结合两种LC／MS方法用于复方丹参滴丸中多成分的鉴定

Identification of multi-component in Danshen Dropping Pills by using a combinative LC/MS approach

目的:建立一种结合两种LC/MS的方法,对复方丹参滴丸(丹参,三七,冰片,等)中的多成分进行鉴定。方法:色谱分离采用Phenomenex Luna C18反相柱(250 mm×4.6 mm,5μm),流动相组成分别为0.2%甲酸水溶液和乙腈,梯度洗脱,流速:1.0 mL/min;质谱定性采用飞行时间质谱(TOF-MS)结合离子阱多级质谱(Trap-MSn),负离子模式扫描。结果:在优化的液质联用条件下,飞行时间质谱筛查出复方中14种成分的分子式,采用离子阱多级质谱共鉴定出13种成分,并对其药材来源进行了归属。结论:本实验建立了一种结合两种LC/MS的分析方法,为中药复方多成分的分析提供了一种有效、可靠的新模式,也同样适用于其它复杂体系的分析。

AIM： To develop a combinative LC/MS for the identification of multi-component in Danshen Dropping Pills （Radix et Rhizorna Salviae miltiorrhizale, Radix et Rhizoma Notoginseng, Borneolum Syntheticum, etc. ）. METHODS： Separation was performed on a Phenomenex Luna C18 reverse-phase column （250 mm × 4.6 mm, 5 μm）. The mobile phase consisted of water containing 0.2% formic acid and acetonitrile was used as gradient elute. The flow rate was 1 mL/min. A combination of time-of-flight mass spectrometer （TOF-MS） and ion trap tandem mass spectrometer （Trap-MSn） was applied for qualitative analysis under negative ion mode. RESULTS： Under optimized LC/MS condition, the molecular formulae of 14 components were screened by TOF-MS and 13 of them were then identified by Trap-MS^n. All of the components were surveyed and classified according to their medicinal materials derivation. CONCLUSION： The established combinative LC/MS method can thus be considered as an effective and credible pattern for the analysis of Chinese multi-herb remedy, as well as other complex systems.