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

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

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,2.7μm)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0.8m L/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。

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 crocin Ⅰ and crocin Ⅱ by 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( 0-5min,5%-20% B; 5-17 min,20%-27% B),column temperature: 15 ℃,flow speech: 0. 8 m L/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. 6000ng( 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 crocinⅠ 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.