摘要
目的:建立同时测定虎杖药材中虎杖苷、白藜芦醇、蒽苷B、大黄素和大黄素甲醚5种活性成分含量的微波萃取与超高效液相色谱(UPLC)分析方法,为完善虎杖的质量标准提供科学依据。方法:采用MDS-8型多通量密闭微波化学工作站,以甲醇为溶剂,160℃微波萃取制备供试品溶液;UPLC分析条件为Waters Acquity H Class UPLC系统,BEH C18色谱柱(2.1mm×100 mm,1.7μm),乙腈-水为流动相,梯度洗脱,流速0.5 mL.min-1,柱温30℃,检测波长226 nm。结果:5种活性成分采用微波萃取10 min可提取完全;经UPLC分析可在12 min内完全分离,且在线性范围内均呈良好的线性关系(r≥0.999 6),平均加样回收率为97.00%～103.7%(n=6),RSD≤2.2%。16个产地的虎杖药材中,每种被测成分的批次间含量差异都比较大,但5种成分的总量相对稳定(3.683 3%～7.103 1%)。结论:微波萃取-UPLC法同时测定虎杖中多个活性成分的含量,方法快捷、分离效果及重现性好,可以用于虎杖的质量控制与评价。
Objective： To establish a microwave extraction and UPLC method for simultaneous determination of polydatin, res- veratrol, anthraglycoside B, emodin and physicion contained in Polygoni Cuspidati Rhizoma et Radix, in order to provide scientific ba- sis for improving quality standards of Polygoni Cuspidati Rhizoma et Radix. Method： The test solutions were prepared in a MDS-8 closed microwave system at 160 ℃ with methanol as the solvent. The UPLC analysis was performed in a Waters Acquity UPLC system. A BEH C18 column （2. 1 mm ×100 ram, 1.7μm） was adopted for gradient elution with acetonitrile and water as the mobile phase. The temperature of column was 30 ℃, and the detection wavelength was 226 nm. Result： The five active components can be complete- ly extracted in 10 minutes and separated completely in 12 minutes according to UPLC analysis, with a good linearity （r≥0. 999 6） within the linear ranges. The average recovery rate was 97.00% -103.7% with RSD≤〈2. 2%. Despite a large difference in content a- mong tested components from Polygoni Cuspidati Rhizoma et Radix, the total content of the five major constituents was relatiely stable （3. 683 3%-7. 103 1% ）. Conclusion： The microwave extraction-ultra performance liquid chromatography method in simultaneous de- termination for contents of five major bioactive components contained in polygoni cuspidati rhizoma et radix is so rapid and highly repro- ducible that it can be used for quality control and assessment of Polygoni Cuspidati Rhizoma et Radix.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2012年第13期1994-1997,共4页
China Journal of Chinese Materia Medica
基金
2010年版<中国药典>国家药品标准提高研究项目(369)
关键词
虎杖
微波萃取
UPLC
含量测定
Polygoni Cuspidati Rhizoma et Radix
microwave extraction
UPLC
determination
