基于指纹图谱和含量测定评价脑得生丸的质量

Quality assessment of Naodesheng pills based on fingerprint and content determination

目的:以高效液相色谱(HPLC)指纹图谱结合含量测定方法,为科学评价脑得生丸的质量提供理论依据。方法:采用HPLC建立脑得生丸的指纹图谱,色谱柱为Inertsil ODS-SP(4.6 mm×250 mm,5μm);流动相为乙腈-0.1%甲酸溶液,梯度洗脱;柱温30℃;检测波长为254 nm;流速为1 ml/min。采用HPLC方法测定脑得生丸中人参皂苷Rg1,色谱柱为Hypersil ODS2(4.6 mm×250 mm,5μm);流动相为乙腈-0.05%磷酸(19∶81),等度洗脱;检测波长为203 nm;流速为1.0 ml/min;进样量为10μl。基于指纹图谱和含量测定结果,对脑得生丸的质量进行评价。结果:建立了脑得生丸的指纹图谱,确定了11个共有峰,15批脑得生丸样品相似度均大于0.97。人参皂苷Rg1的线性方程为y=13600x-9.5581,线性范围是19.2μg/ml^1.920 mg/ml,相关系数是0.9992。15批脑得生丸中有5批样品为过期产品,仅批次为161003样品(过期5个月)含量检测不合格,其他均符合质量标准要求。结论:该方法简便、准确、重复性好,为脑得生丸质量的有效评价与整体控制提供了实验依据。

Objective: To investigate the value of high-performance liquid chromatography(HPLC) fingerprint combined with content determination in the quality assessment of Naodesheng pills,and to provide a theoretical basis for the scientific quality assessment of Naodesheng pills.Methods: HPLC was used to establish the fingerprint of Naodesheng pills on an Inertsil ODS-SP column(4.6 mm×250 mm,5 μm) with a mobile phase of acetonitrile-0.1% formic acid for gradient elution at a column temperature of 30℃,a detection wavelength of 254 nm,and a flow rate of 1 ml/min.HPLC was used to measure the level of ginsenoside Rg1 in Naodesheng pills on a HypersilODS2 column(4.6 mm × 250 mm,5 μm) with a mobile phase of acetonitrile-0.05% phosphoric acid(19 ∶81) for isocratic elution at a detection wavelength of 203 nm,a flow rate of 1 ml/min,and a sample size of 10 μl.The quality of Naodesheng pills was assessed based on the results of fingerprint and content determination.Results: The fingerprint of Naodesheng pills was established,with a total of11 common peaks identified,and 15 batches of Naodesheng pills had a similarity of >0.97.Ginsenoside Rg1 had a linear equation of y = 13600 x-9.5581,with a linear range of 19.2 μg/ml to 1.920 mg/ml and a correlation coefficient of0.9992.Among the 15 batches of Naodesheng pills,5 were expired products,and only the batch 161003(expired for5 months) was tested unqualified;the other batches met the quality standard.Conclusion: This method is simple and accurate with good repeatability and provides an experimental basis for the quality assessment and overall quality control of Naodesheng pills.