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作 者:李祥[1,2] 吕磊[3] 窦幼萌[4] 洪战英[1] 柴逸峰[1]
机构地区:[1]第二军医大学药学院 [2]中国人民解放军62380部队 [3]第二军医大学东方肝胆外科医院药材科 [4]中国人民解放军总医院南楼心血管一科
出 处:《药物分析杂志》2013年第5期788-793,共6页Chinese Journal of Pharmaceutical Analysis
基 金:国家自然科学基金资助(No.81072614)
摘 要:目的:采用高效液相色谱-飞行时间质谱(HPLC-TOF/MS)联用技术分析中药复方三妙丸中的主要化学成分。方法:色谱分离采用SHISEIDO CAPCELL PAK C18色谱柱(3.0 mm×100 mm,3μm),流动相为乙腈(A)-0.1%甲酸水溶液(B),梯度洗脱,流速0.6 mL.min-1,柱温25℃。质谱定性鉴别采用TOF/MS正离子模式扫描,电压4 kV,雾化气压力275.85 kPa,干燥气流速10 L.min-1,干燥气温度350℃。结果:在优化的液质联用条件下,通过飞行时间质谱以及碎片离子裂解分析,鉴定了三妙丸中23个化学成分,包括3组同分异构体。结论:所建立的HPLC-TOF/MS联用法,可为鉴定三妙丸中的化学成分提供一种快速、高效的方法。Objective: To identify the main chemical components in compound Sanmiao pills by high performance liquid chromatography - time - of - flight mass spectrometry ( HPLC - TOF/MS). Methods: A SHISEIDO CAP-CELL PAK C18 column (3.0 mm × 100 mm,3 μm) was used for separation and identification of chemical components in Sanmiao pills with a mobile phase of acetonitrile (A) and 0. 1% formic acid in water solution (B) withgradient elution. The flow rate was set at 0.6 mL · min^ -1 and the column temperature was set at 25 ℃. Time - of - flight mass spectrometer (TOF/MS) was applied for qualitative analysis under positive ion mode. The capillary voltage was set to 4 kV,the nebulizer gas pressure was 275.85 kPa,the drying gas flow rate was set to 10 L · min^-1 at a temperature of 350 ℃. Results: Under optimized LC/MS conditions ,23 chemical constituents of Sanmiao pills in-cluding 3 pairs of isomers were identified through analyses of time - of - flight mass spectrometer and fragment ion splitting. Conclusion : A rapid and efficient HPLC - TOF/MS approach has been established for studying the chem-ical constituents in Sanmiao pills.
关 键 词:复方 三妙丸 高效液相色谱 电喷雾离子源-飞行时间质谱 化学成分 同分异构体 鉴别
分 类 号:R917[医药卫生—药物分析学]
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