清肺咳合剂薄层鉴别及甘草苷含量测定方法的研究

Study on Thin Layer Identification and Determination of Glycyrrhizin Content of Qingfei Ke Mixture

目的:建立清肺咳合剂的薄层鉴别和含量测定方法,以提升制剂的质量标准。方法:采用TLC法定性鉴别制剂中的鱼腥草、甘草流浸膏;采用UPLC法测定制剂中甘草苷的含量,色谱柱为Acquity HSS T3色谱柱(2.1×100 mm,1.8μm),流动相为甲醇0.5%冰乙酸溶液梯度洗脱,柱温35℃,进样体积5μL,流速为0.25 mL/min,检测波长为276 nm。结果:制剂中鱼腥草、甘草流浸膏的TLC特征斑点显色清晰,分离度良好,阴性对照无干扰。甘草苷在1.90~95.1μg/mL浓度范围内与峰面积线性关系良好(r=0.9995,n=6);精密度、稳定性、重复性试验的RSD均小于3.0%;平均加样回收率为96.1%,相应的RSD为1.2%。对8批样品中甘草苷的含量进行测定,结果为51.0~70.7μg/mL。结论:该方法操作简便、结果稳定可靠、专属性和重复性均较好,可用于清肺咳合剂的质量标准提升。

Objective To establish a TLC identification and content determination method for Qingfeike Mixture to improve the quality standard of the preparation.Methods TLC was used to qualitatively identify the Houttuynia cordata and liquorice extracts in the preparation.UPLC was used to determine the content of liquiritin in the preparation.The chromatographic column was Acquity HSS T3 column(2.1×100 mm,1.8μm),the mobile phase was methanol-0.5%glacial acetic acid solution gradient elution,the column temperature was 35°C,the sample volume was 5μL,the flow rate was 0.25 mL/min,and the detection wavelength was 276 nm.Results The TLC characteristic spots of Houttuynia cordata and liquorice extracts in the preparation showed clear color development,good resolution,and no interference from negative controls.The content of liquiritin was determined to be 1.90-95.1μg/mL.The linear relationship between the concentration range of 0.05-1.00 g/mL and the peak area was good(r=0.9995,n=6);the RSDs of precision,stability,and repeatability tests were all less than 3.0%;the average recovery rate was 96.1%,and the corresponding RSD was 1.2%.The content of liquiritin in 8 batches of samples was determined to be 51.0-70.7μg/mL.Conclusion This method is simple to operate,the results are stable and reliable,and the specificity and repeatability are good.It can be used to improve the quality standard of Qingfeike Mixture.