平1,2,3,许彦1,2,尚强1,2,闵建华1,2,周光雄3*   

  1. 1 国家中药现代化工程技术研究中心;2 丽珠医药集团股份有限公司,珠海 519020 ;3 暨南大学药学院,广州 510632
  • 出版日期:2017-08-28 发布日期:2017-08-28

Content Variations of Crocin I,Crocin II and Gardenoside in Gardenia jasminoides var.grandiflora with Different Harvesting Times

LIU He-ping1,2,3,XU Yan1,2,SHANG Qiang1,2,MIN Jian-hua1,2,ZHOU Guang-xiong3*   

  1. 1 National Engineering Research Center for Modernization of Traditional Chinese Medicine; 2 Livzon Pharmaceutical Group Inc.Zhuhai 519020,China; 3 College of Pharmacy Jinan University,Guangzhou 510632,China
  • Online:2017-08-28 Published:2017-08-28

摘要: 建立水栀子药材中西红花苷Ⅰ、西红花苷Ⅱ超高效液相色谱法(UPLC)含量测定的方法,研究不同采收期的水栀子药材中西红花苷Ⅰ、西红花苷Ⅱ和栀子苷含量的变化趋势。西红花苷Ⅰ、西红花苷Ⅱ含量测定采用80%甲醇超声提取,通过UPLCDAD法测定。色谱条件:Aglient Pro120 ECC18(50 mm×4.6 mm,2.7 μm)色谱柱,以水(A)-乙腈(B)为流动相梯度洗脱,0~5 min,5%~20%B;5~17 min,20%~27%B;柱温15 ℃,流速0.8 mL/min,检测波长 440 nm。栀子苷含测采用《中国药典》2015年版一部栀子项下的含量测定方法检测。通过实验, 红花苷Ⅰ、西红花苷Ⅱ分别在49.5560~955.6000 ng、5.9045~1180.9000 ng线性范围内与各自峰面积呈良好的线性关系(r=0.9996、r=0.9998),平均回收率分别为98.17%、99.67%(n=9)。表明建立的西红花苷Ⅰ、西红花苷Ⅱ含量测定方法简便,稳定性、重复性、分离度均好;随着采收期的延长,样本中西红花苷Ⅰ、西红花苷Ⅱ的含量逐步增加,而栀子苷含量先降低后再逐步增加到一个平衡值。本研究为水栀子药材最佳采收期的确定提供了实验依据。

关键词: 水栀子, 西红花苷Ⅰ, 西红花苷Ⅱ, 栀子苷, UPLC-DAD, 含量测定

Abstract: This research aims to establish an UPLC method for the determination of crocin I and crocin II in Gardenia jasminoides var.grandiflora, and study on content variations of crocin I,crocin II and gardenoside in G.jasminoides var.grandiflora with different harvesting times.The extract from 80% methanol ultrasonic extraction was used to determine the contents of crocinⅠand crocinⅡby UPLC-DAD.System suitability conditions were as follows:column:Agilent Pro120 EC C18 (50 mm×4.6 mm,2.7 μm),mobile phase:water(A)-acetonitrile (B) with gradient elution mode (0-5 min,5%-20%B;5-17 min,20%-27%B),column temperature:15 ℃,flow speech:0.8 mL/min,detection wavelength:440 nm.The content of gardenoside was determined by the method of content determination of G.jasminoides from Chinese Pharmacopoeia (2015 edition).The methodological studies showed that the linear ranges were 49.5560-955.6000 ng (r=0.9995) for crocin I,5.9045-1180.9000 ng (r=0.9997) for crocin II.The average recoveries of crocin I and crocin II were 98.17% and 99.67% (n=9),respectively.It was proved that the method for the determination of crocin I and crocin II was simple,stable,reproducible and well separated.With prolonging of harvesting time,the contents of crocin I and crocin II increased gradually.However,the content of gardenoside decreased firstly and then increased gradually to a balance value.The study provided experimental basis for determining the optimal harvesting time of G.jasminoides var.grandiflora fruits.

Key words: Gardenia jasminoides var.grandiflora, crocin I, crocin II, gardenoside, UPLC-DAD, assay