基于TLC和HPLC建立抗疫新药清肺排毒颗粒质量控制体系

Establishment of quality control system for anti-epidemic new drug Qingfei Paidu Granules based on TLC and HPLC

目的:建立清肺排毒颗粒质量控制体系,为保障制剂质量提供检测方法。方法:对清肺排毒颗粒中主要药材进行薄层色谱法(TLC)考察,确立射干、广藿香、甘草、款冬花4味中药饮片TLC鉴别方法,并进行了薄层条件耐用性考察;确立对石膏进行理化鉴别方法;采用高效液相色谱法(HPLC)测定麻黄中盐酸麻黄碱和盐酸伪麻黄碱及黄芩中黄芩苷3种活性成分的含量;采用HPLC,选用Welch UItimate AQ-C18色谱柱,乙腈-0.2%磷酸水溶液为流动相,梯度洗脱,柱温35℃,检测波长256 nm,建立清肺排毒颗粒HPLC特征图谱方法。结果:清肺排毒颗粒中4味中药饮片的薄层鉴别方法良好,在对照药材相应位置均有显色且斑点清晰,阴性无干扰;盐酸麻黄碱、盐酸伪麻黄碱分别在0.026~0.819μg(r=0.9999)、0.026~0.832μg(r=0.9999)线性良好。盐酸麻黄碱平均回收率为98.03%,RSD值为1.97%,盐酸伪麻黄碱平均回收率为96.43%,RSD值为1.62%;黄芩苷在浓度22.60~226.00μg/mL(r=0.9994)线性良好,平均回收率为103.80%,RSD值为1.02%;特征图谱有12个共有峰,在HPLC条件下均分离良好,并指认了7个成分。结论:本研究建立的方法可用于清肺排毒颗粒的质量控制,此方法稳定、可靠、重复性好,此结果为有效提高清肺排毒颗粒质量控制水平提供了科学依据。

Objective:To establish a quality control system for Qingfei Paidu Granules,and to provide detection methods for ensuring the quality of preparations.Methods:The main medicinal materials in Qingfei Paidu Granules were investigated by TLC,established the method of TLC identification of four traditional Chinese medicine pieces,namely Belamcandae Rhizoma,Pogostemonis Herba,Glycyrrhizae Radix et Rhizoma and Flos Farfarae,and the durability of TLC conditions was investigated.The method of physical and chemical identification of Gypsum Fibrosum was established.HPLC was used to determine the contents of three active components,ephedrine hydrochloride,pseudoephedrine hydrochloride in Ephedrae Herba and baicalin in Scutellariae Radix.Meanwhile,the HPLC characteristic chromatogram method of Qingfei Paidu Granules was established.Welch UItimate AQ-C18 chromatographic column was selected,acetonitrile-0.2%phosphoric acid aqueous solution was used as the mobile phase,gradient elution was performed,the column temperature was 35°C,and the detection wavelength was 256 nm.Results:The thin-layer identification method of the four traditional Chinese medicine pieces in Qingfei Paidu Granules was good,and the corresponding positions of the control medicinal materials were all colored with clear spots,and negative without interference.The linear relationship of ephedrine hydrochloride and pseudoephedrine hydrochloride was good,which were 0.026~0.819µg(r=0.9999)and 0.026~0.832µg(r=0.9999),respectively.The average recovery rate of ephedrine hydrochloride was 98.03%,and the RSD value was 1.97%,and the average recovery rate of pseudoephedrine hydrochloride was 96.43%,the RSD value was 1.62%.Baicalin had a good linearity at the concentration of 22.60~226.00µg/mL(r=0.9994),the average recovery rate was 103.8%,and the RSD value was 1.02%.The characteristic chromatogram had 12 common peaks that were well separated under HPLC conditions and identified 7 components.Conclusion:The established method can be used for the quality control of Qingfei Paidu Granules,which is stable,reliable and repeatable.The results of this study provide a scientific basis for effectively improving the quality control level of Qingfei Paidu Granules.