高效液相色谱法同时测定参术止带糖浆中4个有效成分  

Simultaneous determination of four active ingredients in Shenzhu Zhidai Syrup by HPLC

作　　者：马灵珍 何胜利 张贇[3] 凌今[4,5] 

机构地区：[1]亳州职业技术学院药学院,安徽亳州236800 [2]遂成药业股份有限公司,河南新郑451150 [3]上海中医药大学附属龙华医院,上海200032 [4]复旦大学药学院,上海201203 [5]浙江金华广福医院,浙江金华321001

出　　处：《中成药》2015年第11期2422-2426,共5页Chinese Traditional Patent Medicine

基　　金：安徽省高等学校教学质量与教学改革工程实测中心建设项目(20101460)

摘　　要：目的建立高效液相色谱法测定参术止带糖浆（山药、车前子、党参、苍术、陈皮等）中尿囊素、薯蓣皂苷元、京尼平苷酸、毛蕊花糖苷4个有效成分的含有量。方法参术止带糖浆70%甲醇提取液分析采用依利特C18色谱柱（4.6 mm×200 mm,5μm）;以甲醇-乙腈（3∶2）与0.5%冰醋酸溶液为流动相,梯度洗脱;体积流量为0.9m L/min;柱温为室温;检测波长分别为224 nm（尿囊素）、210 nm（薯蓣皂苷元）和254 nm（京尼平苷酸和毛蕊花糖苷）。结果尿囊素在0.085 4~1.708 0μg（r=0.999 8）、薯蓣皂苷元在0.010 6~0.212 0μg（r=0.999 2）、京尼平苷酸在0.095 8~1.916 0μg（r=0.999 5）、毛蕊花糖苷在0.145 2~2.904 0μg（r=0.999 7）范围内线性关系良好;平均加样回收率（n=6）分别为98.4%、97.5%、97.9%、98.6%,RSD为0.69%~1.1%。结论暂定本品每1 m L含山药以尿囊素计不得低于0.35 mg,以薯蓣皂苷元计不得低于0.040 mg;含车前子以京尼平苷酸计不得低于0.38 mg,以毛蕊花糖苷计不得低于0.60 mg。AIM To develop a high-performance liquid chromatography（ HPLC） method for simultaneously determining the contents of four main ingredients（ allantoin,diosgenin,geniposidic acid and verbascoside） in Shenzhu Zhidai Syrup（ Dioscoreae Rhizoma,Plantaginis Semen,Codonopsis Radix,Atractylodis Rhizoma,Citri reticulatae Pericarpium,etc.）. METHODS A Hypersil C18 column was used for chromatographic separation of70% methanolic extract of Shenzhu Zhidai Syrup. The mobile phase consisted of methanol-acetonitrile（ 3 ∶ 2） and0. 5% glacial acetic acid solution in a gradient elution manner,with the column maintained at room temperature,the flow rate at 0. 9 m L / min,and the detection wavelengths were set at 224 nm for allantoin,210 nm for diosgenin,and 254 nm for geniposidic acid and verbascoside. RESULTS There were good linear relationships among allantoin,diosgenin,geniposidic acid and verbascoside,and the peak area values with their concentrations kept within the ranges of 0. 085 4- 1. 708 0 μg（ r = 0. 999 8）,0. 010 6- 0. 212 0 μg（ r = 0. 999 2）,0. 095 8-1. 916 0 μg（ r = 0. 999 5） and 0. 145 2- 2. 904 0 μg（ r = 0. 999 7）,respectively. The average recoveries were98. 4%,97. 5%,97. 9% and 98. 6%,respectively,with RSD of 0. 69%- 1. 1%. CONCLUSIONS The tentative standard for each 1 m L is fixed at least no less than 0. 35 mg allantoin and 0. 040 mg diesgenin of Dioscoreae Rhizoma,0. 38 mg geniposidie acid and 0. 60 mg verbascoside of Plantaginis Semen.

关 键 词：参术止带糖浆 尿囊素 薯蓣皂苷元 京尼平苷酸 毛蕊花糖苷 高效液相色谱 

分 类 号：R927.2[医药卫生—药学]