菊黄口服液质量控制方法研究

Research on quality control method for Juhuang Oral Liquid

目的 对菊黄口服液的质量控制方法 进行研究,建立菊黄口服液定性、定量检测方法 。方法 采用薄层色谱法（TLC）对菊黄口服液方中枸杞子Lyycii Fructus和制黄精PolygonatiRhizoma进行定性分析,苯酚-硫酸法测定菊黄口服液中总多糖的量：并建立RP-HPLC法同时测定菊黄口服液中新绿原酸、绿原酸、隐绿原酸、咖啡酸、木犀草苷、3,4-二咖啡酰奎尼酸、3,5-二咖啡酰奎尼酸、4,5-二咖啡酰奎尼酸8种化学成分的量,采用Odyssil C_（18）色谱柱（250 mm×4.6 mm,5μm）,乙腈-0.05%磷酸水溶液为流动相,梯度洗脱,体积流量1.0 mL/min,检测波长325 nm。结果 TLC鉴别方法 能特征地鉴别枸杞子和制黄精,斑点均清晰,阴性无干扰;总多糖定量测定回归方程A=0.057 8 C＋0.032 5（r=0.999 1,n=8）,线性范围为26.15-196.13 mg/mL,平均加样回收率为99.82%,所测6批样品中总多糖的质量浓度在157.74-166.49 mg/mL：RP-HPLC定量测定时,8种化学成分在测定范围内表现出良好的线性关系（r≥0.999 8）,平均回收率在99.18%-101.06%,RSD在0.79%-1.91%;6个批次样品中8种成分的质量浓度分别为新绿原酸102.9-142.6μg/mL、绿原酸488.6-563.8μg/mL、隐绿原酸58.9-71.6μg/mL、咖啡酸240.7-326.1μg/mL、木犀草苷228.6-302.7μg/mL、3,4-二咖啡酰奎宁酸398.0-485.4μg/mL、3,5-二咖啡酰奎尼酸184.1-203.1μg/mL、4,5-二咖啡酰奎宁酸476.2-561.8μg/mL。结论 TLC鉴别方法 简单易行;总多糖及8种化学成分定量测定的方法 简单、准确、重现性好,可用于菊黄口服液的质量控制。

Objective To establish the quality control method for Juhuang Oral Liquid（JOL） based on the qualitative and quantitative analysis methods.Methods TLC was used to identify Lycii Fructus and Polygonati Rhizoma in JOL.Phenol-sulfuric acid method was used for the detemination of total polysaccharide,HPLC was used to simultaneously determine the contents of neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,coffeic acid,galuteolin,3,4-dicaffeoylquinic acid,3,5-dicaffeoylquinic acid,and4,5-dicaffeoylquinic acid.The Odyssil C_（18）（250 mm× 4.6 mm,5μm） column was used.The mobile phase was acetonitrile-0.05%phosphoric acid solution in gradient elution,at the flow rate of 1.0 mL/min,the detection wavelength was set at 325 nm.Results The identified characteristics of Lycii Fructus and Polygonati Rhizoma by TLC were distinct and the spots were clear,without interference and easy to recognize.When phenol-sulfuric acid method was used to determinate the total polysaccharide content,the regression equation was A = 0.057 8 C ＋ 0.032 5（r = 0.999 1,n = 8）.The linear with its absorbance in the range of 26.15—196.13 mg/mL,the average recoveries was 99.82%.The average content of the total polysaccharide in JOL from six batches is 157.74—166.49 mg/mL.When RP-HPLC was used to determine the eight chemical components,the compounds showed a good linearity（r 0.999 8） in the determination range.The average recoveries were between 99.18%—101.06%with RSDs between 0.79%—1.91%.The average content from the six batches showed neochlorogenic acid 102.9—142.6 μg/mL,chlorogenic acid 488.6 — 563.8 μg/mL,cryptochlorogenic acid 58.9—71.6 μg/mL,coffeic acid 240.7—326.1 μg/mL,galuteolin 228.6—302.7 μg/mL,3,4-dicaffeoylquinic acid398.0—485.4 μg/mL,3,5-dicaffeoylquinic acid 184.1—203.1 μg/mL,and 4,5-dicaffeoylquinic acid 476.2—561.8 μg/mL.Conclusion TLC identification method is simple.The determination method of total polysaccharide and chemical components is simple,accurate,and with a good repeatability.It can be used for the quality control of JOL.