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0.8mL/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 ～955.6000ng、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 Prol20 EC-C1s (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 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.
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