基于薄层鉴别和多指标成分定量的连豆清脉合剂质量评价

Quality Analysis of Liandou Qingmai Mixture by TLC and Multi-component Quantitation

目的:基于多指标成分含量测定及薄层色谱法建立连豆清脉合剂质量控制方法。方法:采用薄层色谱法鉴别连豆清脉合剂中的连翘、黄连和赤芍;采用高效液相色谱法测定连豆清脉合剂中连翘苷、小檗碱含量,色谱柱为XBridge C18,乙腈-0.6%磷酸水溶液为流动相,流速为0.7 mL·min^(-1),柱温为25℃,检测波长为277 nm。结果:连翘、黄连和赤芍3味中药各色谱图斑点清晰,比移值符合要求,阴性均无干扰;连翘苷、小檗碱质量浓度分别为14.84~148.36、5.72~57.22μg·mL^(-1)(r=0.9993)时与峰面积线性关系良好,平均加样回收率分别为99.07%(RSD为2.75%)、99.86%(RSD为3.60%)。3批样品中连翘苷质量浓度分别为409.63、402.29、378.86μg·mL^(-1),小檗碱质量浓度分别为205.61、201.73、163.02μg·mL^(-1)。结论:所建立的多指标成分含量测定及薄层色谱法科学、有效,可用于连豆清脉合剂的质量控制。

Objective:To establish a comprehensive quality control method for Liandou Qingmai Mixture based on multi-component determination and thin layer chromatography(TLC).Methods:Forsythiae Fructus,Coptidis Rhizoma,and Paeoniae Radix Rubra in Liandou Qingmai Mixture were identified by TLC.The contents of forsythoside and berberine in the mixture were determined by high-performance liquid chromatography(HPLC)using an XBridge C18 column,with acetonitrile-0.6%phosphoric acid aqueous solution as mobile phase at a flow rate of 0.7 mL·min^(-1),column temperature of 25℃,and detection wavelength of 277 nm.Results:The TLC showed clear spots for Forsythiae Fructus,Coptidis Rhizoma,and Paeoniae Radix Rubra with appropriate Rf values and no negative interference.The content determination indicated that forsythoside and berberine had a good linear relationship in the range of 14.84-148.36μg·mL^(-1) and 5.72-57.22μg·mL^(-1)(r=0.9993),respectively,with average recoveries of 99.07%(RSD 2.75%)and 99.86%(RSD 3.60%),respectively.The concentration of forsythoside in the three batches was 409.63,402.29,and 378.86μg·mL^(-1),and that of berberine was 205.61,201.73,and 163.02μg·mL^(-1) separately.Conclusion:The established TLC and HPLC methods for multi-components were scientific and effective and could be used as the quality control standard for Liandou Qingmai Mixture.