基于UPLC指纹图谱结合化学模式识别的四季三黄丸质量控制研究  

Quality control research of Sijisanhuang pills based on UPLC fingerprint combined with chemical pattern recognition

作　　者：周亚楠 雷蓉 苏建 白洁 刘永利 ZHOU Ya-nan;LEI Rong;SU Jian;BAI Jie;LIU Yong-li(Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050277,China)

机构地区：[1]河北省药品医疗器械检验研究院,石家庄050227

出　　处：《药物分析杂志》2023年第10期1784-1790,共7页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:采用超高效液相色谱法(UPLC法)建立四季三黄丸的指纹图谱,并结合化学模式识别技术对其进行系统、全面和科学的质量评价,为其质量一致性提供依据。方法:采用UPLC仪,Shimadzu Shim-pack gist C18(100 mm×2.1 mm,2μm)色谱柱,流动相为乙腈-0.1%三氟乙酸水溶液,梯度洗脱,检测波长254 nm。建立20批四季三黄丸的指纹图谱并进行相似度分析,结合主成分分析(PCA)、热图聚类分析(CA)对四季三黄丸进行整体质量评价。结果:建立的指纹图谱方法重复性、稳定性RSD均<2%,共标定了16个共有峰,通过对照品比对指认了11个色谱峰(栀子苷、黄芩苷、汉黄芩苷、盐酸小檗碱、黄芩素、芦荟大黄素、大黄酸、汉黄芩素、大黄素、大黄酚、大黄素甲醚)。20批样品同一企业相似度>0.90,不同企业样品间相似度在0.70~0.80。通过CA及PCA分析20批样品聚成2类,表明不同企业及批次药物质量之间存在差异。结论:本实验建立的分析方法准确、可靠且简便易行,采用指纹图谱结合化学模式识别技术可更加系统、全面地评定不同企业不同批次四季三黄丸的质量的一致性,为四季三黄丸的整体质量控制提供理论基础。Objective:To establish the UPLC fingerprint of Sijisanhuang pills and conduct a systemic,comprehensive quality evaluation of the drug using a chemical pattern recognition method.Methods:Ultra-high performance liquid chromatography instrument and Shimadzu Shim-pack gist C_(18)(100 mm×2.1 mm,2μm)chromatographic column was employed,the separation was performed with the mobile phase consisting of acetonitrile and 0.1%trifluoroacetic acid elution,and the detection wavelength was set at 254 nm to establish the UPLC fingerprint of Sijisanhuang pills.Then,the further quality assessment was carried out by similarity evaluation,cluster analysis(CA),principal component analysis(PCA)and orthogonal partial least squares discriminant analysis(OPLS-DA).Results:The method had good repeatability and stability with RSD<2%.Sixteen peaks were recognised as common peaks in the fingerprint.Eleven chromatographic peaks were identified with reference substances,they were geniposide,baicalin,wogonoside,berberine hydrochloride,baicalein,aloe emodin,rhein,wogonin,emodin,chrysophanol,physcion.The similarity values between samples from the same manufacturer were above 0.90.The similarity values between samples from different enterprises ranged from 0.70 to 0.80.Some difference was discovered between the batches of this drug by CA and PCA.Conclusion:The analysis method established in this study is accurate,reliable and simple.The drug quality of Sijisanhuang pills can be evaluated systematically and comprehensively using a fingerprint combined with chemical pattern recognition technique.What's more,it is also suitable for the evaluation of the overall quality of Sijisanhuang pills.

关 键 词：四季三黄丸 超高效液相色谱 指纹图谱 聚类分析 主成分分析 质量评价 栀子苷 黄芩苷 汉黄芩苷 盐酸小檗碱 黄芩素 芦荟大黄素 大黄酸 汉黄芩素 大黄素 大黄酚 大黄素甲醚 

分 类 号：R917[医药卫生—药物分析学]