越鞠胶囊中香附、栀子TLC鉴别和栀子苷含量测定研究

目的:建立越鞠胶囊中香附、栀子的TLC定性鉴别法和栀子苷的高效液相色谱含量测定法。方法;以α-香附酮为对照品,采用正己烷-醋酸乙酯(9:1)为展开剂,在UV254nm下检视,和以栀子苷为对照品,采用氯仿-甲醇(3:1)为展开剂,香草醛硫酸试液为显色剂,分别对越鞠胶囊中香附和栀子进行薄层色谱法定性鉴别。采用Hpersil C_(18)柱(4.6mm×250mm,5μm),甲醇-水(25:75)为流动相,在238nm检测波长下,以HPLC法测定了越鞠胶囊中栀子苷的含量。结果:越鞠胶囊薄层色谱中,α-香附酮和栀子苷斑点清晰,阴性对照无干扰,并改进了药典中定性鉴别方法的某些缺陷。HPLC定量分析中,栀子苷线性范围为 0.30～1.50 μg(r=1.000),平均回收率为103.6％,RSD=1.0％。方法灵敏度高,结果准确,重现性好。结论:分析方法简便可行,可用于该制剂的质量控制。

TLC Identification for Rhizoma Cyperi and Fructus Gardeniae and the Quantitative Analysis of Geniposide by HPLC in Yueju Capsules

Objective:To develop the TLC identification for Rhizoma Cyperi and Fructus Gardeniae and the quantitative analysis of geniposide by HPLC in Yueju capsules. Methods:Rhizoma Cyperi and Fructus Gardeniae were i-dentified by TLC,respectively,using a -cyperone and geniposide as reference substansces, and hexane -acetate(9 : 1) and chloroform - methanol (3:1 ) as mobile phases. Geniposide contents were determined by HPLC using the ODS reversed -phase column of Hypersil C18(4. 6 mm x250 mm,5 um) ,the mobile phase was a combination of methanol and water (25:75) at the flow rate of 1. 0 mL . min-1 ,and the eluate was monitored with UV absorption at 238 nm. Results: The TLC chromatograms of a -cyperone and geniposide were of clearness, good separation, and nointerference. The geniposide contents in Yueju capsules were determined by HPLC,in the linear range of 0. 30 to 1.50ug(r = 1.000)and the recoveries of 103. 6% (RSD = 1. 0% ). Conclusions:The developed TLC identification for Rhizoma Cyperi and Fructus Gardeniae have some advantages over those described in Chinese Pharmacopoeia. The HPLC analysis of geniposide in Yueju capsules is of good accuracy, reproducibility and practice .