基于高分辨质谱物质基础的蓝芩颗粒指纹图谱质量评价研究

Study on Fingerprint Quality Evaluation of Lanqin Granules Based on Orbitrap Ultra-high Resolution Mass Spectrometry

关键词:  蓝芩颗粒  指纹图谱  相似度  物质基础  质量评价

Key words:  Lanqin granules  fingerprint  similarity  material basis  quality evaluation

摘要:

目的 建立蓝芩颗粒的HPLC指纹图谱，整体评价该制剂质量。方法 采用HPLC测定蓝芩颗粒的指纹图谱，采用Waters Xselect HSS T3 C₁₈色谱柱(4.6 mm×150 mm，3.5 μm)，乙腈为流动相A，0.05 mol·L^-1甲酸铵的0.05%甲酸溶液为流动相B，梯度洗脱，流速0.7 mL·min^-1，柱温为35℃，检测波长为254 nm；采用HPLC-Orbitrap-MS/MS对蓝芩颗粒物质基础进行研究并对各色谱峰进行归属；同时应用中药色谱指纹图谱相似度软件，对2家生产企业的54批样品进行相似度评价。结果 建立了蓝芩颗粒的HPLC指纹图谱；鉴定共有峰30个，分别归属于板蓝根、黄芩、栀子、黄柏和胖大海5味药；54批样品的相似度为0.92~0.99，相似度评价结果显示，蓝芩颗粒各企业之间的差异较小，整体质量较高。结论 建立的指纹图谱能快速、特征性地对蓝芩颗粒质量进行综合评价。

Abstract:

OBJECTIVE To establish the HPLC fingerprint of Lanqin granules for the quality evaluation and control. METHODS HPLC fingerprint of Lanqin granules was performed on a Waters Xselect HSS T3 C₁₈ column(4.6 mm×150 mm, 3.5 μm). The mobile phase was acetonitrile(A)-0.05mol·L ^-1 ammonium formate(containing 0.05% formic acid)(B) with gradient elution, with the flow rate of 0.7 mL·min^–1, the column temperature was 35 ℃ and the detection wavelength was 254 nm. The material basis of Lanqin granules was studied and the characteristic peaks were identified by HPLC-Orbitrap-MS/MS. Similarity of 54 batches samples from 2 manufactures were evaluated by chromatographic fingerprint similarity evaluation software. RESULTS The HPLC fingerprint of Lanqin granules was established and 30 common peaks were identified. The detected peaks belonged to Isatidis Radix, Scutellariae Radix, Gardeniae Fructus, Phellodendri Chinensis Cortex and Sterculiae Lychnophorae Semen, respectively. The similarity values of 54 batches samples ranged from 0.92 to 0.99. Similarity evaluation results showed that the difference between enterprises was small, the overall quality was good. CONCLUSION The established fingerprint can quickly and characteristic comprehensively evaluate the quality of Lanqin granules.