基于HPLC-Q-TOF-MS、指纹图谱和含量测定的精气神口服液质量评价研究

郑超; 石德志; 汤志锋; 张云羽; 钟绍辉; 肖莲莲; 刘华兰; 廖楠汐; 嵇晶; 郑云枫; 程建明

doi:10.14148/j.issn.1672-0482.2023.0860

基于HPLC-Q-TOF-MS、指纹图谱和含量测定的精气神口服液质量评价研究

Study on Quality Evaluation of Jingqishen Oral Liquid Based on HPLC-Q-TOF-MS, Fingerprint and Content Determination

摘要

摘要:
目的建立精气神口服液HPLC-ELSD指纹图谱及其活性成分的含量测定方法。
方法采用HPLC-Q-TOF-MS技术对精气神口服液化学成分进行分析, 应用相似度评价对数据进行研究。采用Agilent TC-C₁₈(250 mm×4.6 mm, 5 μm)色谱柱, 以乙腈(A)-水溶液(B)为流动相进行梯度洗脱, 建立精气神口服液HPLC-ELSD指纹图谱并进行含量测定。
结果 HPLC-Q-TOF-MS共鉴定出75个化合物；通过10批样品HPLC-ELSD指纹图谱标定了14个共有峰, 通过对照品比对, 共指认了斯皮诺素、酸枣仁皂苷A、人参皂苷Rg₁、人参皂苷Re、人参皂苷Rb₁、人参皂苷Rd、人参皂苷Rf、人参皂苷Rg₃8个色谱峰。为进一步控制口服液的整体质量, 选取其中斯皮诺素、人参皂苷Rg₁、人参皂苷Re和人参皂苷Rb₁4个活性成分, 进行含量测定, 各活性成分线性关系良好, 建立的方法灵敏度高，稳定性和准确度良好。
结论建立的含量测定与指纹图谱同时测定的方法准确、稳定, 可全面评价与控制精气神口服液的质量。

Abstract:
OBJECTIVE To establish HPLC-ELSD fingerprint of Jingqishen (JQS) oral liquid and the content determination method of its active ingredients.
METHODS An Agilent TC-C₁₈ (250 mm×4.6 mm, 5 μm) chromatographic column was used, and acetonitrile (A)-water solution (B) was adopted as the mobile phase for gradient elution to establish the HPLC-ELSD fingerprint of JQS oral liquid. The chemical composition of JQS oral liquid was analyzed by HPLC-Q-TOF-MS technology. The similarity evaluation was applied to study the data.
RESULTS A total of 75 compounds were identified, and 14 common peaks were calibrated by the fingerprint of 10 samples. Through comparison with reference standards, a total of 8 chromatographic peaks were identified: Spinosin, Jujuboside A, Ginsenoside Rg₁, Ginsenoside Re, Ginsenoside Rb₁, Ginsenoside Rd, Ginsenoside Rf, Ginsenoside Rg₃ were identified. In order to further control the overall quality of oral liquid, 4 active ingredients, Spinosin, Ginsenoside Rg₁, Ginsenoside Re and Ginsenoside Rb₁, were selected for content determination. Each active ingredient had a good linear relationship, and the established method had high sensitivity, good stability and accuracy.
CONCLUSION The methods of content determination and fingerprint measurement established in this study are accurate and stable, and they control the quality of the JQS oral liquid comprehensively.

HTML全文

参考文献(20)

施引文献

资源附件(0)