微波萃取-UPLC同时测定虎杖中5种主要活性成分的含量

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,1.7 μm),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.

Simultaneous determination of contents of five major bioactive components contained in Polygoni Cuspidati Rhizoma et Radix by microwave extraction-ultra performance liquid chromatography

Objective: To establish a microwave extraction and UPLC method for simultaneous determination of polydatin,resveratrol,anthraglycoside B,emodin and physicion contained in Polygoni Cuspidati Rhizoma et Radix,in order to provide scientific basis 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 mm,1.7 μm) 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 completely 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 among 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 determination for contents of five major bioactive components contained in polygoni cuspidati rhizoma et radix is so rapid and highly reproducible that it can be used for quality control and assessment of Polygoni Cuspidati Rhizoma et Radix.