论文部分内容阅读
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,1.7μm);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 m L/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 ultra-fast liquid chromatography (UFLC) fingerprints of Huxiang Zhengqi Dropping Pills (HZDP) to provide a reference for the quality control of this preparation. Methods Waters Acquity UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm) was used. The mobile phase was acetonitrile-0.2% formic acid aqueous solution. The gradient elution was 0-6 min, 10-15% acetonitrile and 6-9 min , 15% -20% acetonitrile, 9-14 min, 20-30% acetonitrile, 14-19 min, 30-50% acetonitrile, 19-21 min, 50-65% acetonitrile, 21-26 min, 65 % To 75% acetonitrile, 26 to 28 min, 75% acetonitrile, 28 to 30 min, 75% to 10% acetonitrile, 30 to 32 min, 10% acetonitrile, Detection wavelength of 300 nm. The 11 batches of HZDP samples were analyzed by using the similarity evaluation system of chromatographic fingerprints of traditional Chinese medicines (2004A version). Results The control fingerprints of 11 batches of HZDP were established and 18 common peaks were identified. Among them, 13 were assigned to medicinal herbs. The common peaks of 6, 7, 9, 10 and 12 originated from the common peaks of Angelica dahurica, 4,5,8 The common peaks of Citrus No. 1, No. 1, No. 2, No. 11 and No. 11 were from Magnolia officinalis, the common peak of No. 17 was derived from Atractylodes japonica and compared with the reference standard and ultra-fast liquid chromatography-ion trap-time of flight tandem mass spectrometry (UFLC- IT-TOF / MS) identified its chemical composition. Conclusion The method is simple, accurate, reliable and reproducible. It can provide a reference for the material basic research and quality control of HZDP.