超高效液相色谱法测定五子衍宗丸中五味子甲素的含量

摘要

目的 建立五子衍宗丸中五味子甲素含量测定的超高效液相色谱法(UPLC),并比较不同溶剂对五味子甲素的提取效果. 方法 色谱柱:Waters ACQUITY UPLC BEH C18(2.1 mm× 100 mm,1.7 μm);流动相ACN∶0.2％ HAc =49∶51;流速0.4 ml/min,柱温30℃,进样体积1μl,检测波长250 nm. 结果五味子甲素在0.001 3-0.05 μg范围内具有良好的线性关系(r =0.999 9);平均回收率为101.73％,RSD为2.29％;70℃蒸馏水、常温蒸馏水、70％乙醇、无水乙醇和DMSO 5种溶剂提取五味子甲素得率分别为,0.013％,0.012％,0.008％,0％和0％. 结论UPLC简便、准确、重现性好,可用于五子衍宗丸中五味子甲素的含量测定.%Objective To establish the method for determining the content of deoxyschizandrin in Wuzi Yanzong pills by ultra performance liquid chromatography(UPLC) and compare the efficacy of extraction of deoxyschizandrin with different solvents.Methods The analysis was carried out on Waters ACQUITY UPLC BEH C18 (2.1 mm × 100 mm,1.7 μm) with ethanol-0.2％ glacial acetic acid (49∶51) as mobile phase,flow rate of 0.4 ml/min and wave length of 250 nm at 30 ℃.The 70％ ethanol,100％ ethanol,DMSO,70 ℃ distilled water and distilled water at room temperature were used as the solvents to extract the deoxyschizandrin.Results The deoxyschizandrin showed a good linear relationship between concentration and peak area in the range of 0.001 3-0.05 μg (r =0.999 9).The recovery was 101.73％ with RSD of 2.29％.The extraction rates of 70％ ethanol,100％ ethanol,DMSO,70 ℃ distilled water and distilled water at room temperature were 0.013％,0.012％,0.008％,0％ and 0％.Conclusion The method has good reproducibility and sensitivity to determine the content of deoxyschizandrin in Wuzi Yanzong pills.The 70％ ethanol is the best extraction solvent.