银黄滴丸HPLC指纹图谱研究

Study on HPLC fingerprint of Yinhuang Drop Pills

目的利用HPLC法建立银黄滴丸的指纹图谱。方法采用色谱柱Kromasil 100-5C18(250 mm×4.6 mm,5μm),柱温30℃,流动相为乙腈-0.4%磷酸溶液,进行梯度洗脱,检测波长为327 nm;通过《中药色谱指纹图谱相似度评价软件》(2012)对10批银黄滴丸的指纹图谱进行了相似度计算;通过药材对照对共有峰进行归属;通过对照品对照指认共有峰。结果银黄滴丸HPLC指纹图谱有7个共有峰,6个共有峰(峰1、2、3、4、5、6)来自于金银花药材,1个共有峰(峰7)来自黄芩药材;通过对照品比对,指认了7个成分,分别为新绿原酸(峰1)、绿原酸(峰2)、隐绿原酸(峰3)、3,4-O-二咖啡酰奎宁酸(峰4)、3,5-O-二咖啡酰奎宁酸(峰5)、4,5-O-二咖啡酰奎宁酸(峰6)、黄芩苷(峰7);10批样品相似度均大于0.9。结论建立的指纹图谱具有良好的精密度、重复性和稳定性,可以很好地控制药品质量。

Objective To establish the specific chromatogram of Yinhuang Drop Pills（YDP） by High performance liquid chromatography. Methods The chromatographic column Kromasil 100-5C18（250 mm × 4.6 mm, 5 μm） was used, acetonitrile-0.4% phosphoric acid as mobile phase with gradient elution, and the detection wavelength was 372 nm. Through similarity evaluation software, the similarity of specific chromatogram of 10 batches YDP were calculated. Results The HPLC specific chromatogram of YDP showed 7 common peaks, of which 6 peaks（neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, 3,4-O-dicaffeoylquinic acid, 3,5-O-dicaffeoylquinic acid, and 4,5-O-dicaffeoylquinic acid） from Lonicerae Flos, 1 common peaks（baicalin） from Scutellariae Radix; By comparing with the reference substances, identified 7 components, respectively, the neochlorogenic acid（peak 1）, chlorogenic acid（peak 2）, cryptochlorogenic acid（peak 3）, 3,4-O-dicaffeoylquinic acid（peak 4）, 3,5-O-dicaffeoylquinic acid（peak 5）, 4,5-O-dicaffeoylquinic acid（peak 6）, baicalin（peak 7）. By the methodology validation, verified that this method has good precision, repeatability and stability, 10 batches of sample similarity is greater than 0.9. Conclusion This method was available for the quality control of YDP.