除风益损颗粒质量控制方法研究

Study on the Quality Control Method of Chufeng Yisun Granules

目的:采用薄层色谱法和高效液相色谱法建立除风益损颗粒的质量控制方法。方法:采用薄层色谱法定性鉴别除风益损颗粒中赤芍、牡丹皮、当归、川芎、大黄、防风、女贞子;高效液相色谱法(HPLC)对黄芩中黄芩苷进行含量测定,采用Waters Atlantis d C_(18)(4.6 mm×250 mm,5μm)色谱柱,以甲醇-0.4%磷酸溶液(47∶53)为流动相,检测波长280 nm,流速1.0 mL·min^(-1),柱温25℃,进样量10μL。结果:采用薄层色谱法建立了除风益损颗粒中赤芍、牡丹皮、当归、川芎、大黄、防风、女贞子的定性鉴别方法,斑点清晰,阴性无干扰;采用高效液相色谱法建立了除风益损颗粒中黄芩苷含量测定的方法,专属性强,黄芩苷在0.101~1.01μg(r=0.9997)范围内线性关系良好,平均回收率为100.22%,RSD为0.84%。结论:建立的薄层色谱法鉴别及含量测定方法专属性强、重复性好,可用于除风益损颗粒的质量控制。

Objective:The quality control method of chufeng yisun granules was established by TLC and HPLC.Methods:TLC was used to qualitatively identify the components of Radix Paeoniae Rubra,Moutan Cortex,Angelicae Sinensis Radix,Chuanxiong Rhizoma,Rhei Radix et Rhizoma,Saposhnidoviae Radix,Ligustri Lucidi Fructus in chufeng yisun granules,and the content of baicalin in chufeng yisun granules was determined by HPLC.The Waters Atlantis dC_(18)(4.6 mm×250 mm,5μm)column was used with methanol-0.4%phosphate water(47∶53)as mobile phase.The detection wavelength was 280 nm.The flow rate was 1.0 mL·min^(-1).The column tem-perature was 25℃and the injection volume was 10μL.Results:The qualitative identification methods of Radix Paeoniae Rubra,Mou-tan Cortex,Angelicae Sinensis Radix,Chuanxiong Rhizoma,Rhei Radix et Rhizoma,Saposhnidoviae Radix,Ligustri Lucidi Fructus in chufeng yisun granules were establised by TLC.The TLC chromatography showed the same color spots in the same position of the corre-sponding control drugs,and the negative samples showed no interference.A HPLC method for the determination of baicalin in chufeng yisun granules was established,which is highly specific,and baicalin has a good linear relationship in the range of 0.101~1.01μg(r=0.9997).The average recovery was 100.22%,and RSD was 0.84%.Conclusion:The TLC identification method and the HPLC method for content determination established in this study have strong specificity and good reproducibility,which can be used for the qual-ity control of chufeng yisun granules.