目的 建立藿香正气滴丸(HZDP)的超快速液相色谱(UFLC)指纹图谱, 为该制剂的质量控制提供参考依据。方法 采用Waters Acquity UPLC BEH C₁₈色谱柱(100 mm×2.1 mm, 1.7 μm);流动相为乙腈-0.2%甲酸水溶液, 梯度洗脱:0～6 min, 10%～15%乙腈;6～9 min, 15%～20%乙腈;9～14 min, 20%～30%乙腈;14～19 min, 30%～50%乙腈;19～21 min, 50%～65%乙腈;21～26 min, 65%～75%乙腈;26～28 min, 75%乙腈;28～30 min, 75%～10%乙腈;30～32 min, 10%乙腈;体积流量为0.4 mL/min;柱温30 ℃;检测波长300 nm。采用中药色谱指纹图谱相似度评价系统软件(2004A版)分析11批HZDP样品。结果 建立了11批HZDP的对照指纹图谱, 确定了18个共有峰;其中13个归属到药材, 6、7、9、10、12号共有峰来源于白芷, 4、5、8号共有峰来源于陈皮, 1、2、11、13号共有峰来源于厚朴, 17号共有峰来源于苍术, 并通过对照品对照法和超快速液相色谱-离子阱-飞行时间串联质谱仪(UFLC-IT-TOF/MS)鉴定了其化学成分。结论 该方法操作简便、准确可靠、重复性好, 可为HZDP的物质基础研究和质量控制提供参考。

Objective To establish the ultra-fast liquid chromatographic (UFLC) fingerprint of Huoxiang Zhengqi Dripping Pill (HZDP) for evaluating the quality of the preparation. Methods The UFLC separation was achieved on an Waters Acquity UPLC BEH C₁₈ column (100 mm × 2.1 mm, 1.7 μm) with acetonitrile (A)-0.2% formic acid solution (B) as mobile phase at the flow rate of 0.4 mL/min by gradient elution of 0—6 min, 10% →15% A, 6—9 min, 15% →20% A, 9—14 min, 20% →30% A, 14—19 min, 30% → 50% A, 19—21 min, 50% →65% A, 21—26 min, 65% →75% A, 26—28 min, 75% A, 28—30 min, 75% →10% A, 30—32 min, 10% A. The column temperature was 30 ℃. The UV detection wavelength was 300 nm. The similarity of 11 batches of HZDP was analyzed with similarity evaluation system for chromatographic fingerprint of tradition Chinese medicine (Version 2004 A). Results Fingerprints of 11 batches of HZDP were established and 18 common peaks were identified, 13 of which belonged to herbs and were identified by the reference substance and UFLC-IT-TOF/MS. Among them, five common peaks (peaks 6, 7, 9, 10, and 12) came from Angelicae Dahuricae Radix, three common peaks (peaks 4, 5, and 8) came from Citri Reticulatae Pericarpium, four common peaks (peak 1, 2, 11, and13) came from Magnoliae Officmalis Cortex, and one common peak (peak 17) came from Atractlodis Rhizoma. Conclusion The method is rapid, accurate, reliable, and reproducible. The established fingerprint could provide the references for the study of substance basis and quality control of HZDP.

国家"十二五"科技重大专项"重大新药创制"资助(2013zx09402202)