建立了高效毛细管电泳-电喷雾飞行时间质谱联用(HPCE—ESI—TOF/MS)快速定性分析黄连中生物碱类化合物的分析方法.使用未涂层石英毛细管,以50mmol/L 乙酸铵-0.5%甲醇溶液(用氨水调至pH=7.2)作为运行缓冲液,分离电压为25kV;鞘液组成为50%甲醇-49.5%水-0.5%乙酸,鞘液流速为4μL/mn;质谱选用正离子模式,碰撞电压(Fragmentor)为100V.结果表明,通过各色谱峰紫外光谱和质谱测得精确分子量结果,结合文献,对黄连中7种生物碱进行了鉴定.表明本方法简便、快速,是黄连中生物碱类化合物快速分离、鉴别的有效方法.
A new method for the analysis of alkaloids in Coptis chinensis Franch was established by high performance capillary electrophoresis-electrospray ionization time of flight mass spectrometry (HPCE-ESI-TOF/MS). The real samples were separated by an uncoated capillary. 50 mmol/L ammonium acetate containing 0.5% methanol (pH=7.2) was used as the running buffer, and separation voltage was 25 kV. A coaxial sheath flow interface was used as the CE-MS interface, and a 50% methanol-49.5% water- 0.5% acetic acid mixture was used as the sheath liquid with a flow rate of 4 μL/min. The lens voltages in a positive ion mode with a collision induced dissociation (CID) voltage of 100 V were used for ESI-TOF/MS analysis. Seven alkaloids in Coptis chinensis Franch methanol extracts were separated and identified by CE-DAD and CE-ESI-TOF/MS. The coupling of HPCE separation with accurate mass measurement capability of ESI-TOF/MS provides an attractive tool for the identification of alkaloid compounds in Coptis chinensis Franch.