基于指纹图谱的银翘解毒颗粒质量评价

Quality Evaluation of Yinqiao Jiedu Granules by HPLC Fingerprint

关键词:  银翘解毒颗粒  指纹图谱  相似度  质量评价

Key words:  Yinqiao Jiedu granules  fingerprint  similarity analysis  quality evaluation

摘要:

目的 采用HPLC建立银翘解毒颗粒指纹图谱，整体评价该制剂质量。方法 采用Waters CORTECS^TM C₁₈色谱柱（4.6 mm×150 mm，2.7 μm），以乙腈为流动相A，0.1%甲酸为流动相B，梯度洗脱，流速为0.5 mL·min^-1，柱温为25℃，检测波长为245 nm；采用LC-MS对银翘解毒颗粒物质基础进行解析并对色谱峰进行归属；运用中药色谱指纹图谱相似度评价系统软件，对28家生产企业的28批样品进行相似度评价。结果 建立了银翘解毒颗粒的HPLC指纹图谱；检测到34个成分，鉴定了其中30个成分，特征峰分别归属于金银花、连翘、牛蒡子、薄荷、荆芥、甘草和淡豆豉7味药；28批样品的相似度值为0.77~0.99。结论 相似度评价结果发现个别企业存在低劣饮片投料或工艺过程控制不严等违规生产现象。建立的指纹图谱方法便捷、特征性强、重复性好，为综合评价和控制产品质量提供了依据。

Abstract:

OBJECTIVE To establish the HPLC fingerprint of Yinqiao Jiedu granules for the quality evaluation and control. METHODS HPLC was performed on a Waters CORTECS^TM C₁₈ column (4.6 mm×150 mm, 2.7 μm) at 25℃. The mobile phase was acetonitrile-water (containing 0.1% formic acid) with gradient elution, with the flow rate as 0.5 mL·min^-1 and the detection wavelength as 245 nm. The characteristic peaks were identified by HPLC/QQQ-MS. Similarity of 28 batches samples from 28 nanufacturing enterprise were evaluated by chromatographic fingerprint similarity evaluation software. RESULTS The fingerprint of Yinqiao Jiedu granules was established and 34 peaks were detected, 30 of them were identified. The detected peaks belonged to Lonicerae Japonicae Flos, Forsythiae Fructus, Arctii Fructus, Menthae Haplocalycis Herba, Schizonepetae Herba, Glycyrrhizae Radix Et Rhizoma and Sojae Semen Praeparatum, respectively. The similarity values of 28 batches samples ranged from 0.77 to 0.99. CONCLUSION Some illegal production phenomena are found with raw materials of poor quality or less amount, and lax process control, etc. The method of fingerprint is simple, specific and reproducible. This study provides the basis of comprehensive evaluation and quality control.