| 摘要: |
| 目的 基于超高效液相色谱-电喷雾检测器（UPLC-CAD）建立痰热清胶囊特征图谱和多成分同时定量的整合分析方法，为优化其质量标准提供参考。方法 采用Hypersil GOLD（2.1mm×100mm,3μm）色谱柱，以乙腈-0.1%甲酸水溶液为流动相，梯度洗脱，流速0.2mL·min-1，柱温30℃，进样量5μL。CAD雾化器温度35℃，采集频率5Hz，过滤常数5.0s。采用UPLC-CAD建立痰热清胶囊的特征图谱，结合相似度评价、主成分分析对10批痰热清胶囊进行质量评价。同时以连翘酯苷A、黄芩苷、连翘苷、胆酸、熊去氧胆酸、鹅去氧胆酸及去氧胆酸7个活性成分为指标，建立其含量测定方法。结果 痰热清胶囊的UPLC-CAD特征图谱共标定了47个共有特征峰，相似度均在0.970以上。经对照品比对指认出9个化学成分。定量分析的7个成分在各自浓度范围内呈良好的线性关系，r值在0.9991～0.9998之间，平均加样回收率（n=6）为96.94%～100.23%，RSD为1.33%～2.62%。10批样品中连翘酯苷A、黄芩苷、连翘苷、胆酸、熊去氧胆酸、鹅去氧胆酸及去氧胆酸的含量分别为10.40～13.40、171.26～186.94、3.54～4.47、3.77～5.25、154.74～168.64、88.71～96.70、10.21～11.50mg·g-1。主成分分析结果显示：主成分1～9是影响痰热清胶囊质量评价的主要因子。结论 本研究建立的UPLC特征图谱和多指标成分含量同时测定方法准确、简单，专属性强，重复性好，能较全面地反映该制剂的内在质量，可用于有效地评价痰热清胶囊的质量。 |
| 关键词: 痰热清胶囊 特征图谱 含量测定 UPLC-CAD 质量评价 |
| DOI：10.13748/j.cnki.issn1007-7693.20232821 |
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| 基金项目: |
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| Quality evaluation of Tanreqing capsules based on UPLC-CAD Characteristic Chromatogram and quantitative analysis of multi-components |
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liuyue, fengsuxiang
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Henan University of Chinese Medicine
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| Abstract: |
| ABSTRACT: OBJECTIVE To establish an integrated analytical method based on ultra performance liquid chromatography with electrospray detector (UPLC-CAD) for the characterization of Tanreqing capsules with simultaneous quantification of multiple components in order to provide a reference for optimizing their quality standards. METHODS A Hypersil GOLD (2.1mm×100mm, 3μm) column was used with acetonitrile-0.1% formic acid aqueous solution as the mobile phase, gradient elution, the flow rate was 0.2mL·min-1, the column temperature was 30℃, the injection volume was 5μL. The CAD atomizing chamber temperature was 35℃, the acquisition frequency was 5Hz, and the filter was 5.0s. The UPLC-CAD was used to establish the characteristic chromatogram of Tanreqing capsules. The quality of the 10 batches of Tanreqing capsules was evaluated by UPLC-CAD, combined with similarity evaluation and principal component analysis. At the same time, the seven active ingredients, forsythoside A, baicalin, phillyrin, cholic acid, ursodiol, chenodeoxycholic acid and deoxycholic acid, were used as indicators to establish their content determination methods. RESULTS The UPLC-CAD characteristic chromatogram of Tanreqing capsules was established, and forty-seven common peaks were identified, all with similarity above 0.970. nine of the chemical components were identified by comparison with the reference substance. seven components analyzed quantitatively had good linear relationship in the range of mass concentration, with r values were 0.9991-0.9998, and the average recoveries (n=6) were 96.94%-100.23% with the RSDs of 1.33%-2.62%. The concentrations of 10 batches of samples of forsythoside A, baicalin, phillyrin, cholic acid, ursodiol, chenodeoxycholic acid and deoxycholic acid, were 10.40～13.40、171.26～186.94、3.54～4.47、3.77～5.25、154.74～168.64、88.77～96.70、10.21～11.50 mg·g-1, respectively, and the results of principal component analysis showed that the principal components 1-9 were the main factor affecting the quality evaluation of Tanreqing capsules. CONCLUSION The quality of the different batches of Tanreqing capsules is consistent. The established UPLC characterization chromatogram and the simultaneous determination of the multi-indicator component content are accurate, simple, specific and reproducible, which can reflect the intrinsic quality of the preparation more comprehensively and can be used to effectively evaluate the quality of the Tanreqing capsules. |
| Key words: Tanreqing capsules Characteristic chromatogram content determination UPLC-CAD quality evaluation |
