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    基于UPLC-CAD指纹图谱和多成分含量测定的痰热清胶囊质量评价

    Quality Evaluation of Tanreqing Capsules Based on UPLC-CAD Fingerprint and of Multi-Component Content Determination

      摘要
    • 摘要:
      目的  基于超高效液相色谱-电喷雾检测器(UPLC-CAD)建立痰热清胶囊指纹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(2.1 mm×100 mm, 3 µm)色谱柱，以乙腈-0.1%甲酸水溶液为流动相，梯度洗脱，流量0.2 mL·min−1，柱温30 ℃，进样量5 μL。CAD雾化器温度35 ℃，采集频率5 Hz，过滤常数5.0 s。采用UPLC-CAD建立痰热清胶囊的指纹图谱，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指纹图谱共标定了47个共有峰，相似度均>0.970。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，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、10.21~11.50 mg·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指纹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，可有效地评价痰热清胶囊的质量。

       

      Abstract:
      OBJECTIVE  To establish an integrated analytical method of fingerprints and simultaneous quantification of multiple components to provide a reference for optimizing their quality standards based on ultra performance liquid chromatography with electrospray detector(UPLC-CAD).
      METHODS  A Hypersil GOLD(2.1 mm×100 mm, 3 µm) column was used with acetonitrile-0.1% formic acid aqueous solution as the mobile phase, gradient elution, the flow rate was 0.2 mL·min−1, the column temperature was 30 ℃, the injection volume was 5 μL. The CAD atomizing chamber temperature was 35 ℃, the acquisition frequency was 5 Hz, and the filter was 5.0 s. The UPLC-CAD was used to establish the fingerprints 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 fingerprints of Tanreqing capsules identified 47 common characteristic peaks with similarity values above 0.970. Nine chemical components were identified by comparison with the reference substance. The seven components for quantitative analysis showed good linearity in their respective concentration ranges, with r values were 0.9991−0.999 8. The average recovery rates(n=6) were 96.94%−100.23%, with RSDs of 1.33%−2.62%. The contents of forsythoside A, baicalin, phillyrin, cholic acid, ursodiol, chenodeoxycholic acid and deoxycholic acid in the 10 batches of samples 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. Principal component analysis showed that the first to ninth principal components were the main factors affecting the quality evaluation of Tanreqing capsules.
      CONCLUSION  The established UPLC fingerprint and the simultaneous determination of the multi-indicator component content are accurate, simple, specific and reproducible, which can effectively evaluate the quality of Tanreqing capsules.

       

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