Key Lab of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian, 116023, Liaoning, China.
University of Chinese Academy of Sciences, Beijing, 100049, China.
Anal Bioanal Chem. 2020 Oct;412(26):7073-7083. doi: 10.1007/s00216-020-02841-z. Epub 2020 Aug 18.
A model consisting of quantitative fingerprinting integrated with fundamental statistical analysis was established to carry out quality control analysis of Shuang-huang-lian (SHL) oral liquid. The quantitative fingerprinting approach was developed by systematic investigation of the chromatographic condition and optimization of a gradient using a complex sample analysis software system (CSASS). Five pivotal components from three traditional Chinese medicines of SHL oral liquid were determined at dual wavelengths, including phillyrin, baicalin, chlorogenic acid, neochlorogenic acid and cryptochlorogenic acid. Among them, neochlorogenic acid and cryptochlorogenic acid were quantified by quantitative analysis of multi-components with a single marker (QAMS) method. Further, the developed quantitative fingerprinting approach was validated. Good linearity with correlation coefficients (R) higher than 0.9999 were achieved for phillyrin, baicalin and chlorogenic acid. Recoveries of the three analytes were between 96% and 108%. Relative standard deviation (RSD) values were below 3% regarding the stability and intra-day and inter-day precision. Besides, the feasibility of the QAMS method was verified by an external standard method (ESM) using 18 batches of SHL oral liquid. Fifty-nine batches of SHL oral liquid from nine manufacturers were then analyzed. Effective distinction was realized based on a linear principal component analysis (linear-PCA) model by the combination of the quantitative data and chromatographic fingerprinting. The linear-PCA model based on quantitative chromatographic fingerprinting exhibited great advantage over conventional similarity analysis to distinguish between different samples. The strategy provided a particularly simple and effective approach for quality evaluation of SHL oral liquid from various manufacturers. Graphical abstract.
建立了一个由定量指纹图谱与基本统计分析相结合的模型，用于对双黄连口服液进行质量控制分析。该定量指纹图谱方法通过系统研究色谱条件和使用复杂样品分析软件系统（CSASS）优化梯度来开发。在双波长下测定了双黄连口服液三种中药的五个关键成分，包括连翘酯苷、黄芩苷、绿原酸、新绿原酸和隐绿原酸。其中，新绿原酸和隐绿原酸通过定量分析多成分单一标志物（QAMS）方法进行定量。进一步验证了所建立的定量指纹图谱方法。连翘酯苷、黄芩苷和绿原酸均具有良好的线性关系，相关系数（R）均高于 0.9999。三种分析物的回收率在 96%至 108%之间。稳定性、日内和日间精密度的相对标准偏差（RSD）值均低于 3%。此外，通过使用 18 批双黄连口服液的外标法（ESM）验证了 QAMS 方法的可行性。然后对来自九个制造商的 59 批双黄连口服液进行了分析。通过定量数据和色谱指纹图谱的结合，基于线性主成分分析（linear-PCA）模型实现了有效的区分。基于定量色谱指纹图谱的线性 PCA 模型在区分不同样品方面优于传统的相似性分析，具有很大的优势。该策略为来自不同制造商的双黄连口服液的质量评价提供了一种特别简单有效的方法。
