Liu Ren-min, He Feng-yun, Sun Ai-ling
School of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, China.
Yao Xue Xue Bao. 2004 May;39(5):363-6.
To establish a method for separation and identification of alkaloids in Stephania tetrandra S. Moore methanol extracts by using non-aqueous capillary electrophoresis interfaced with electrospray ionization ion trap mass spectrometry.
The molecular ions or adducts of alkaloids and fragments of specific parent ions were used for the identification. An uncoated capillary (86 cm x 75 microm ID, on-line UV detection occurred at 21 cm from the inlet of the capillary) was used. Ammonium acetate (50 mmol x L(-1)) containing 4% HAc in methanol was used as the running buffer; separation voltage was 25 kV. A coaxial sheath flow interface was used as the CE-MS interface; the electrospray voltage was 4.5 kV; the temperature of aluminium capillary was 170 degrees C; 60% isopropanol-39% water-1% HAc was used as the sheath liquid with the flow rate of 5 microL x min(-1); the collision energy of MS-MS was set at 30% and the least ion counts was 1 x 10(5).
The alkaloids in Stephania tetrandra S. Moore methanol extracts were separated and identified by CE-ESI-MS/MS. The proposed method is of high accuracy and can be used for the investigation of traditional Chinese medicine.
建立一种采用非水毛细管电泳-电喷雾电离离子阱质谱联用技术分离鉴定防己甲醇提取物中生物碱的方法。
利用生物碱的分子离子或加合物以及特定母离子的碎片进行鉴定。使用未涂层毛细管(86 cm×75 μm内径,在线紫外检测在距毛细管入口21 cm处进行)。以含4%醋酸的50 mmol·L⁻¹醋酸铵甲醇溶液作为运行缓冲液;分离电压为25 kV。采用同轴鞘流接口作为毛细管电泳-质谱联用接口;电喷雾电压为4.5 kV;铝质毛细管温度为170℃;以60%异丙醇-39%水-1%醋酸作为鞘液,流速为5 μL·min⁻¹;串联质谱的碰撞能量设定为30%,最小离子计数为1×10⁵。
采用毛细管电泳-电喷雾电离串联质谱法对防己甲醇提取物中的生物碱进行了分离和鉴定。该方法准确性高,可用于中药研究。