安胎丸UPLC指纹图谱及模式识别研究

目的:建立安胎丸的超高效液相指纹图谱分析方法,为评价其质量提供依据。方法:采用UPLC法,色谱柱为Agilent SB-C₁₈(100 mm×2.1 mm,1.8μm);以乙腈-0.4%磷酸水溶液为流动相进行梯度洗脱,体积流量0.3 mL·min^-1;0~2 min检测波长为280 nm,2~8 min检测波长为230 nm,8~9.4 min检测波长为316 nm,9.4~35 min检测波长为280 nm;柱温35℃;进样量2μL。通过相似度评价,结合聚类分析(cluster analysis,CA)、主成分分析(principal component analysis,PCA)及正交偏最小二乘判别分析(orthogonal partial least squares discriminant analysis,OPLS-DA)对12批次安胎丸指纹图谱进行质量评价。结果:标定了安胎丸UPLC指纹图谱的24个共有峰,指认了9个成分:芍药内酯苷、芍药苷、阿魏酸、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、洋川芎内酯A、白术内酯I;12批样品相似度均在0.9以上。通过主成分分析、聚类分析及正交偏最小二乘判别分析,12批样品聚成3类,并发现阿魏酸、黄芩素等差异较大的5个成分。结论:安胎丸的UPLC指纹图谱的构建和化学模式的识别为安胎丸的质量控制提供更全面的参考。

Objective:To establish a UPLC fingerprint of Antai pills for reference of the effective quality control.Methods:The fingerprint of Antai pills was developed with UPLC. The separation was carried out on an Agilent SB-C₁₈ column(100 mm×2.1 mm, 1.8μm) with the mobile phase consisting of acetonitrile and 0.4% phosphoric acid at 0.3 mL·min^-1.The detection wavelength was 280 nm from 0 to 2 min, 230 nm from 2 to 8 min, 316 nm from 8 to 9.4 min and 280 nm from 9.4 to 35 min. The column temperature was 35℃, and the sample volume was 2μL.Similarity evaluation combined with cluster analysis(CA), principal components analysis(PCA) and orthogonal partial least squares discriminant analysis(OPLS-DA) were used to evaluate the fingerprint of 12 batches of Antai pills.Results:The common mode of the fingerprint was set up with 24 common peaks, and 9 of them were identified. The similar degrees of 12 batches of samples were over 0.9, they were albiflorin, paeoniflorin, ferulic acid, baicalin, wogonoside, baicalein, wogonin, senkyunolide A, and atractylenolideⅠ. Totally 12 batches of samples could be classified into three clusters. A brief list of five differential compounds was presented, including ferulic acid and baicalein.Conclusion:The establishment of UPLC fingerprint of Antai pills and the application of chemical pattern recognition can provide a more comprehensive reference for quality control.