目的 建立一测多评(QAMS)与指纹图谱结合的方法评价丹红化瘀口服液(Danhong Huayu Oral Solution,DHOS)。方法 采用Waters XBridge C₁₈色谱柱(250 mm×4.6 mm,5 μm),以乙腈-0.5%甲酸水溶液进行梯度洗脱,柱温30℃,检测波长286 nm,体积流量1 mL/min。结果 建立了DHOS HPLC指纹图谱,确定了18个共有峰,并指认了其中丹参素钠、原儿茶醛、丹酚酸D、柚皮苷、橙皮苷、新橙皮苷、丹酚酸B、丹酚酸A共8个共有峰。通过相似度评价、主成分分析对10批DHOS HPLC指纹图谱进行综合分析,10批制剂的相似度计算均大于0.9,找到影响指纹图谱的主要成分为丹酚酸A、丹酚酸D等。以新橙皮苷为内参物,建立了可同时测定DHOS中丹参素钠、原儿茶醛、丹酚酸D、柚皮苷、丹酚酸B含量的一测多评法,6种主要成分QAMS法与外标法的测定结果间无显著差异,10批DHOS中丹参素钠、原儿茶醛、丹酚酸D、柚皮苷、新橙皮苷、丹酚酸B质量浓度分别为3.853 2~4.390 4、0.264 0~0.425 7、0.560 7~0.855 0、0.889 2~1.797 8、0.754 2~1.091 8、0.178 2~0.382 4 mg/mL。结论 建立DHOS的HPLC指纹图谱评价方法和一测多评含量测定法,为DHOS提供了切实可行的整体质量评价方法。

Objective To establish a comprehensive assessment system for Danhong Huayu Oral Solution (丹红化瘀口服液, DHOS) through integrating quantitative analysis of multi-components by single-marker (QAMS) and fingerprint. Methods HPLC analysis was performed on a Waters XBridge C₁₈ (250 mm × 4.6 mm, 5 μm) column, eluted at 30℃ with acetonitrile-0.5% formic acid aqueous solution as mobile phase in gradient elution. The detection wavelength was 286 nm and the flow rate was 1 mL/min. Results The fingerprint of DHOS was established, 18 common peaks were calibrated. Eight common peaks were identified, including sodium danshensu, protocatechualdehyde, salvianolic acid D, naringin, hesperidin, neohesperidin, salvianolic acid B and salvianolic acid A. The fingerprints of 10 batches of DHOS were comprehensively analyzed with similarity evaluation and principal component analysis, leading to the results that the similarity of 10 batches of preparations was greater than 0.9, and the main components affecting the fingerprint were identified as salvianolic acid A and salvianolic acid D. Furthermore, by using the neohesperidin as internal reference standard, QAMS was established to determine the contents of sodium danshensu, protocatechualdehyde, salvianolic acid D, naringin and salvianolic acid B in DHOS. And there was no significant difference between the quantitative results of external standard method (ESM) and QAMS method. Contents of the six main components above were 3.853 2-4.390 4, 0.264 0-0.425 7, 0.560 7-0.855 0, 0.889 2-1.797 8, 0.754 2-1.091 8, 0.178 2-0.382 4 mg/mL, respectively. Conclusion The fingerprint and the QAMS method of DHOS were established in this study, which will provide a feasible method to evaluate the quality of DHOS.

R283.6

国家药典委员会药品标准制修订—丹红化瘀口服液质量标准提升（2019Z012）；广州市科学技术协会2019年“广州市院士专家工作站”建设项目资助（600180）