基于HPLC多指标成分含量测定结合化学计量学的小儿康颗粒质量评价

Quality evaluation of Xiao′erkang Granules based on HPLC multi-component quantification analysis and chemometrics analysis

目的建立HPLC多指标成分定量测定与化学计量学相结合的小儿康颗粒质量评价方法。方法以Waters SunFire C 18(250 mm×4.6 mm,5μm)为液相色谱柱,柱温30℃;流动相:乙腈-0.1%磷酸溶液,梯度洗脱,体积流量:1.0 ml/min;检测波长分别为340 nm(牡荆素葡萄糖苷、牡荆素鼠李糖苷和金丝桃苷)、230 nm(氧化芍药苷、芍药苷和苯甲酰芍药苷)和203 nm(太子参环肽B);采用SPSS 26.0统计软件聚类分析、主成分分析等对不同厂家生产的小儿康颗粒进行质量评价。结果牡荆素葡萄糖苷、牡荆素鼠李糖苷、金丝桃苷、氧化芍药苷、芍药苷、苯甲酰芍药苷、太子参环肽B分别在2.18~54.50、15.89~397.25、2.72~68.00、1.39~34.75、12.68~317.00、0.96~24.00、0.79~19.75μg/ml范围内线性关系良好(r≥0.9992);平均加样回收率分别为98.67%、100.11%、97.96%、97.68%、99.64%、96.86%、96.92%,RSD分别为1.48%、0.64%、1.27%、1.32%、0.91%、1.13%和0.87%;12批小儿康颗粒样品聚为3类,主成分分析结果显示,主成分1~3是影响小儿康颗粒质量评价的主要因子。结论该方法操作简便、重复性好,可用于小儿康颗粒的质量控制和综合评价。

Objective To establish a quality evaluation method of Xiao′erkang Granules based on HPLC multi-component quantification analysis and chemometrics analysis.Methods Separation was carried out with the Waters SunFire C18(250 mm×4.6 mm,5μm)as the chromatographic column and with cetonitrile-0.1%phosphoric acid solution as the mobile phase in a gradient elution mode.The column temperature was 30℃,and the flow rate was set at 1.0 ml/min.The detection wavelength was set at 340 nm for vitexin-4”-o-glucoside,vitexin-2′′-o-rhamnoside and hyperoside,230 nm for oxypaeoniflorin,paeoniflorin and benzoylpaeoniflorin,and 203 nm for heterophyllin B.The chemometrics methods such as cluster analysis and principal component analysis by SPSS 26.0 statistical software were used to evaluate the quality of Xiao′erkang Granules from different manufacturers.Results Vitexin-4”-o-glucoside,vitexin-2′′-o-rhamnoside,hyperoside,oxypaeoniflorin,paeoniflorin,benzoylpaeoniflorin and heterophyllin B showed good linear relationships within the ranges of 2.18~54.50,15.89~397.25,2.72~68.00,1.39~34.75,12.68~317.00,0.96~24.00,and 0.79~19.75μg/ml(r≥0.9992),whose average recoveries were 98.67%,100.11%,97.96%,97.68%,99.64%,96.86%and 96.92%with the RSD s being 1.48%,0.64%,1.27%,1.32%,0.91%,1.13%and 0.87%,respectively.The samples of 12 batches of Xiao′erkang Granules could be divided into 3 categories.The results of principal component analysis showed that the principal components 1~3 were the main factors affecting the quality evaluation of Xiao′erkang Granules.Conclusion This method is simple and repeatable,and it can be used in the quality control and comprehensive evaluation of Xiao′erkang Granules.