用HPLC指纹图谱对复方丹参片的信息质量控制研究

Information quality control of compound Salvia Miltrorrhiza tablets by HPLC fingerprints

目的采用双定性双定量相似度等46个参数作为评价的信息参量,以建立复方丹参片(CSMTs)HPLC指纹图谱的信息质量控制方法。方法采用反相HPLC法以Century SIL C18BDS柱(200 mm×4.6 mm,5μm);以1%醋酸水-1%醋酸甲醇为流动相梯度洗脱,紫外检测波长290 nm,柱温(30.00±0.15)℃,进样量5μL。以双定性相似度为参量通过对20批CSMTs进行系统聚类分析确定用其中10批生成CSMT对照指纹图谱(RFP),以此RFP为标准计算20批CSMTs的双定性双定量相似度,据此进行宏观定性定量质量评价;以色谱指纹图谱指数F等42个信息参量进行信息质量特征评价。结果以丹酚酸B(SAB)为参照物峰,确定40个指纹峰,建立了CSMTs的HPLC指纹图谱。用双定性和双定量相似度评价8批样品的化学成分数量、分布比例和含量都合格,5批双定性相似度不合格,其他7批含量都明显偏低。结论在OTC中随机选择的20批CSMTs,用HPLC指纹图谱鉴定完全合格品8批,双定性相似度不合格品5批及双定量相似度不合格品7批。因此所建立的CSMTs的HPLC指纹图谱可用于CSMTs生产质量控制。本研究证明用中药色谱指纹图谱技术结合多变量参数控制中药复方制剂质量的信息质量控制方法可行且准确可靠。

Objective To establish an information quality control of Compound Salvia Miltrorrhiza Tablets （CSMTs） by HPLC fingerprints using 46 parameters such as dual qualitative and dual quantitative similarities as assessment parameters. Methods CFPs were determined by injecting 5 μL of the sample solution each time on a CenturySIL C18 BDS column （200 mm×4. 6 mm, 5 μm） with the gradient elution solvent system composing of 1% acetic acid water and 1% acetic acid methanol. The flow rate was 1 mL · min^- 1, the column temperature was maintained at （30. 00 ± 0.15） C, and the signals were acquired at 290 nm. The referential fingerprint （RFP） was produced in terms of the average model of 10 batches of CSMTs, according to the result of hierarchical clustering analysis using dual qualitative similarities and dual quantitative similarities （DQDQS） as variables. The whole 20 batches of CSMTs were evaluated by the values of DQDQS, respectively, and the 42 information parameters such as the CFP index F and so on. Results The CFPs containing 40 co-possessing peaks were obtained by choosing salvianolic acid B peak as the reference peak. The chemical component quantity, the chemical constituents distribution, and the total content of the chemical components in 8 batches of CSMTs were completely qualified, while the dual qualitative similarities of 5 batches were unqualified and the contents of 7 batches were relatively low. Conclusion Among the 20 batches of CSMTs randomly brought from drugstores, 8 batches were qualified, 5 batches were unqualified in dual qualitative similarities and the other 7 batches were unqualified in dual quantitative similarities. This new HPLC method with good precision and reproducibility can be applied in the quality control of CSMTs. The information quality control of traditional Chinese medicine using the fingerprint chromatogram combined with multi-dimentional information parameters is feasible and reliable.