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目的建立血栓心脉宁片(XXT)的UPLC-PDA指纹图谱,考察不同批次XXT质量的一致性,为XXT质量稳定性提供可靠的科学依据。方法样品经甲醇提取,采用Waters Acquity UPLC HSS T3(50 mm×2.1 mm,1.8μm)色谱柱,以乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,190~400 nm波长扫描,体积流量0.5 m L/min,进样量3μL,柱温40℃;对30批XXT样品进行方法学考察、相似度计算和聚类分析;单味药材进行共有峰归属,并通过对照品对共有峰的化学成分进行指认。结果建立了XXT UPLC-PDA指纹图谱,280 nm波长下标定28个共有峰,其中1、10、12~16、18、21~28号峰来自丹参,2~4、6、8、9、17号峰来自川芎,3、7、9、11、16号峰来自毛冬青、5号峰来自槐花,19、20号峰来自蟾酥,经对照品比对指认出4号峰为阿魏酸、5号峰为芦丁、13号峰为丹酚酸B、19号峰为酯蟾毒配基、20号峰为华蟾酥毒基、28号峰为丹参酮IIA;通过聚类分析30批XXT可分为2类,经中药色谱指纹图谱评价软件(2012版)计算得30批XXT相似度均大于0.960。结论建立的XXT UPLC-PDA指纹图谱具有良好的精密度、稳定性和重复性,方法简便可靠,可为进一步完善XXT的质量评价提供参考依据。
OBJECTIVE To establish a UPLC-PDA fingerprint of thrombus Xintang Ning tablets (XXT) and investigate the consistency of XXT quality in different batches so as to provide a reliable scientific basis for the quality stability of XXT. Methods The samples were extracted with methanol and eluted with a Waters Acquity UPLC HSS T3 (50 mm × 2.1 mm, 1.8 μm) column using gradient elution with acetonitrile-0.1% formic acid as mobile phase. The wavelength was scanned at 190-400 nm and the volume flow rate was 0.5 m L / min, the injection volume 3μL, the column temperature 40 ℃; 30 batches of XXT samples for methodological study, similarity calculation and cluster analysis; single herbs common peak assignments, and through the reference substance on the shared peak chemistry Ingredients to be identified. Results The fingerprint of XXT UPLC-PDA was established and 28 common peaks were calibrated at 280 nm. Peaks 1, 10, 12-16, 18 and 21-28 were derived from Salvia miltiorrhiza, 2-4, 8, 8, No. peak from Chuanxiong, 3,7,9,11,16 peak from Mao Dongqing, No. 5 peak from Sophora japonica, No. 19,20 peak from toad, the control identified as No. 4 peak ferulic acid, Peak No. 5 was rutin, peak No. 13 was salvianolic acid B, peak No. 19 was ester topoisoning ligand, peak No. 20 was cinobufacidin and peak No. 28 was tanshinone IIA; Divided into two categories, by the Chinese medicine chromatographic fingerprint evaluation software (2012 version) calculated 30 batches of XXT similarity are greater than 0.960. Conclusion The established fingerprint of XXT UPLC-PDA has good precision, stability and repeatability. The method is simple and reliable, which can provide a reference for further improving the quality evaluation of XXT.