摘要
目的:建立地榆总皂苷中地榆皂苷-Ⅰ和地榆皂苷-Ⅱ的含量测定方法。方法:以Agilent ODS C_(18)柱(250mm×4.6mm,5μm)分离,流速1.0mL/min,柱温40℃;漂移管温度100℃,气体流速3.0L/min;不分流模式;地榆皂苷-Ⅰ的流动相A为甲醇-乙腈(1∶1),流动B为水,梯度洗脱。地榆皂苷-Ⅱ的流动相A为乙腈,流动B为水,梯度洗脱,测定地榆总皂苷中地榆皂苷-Ⅰ和地榆皂苷-Ⅱ的含量。结果:以该HPLC-ELSD条件进行分析,得到地榆皂苷-Ⅰ和地榆皂苷-Ⅱ分别在0.4104-4.1040μg(r=0.9997)、50.42-10.08μg(r=0.9987)范围内呈良好的线性关系;测得平均回收率分别为100.72%(RSD=1.45%)、96.78%(RSD=1.75%),地榆总皂苷中地榆皂苷-Ⅰ的含量为84.39%-85.75%,地榆皂苷-Ⅱ含量为3.440%-4.483%。结论:HPLC-ELSD法简便、准确、重现性好,可用于地榆总皂苷中地榆皂苷-Ⅰ和地榆皂苷-Ⅱ的含量测定。
Objective: To establish the quantification method for ziyuglycoside-Ⅰ and ziyuglycoside-Ⅱ inburnet total saponins. Methods: The opotimize HPLC-ELSD condition were confirmed for the determination of ziyuglycoside-Ⅰ and ziyuglycoside-Ⅱ in Radix Sanguisorbae respectively: Determination was carried out on Agilent ODS-C_(18)(250mm×4.6mm, 5μm) column, the flow rate maintained was 1.0m L/min. The column temperature was set as 40℃. The temperature of drift tube was 100℃, the flow rate was 3.0L/min for ELSD while adopt by pass mode. For ziyuglycoside-Ⅰ, mobile phase A was methanol-acetonitrile(1∶1) and mobile phase B was ultrapure water, it was eluted according to gradient concentration. For ziyuglycoside-Ⅱ, mobile phase A was acetonitrile and mobile phase B was ultrapure water, it was eluted according to gradienit concentration. The contents of ziyuglycoside-Ⅰ and ziyuglycoside-Ⅱ inburnet total saponins were determined. Results: There was a good linear relationship between the concentration of ziyuglycoside-Ⅰ and ziyuglycoside-Ⅱ, and the peak area value when the concentrations of ziyuglycoside-Ⅰ and ziyuglycoside-Ⅱ were within the ranges of 0.4104-4.1040μg(r=0.9997) and 50.42-10.08μg(r=0.9987), respectively. The average recoveries were 100.72%(RSD=1.45%) and 96.78%(RSD=1.75%), respectively. The contents of ziyuglycoside-Ⅰ was 84.39%-85.75%, and ziyuglycoside-Ⅱ was 3.440%-4.483%. Conclusion: HPLC-ELSD method is simple, rapid, accurate, stable and reproducible, which are suitable for the determination of ziyuglycoside-Ⅰ and ziyuglycoside-Ⅱ in the quality control of burnet total saponins.
出处
《中华中医药杂志》
CAS
CSCD
北大核心
2017年第6期2639-2642,共4页
China Journal of Traditional Chinese Medicine and Pharmacy
基金
国家自然科学基金项目(No.81373976)
国家科技重大专项重大新药创制专项项目(No.2013ZX09103002-013)~~
