基于一测多评法的急支糖浆质量评价方法的建立及验证

Establishment and verification of quality evaluation method of Jizhi Syrup based on quantitative analysis of multi-components by single marker

基于高效液相色谱的紫外多波长检测系统,建立一种急支糖浆的一测多评法,同时测定盐酸麻黄碱、原儿茶酸、新绿原酸、对羟基苯甲酸、柚皮苷、新橙皮苷、甘草酸和白花前胡甲素的含量,并验证其在急支糖浆质量评价中的可行性。分别在210、254、280、320 nm波长下,以柚皮苷为内参物,建立与其他7个成分的相对校正因子和待测色谱峰定位方法,并进行系统耐用性考察以及与外标法含量测定结果的对比,验证一测多评法的准确性和可行性。结果表明,急支糖浆中盐酸麻黄碱、原儿茶酸、新绿原酸、对羟基苯甲酸、新橙皮苷、甘草酸和白花前胡甲素相对于柚皮苷的相对校正因子分别为0.846、0.582、0.608、0.293、0.913、2.207、0.940,在不同实验条件下耐用性良好,一测多评法和外标法对15批样品的含量测定结果无显著差异。所检测的8个成分中,除原儿茶酸和新绿原酸外其余均为单味药材的专属性成分,且甘草酸和白花前胡甲素是首次在急支糖浆中检测出,弥补了甘草、前胡药材无成分检出的空白。该研究所建立的一测多评法便捷高效、专属性强、准确可靠,可以全面有效地评价急支糖浆的质量,确保临床使用安全有效。

A quantitative analysis of multi-components by single marker(QAMS)method was established for the simultaneous determination of ephedrine hydrochloride,protocatechuic acid,5-caffeoylquinic acid,4-hydroxybenzoic acid,naringin,neohesperidin,glycyrrhizic acid,and praeruptorin A in Jizhi Syrup by high performance liquid chromatography(HPLC)with ultraviolet multi-wavelength detection system,and its feasibility in quality evaluation of Jizhi syrup was verified.With naringin as the internal reference substance,the relative correction factors and chromatographic peak localization methods of other seven components were respectively established at 210,254,280,and 320 nm.The method reproducibility was validated,and the result of QAMS were compared with those obtained by the external standard method(ESM)to verify the accuracy and feasibility of the method.The relative correction factors of ephedrine hydrochloride,protocatechuic acid,5-caffeoylquinic acid,4-hydroxybenzoic acid,neohesperidin,glycyrrhizic acid,and praeruptorin A with naringin as reference were 0.846,0.582,0.608,0.293,0.913,2.207,and 0.940,respectively,which presented excellent reproducibility under different experimental conditions.Furthermore,QAMS and ESM showed no significant difference in the results for 15 batches of samples.Except protocatechuic acid and 5-caffeoylquinic acid,other six compounds were the exclusive components of single medicinal materials.In addition,glycyrrhizic acid and praeruptorin A were identified in the Jizhi Syrup for the first time,filling up the blank of no component detected in Glycyrrhizae Radix et Rhizoma and Peucedani Radix.The method established in this study is convenient,efficient,specific,accurate,and reliable,which can comprehensively and effectively evaluate the quality of Jizhi Syrup to ensure the safety and efficacy of this drug in clinical application.