香卿止痛喷雾剂指纹图谱建立及指标成分含量测定研究

Fingerprint establishment and determination of index components in Xiangqing Zhitong spray

目的建立香卿止痛喷雾剂UPLC指纹图谱和HPLC含量测定方法,结合化学模式识别分析,为其质量评价提供依据。方法采用Waters CORTECS T3色谱柱(4.6 mm×50 mm,2.7μm),以0.1%磷酸水溶液-甲醇为流动相,梯度洗脱,检测波长220 nm,流速1.0 mL·min^(-1),柱温25℃,建立10批香卿止痛喷雾剂指纹图谱并计算相似度,采用SIMCA软件进行主成分分析和正交偏最小二乘法判别分析。采用Agilent 5 TC-C18(2)色谱柱(4.6 mm×250mm,5μm),以1%冰醋酸水溶液-甲醇为流动相,梯度洗脱,检测波长274 nm,流速1.0m L·min^(-1),柱温25℃,建立丹皮酚、槲皮苷含量测定方法。结果建立了香卿止痛喷雾剂的共有模式指纹图谱,标定19个共有峰,指认了丹皮酚、槲皮苷2个成分,10批样品相似度均大于0.99,化学模式识别分析得到丹皮酚等3个质量差异标志物,含量测定结果显示槲皮苷为3.932~4.168 mg·mL^(-1),丹皮酚为1.973~2.403 mg·mL^(-1),批次间差异趋势与化学模式识别分析结果一致。结论所建指纹图谱和含量测定方法简便可靠,可为香卿止痛喷雾剂的全面质量评价和生产过程质量控制提供参考。

Objective To establish the UPLC fingerprint and HPLC content determination of Xiangqing Zhitong spray,and combine with chemical pattern recognition to provide basis for its quality evaluation.Methods The UPLC fingerprint was performed on a Waters CORTECS T3 column(4.6 mm×50 mm,2.7μm)with 0.1%phosphoric acid solution-methanol as the mobile phase in a gradient elution mode.The detection wavelength was 220 nm,the flow rate was 1.0 mL·min^(-1) and the column temperature was 25℃.The fingerprints of 10 batches of Xiangqing Zhitong spray were established and the similarity was evaluated.SIMCA software was used for principal component analysis and orthogonal partial least squares discriminant analysis.The index components were determined on an Agilent 5 TC-C18(2)column(4.6 mm×250 mm,5μm)with 1%glacial acetic acid-methanol as the mobile phase in a gradient elution mode.The detection wavelength was 274 nm,the flow rate was 1.0 mL·min^(-1),and the column temperature was 25℃.Results The common pattern fingerprint of Xiangqing Zhitong spray was established.Totally 19 common peaks were marked,and two components were identified as paeonol and quercetin.The similarity of 10 batches of samples was higher than 0.99.Three quality difference markers,including paeonol,were obtained by chemical pattern recognition.The content of quercetin was 3.932~4.168 mg·mL^(-1),and paeonol was 1.973~2.403 mg·mL^(-1).The difference between batches was consistent with the results of chemical pattern analysis.Conclusion The fingerprint and content determination methods are simple and reliable,which can provide reference for the overall quality evaluation control of Xiangqing Zhitong spray.