首页|基于指纹图谱及化学计量分析和多成分检测的银菊合剂的质量控制

基于指纹图谱及化学计量分析和多成分检测的银菊合剂的质量控制

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建立银菊合剂的高效液相指纹图谱,并测定不同批次间有效成分(绿原酸、木犀草素及甘草素)的含量,为银菊合剂的质量控制提供参考.采用Agilent C18色谱柱,选择乙腈和0.1%磷酸水溶液作为流动相,进行梯度洗脱分析;设定流速为1.0 mL/min;保持柱温在30 ℃;以327 nm作为检测波长;样品进样量为10μL.建立10批银菊合剂的高效液相指纹图谱,进行相似度评价和化学计量学分析,同时测定绿原酸、木犀草素及甘草素的含量.建立了 10批银菊合剂的高效液相色谱(HPLC)指纹图谱,共标定出 11个共有峰,相似度均大于0.95,指认出其中3个成分进行质量浓度测定,绿原酸质量浓度为825.68~850.17 μg/mL,甘草素质量浓度为17.31~24.02 μg/mL,木犀草素质量浓度为34.31~34.98μg/mL.聚类分析和主成分分析均将10批银菊合剂大致分为3类,峰1、峰2(绿原酸)及峰4的变量重要性投影值均大于1,其中峰1对主成分1影响较大,峰2(绿原酸)对主成分2影响较大,峰3对主成分3影响较大.将色谱共有峰峰面积作为变量,通过偏最小二乘判别分析(OPLS-DA)进行模型构建.RX2为0.727,Q2为0.51,均超过0.5,显示该模型具有良好的稳定性和可靠性,对照品指认的绿原酸、甘草素和木犀草素可作为潜在质量标志物.研究构建的指纹图谱及多成分含量测定方法稳定可靠、简便快捷,可用于银菊合剂的质量控制.
Quality Control Research on Yinju Mixture Based on Fingerprint Spectrum Combined with Chemometrics Analysis and Multi-component Content Determination
To establish the HPLC fingerprint of Yinju mixture and determine the contents of active components(chl orogenic acid,luteolin and glycyrrhizin)in different batches,so as to provide a reference for the quality control of Yinju mixture.Agilent C18 column was utilized,apply-ing a gradient elution with a mobile phase of acetonitrile and a 0.1%phosphoric acid solution;the flow rate was set at 1 mL/min;the column temperature was 30 ℃;the detection wavelength was 327 nm;and the injection volume was 10 μL.The HPLC fingerprint was established for 10 batches of Yinju Mixture,with similarity evaluation and chemometric analysis conducted,alongside the determination of the contents of chloro-genic acid,luteolin,and glycyrrhizic acid.A total of 11 common peaks were identified,all with similarities greater than 0.95,and the contents of three components were quantified:chlorogenic acid ranging from 825.68 to 850.17 μg/mL,glycyrrhizic acid from 17.31 to 24.02 µg/mL,and luteolin from 34.31 to 34.98 μg/mL.Cluster analysis and principal component analysis categorized the 10 batches of Yinju Mixture into three general groups.The variable importance in the projection(VIP)values for peak 1,peak 2(chlorogenic acid),and peak 4 all exceeded 1,indicating a significant influence on the respective principal components,particularly peak 1 on the first,peak 2 on the second,and peak 3 on the third.An orthogonal partial least squares-discriminant analysis(OPLS-DA)model was constructed using the common peak areas as varia-bles,with RX2 at 0.727 and Q2 at 0.5 1,both exceeding 0.5,indicating that the model has good stability and reliability.The identified stand-ards of chlorogenic acid,glycyrrhizic acid,and luteolin are potential quality markers.The fingerprint and multi-component content determina-tion methods established in this study are stable and reliable,simple and fast,and can be used for the quality control of Yinju Mixture.

Yinju MixtureFingerprintsStoichiometryContent DeterminationQuality MarkerQuality Control

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庆阳市中医医院 制剂室,甘肃 庆阳 745000

银菊合剂 指纹图谱 化学计量学 含量测定 质量标志物 质量控制

2024

云南化工
云南省化工研究院 云天化集团有限责任公司 云南煤化工集团有限公司 云南省化学化工学会

云南化工

影响因子:0.272
ISSN:1004-275X
年,卷(期):2024.51(12)