摘要
芪苓制剂超微粉用甲醇提取,固相萃取小柱纯化,40%甲醇淋洗,60%甲醇洗脱后收集洗脱液.色谱条件:色谱柱ZORBAX SB-C18(4.6 mm×150 mm,5μm),流动相为甲醇-乙腈-水(30∶30∶40),流速1.0 mL.min-1,检测波长220 nm,柱温30℃.结果显示,白术内酯Ⅲ含量为0.77-27.02μg.mL-1时呈良好的线性关系(r2=0.9989),检测限为3.86 ng.mL-1,平均回收率为93.05%,RSD为4.04%.
A high performance liquid chromatography(HPLC) method for determination of Actractylenolide Ⅲ in Qiling preparation ultra micro powder was established.Medicament of Qiling ultra micro powder was extracted with methanol,purified by solid-phase extraction,rinsed with 40%,eluted with 60% methanol,then concentrated.The optimal conditions for separation and detection were achieved on a C18 analytical column with an mobile phase consisted of methanol-acetonitrile-water(30∶30∶40) at the flow-rate of 1 mL·min-1.The detection wavelength was 220 nm.The column temperature was maintained at 30 ℃.The result indicated that the calibration curves for Actractylenolide Ⅲ were linear in the range of 0.77-27.02 μg·mL-1(r2=0.9989),and the limit of quantification was 3.86 ng·mL-1.The recovery was 93.05% with RSD 4.04%.
出处
《福建农林大学学报(自然科学版)》
CSCD
北大核心
2010年第3期286-289,共4页
Journal of Fujian Agriculture and Forestry University:Natural Science Edition
基金
福建省科技厅重大项目(2006NZ0003-1)
福建省教育厅资助项目(JA08068)
关键词
芪苓制剂超微粉
高效液相色谱
白术内酯Ⅲ
固相萃取
medicament of Qiling ultra micro powder
high performance liquid chromatography
Atractylenolide Ⅲ
solid-phase extraction