HPLC-ESI/MS对肌萎灵冻干粉指纹图谱特征峰的鉴定

Identification of the Fingerprint Characteristic Peak of Jiweiling Freeze-dried Powder by HPLC-ESI/MS

关键词:  液相色谱-质谱联用法  肌萎灵冻干粉  指纹图谱

Key words:  LC-MS  Jiweiling freeze-dried powder  fingerprint

摘要:

目的 采用液相色谱-质谱联用法对肌萎灵冻干粉特征峰进行指认鉴定。方法 采用Symmetry C18(4.6 mm×250 mm，5 μm)色谱柱，流动相为乙腈-水-1%乙酸，流速1.0 mL·min^-1；柱温：30 ℃；离子源为大气压电喷雾电离源(ESI)，雾化气压力：275.8 kPa；辅助气压力：137.9 kPa；毛细管温度：340 ℃；喷雾电压：4.2 kV。选择正负离子扫描方式，记录总离子流(TIC)色谱图及其特征碎片。结果 肌萎灵冻干粉指纹图谱特征峰标出12个峰，其中7个色谱峰为人参主要成分，另外5个峰为淫羊藿主要成分。结论 本试验确定了肌萎灵冻干粉主要功效的化学物质基础及其来源，对肌萎灵冻干粉化学表征及质量评价有重要的参考价值。

Abstract:

OBJECTIVE To develop an HPLC-ESI/MS method for the identification of the fingerprint characteristic peak of Jiweiling freeze-dried powder. METHODS With a Symmetry C18 column(4.6 mm×250 mm, 5 μm), acetonitrile-water-1% acetic acid was used as mobile phase at a flow rate of 1.0 mL·min^-1, eluted in gradient mode and column temperature maintained at 30 ℃. The sample was determined by mass spectrum with API-ESI ionization source. The pressure of atomization room was 275.8 kPa, the pressure of adjunctive gas was 137.9 kPa, the temperature of capillary was 340 ℃, the atomization voltage was 4.2 kV. The positive and negative canner mode was selected, the total ion current(TIC) chromatography and characteristic fragment ions were recorded. RESULTS Twelve major chromatographic peaks were marked in the fingerprint characteristic peak of Jiweiling freeze-dried powder. Seven chromatographic peaks were founded in Ginseng Radix et Rhizoma, five chromatographic peaks were founded in Epimedii Folium. CONCLUSION The chemical constituents and the sources of Jiweiling freeze-dried powder is identified. And it is quite valuable for the quality evaluation as well as chemical characterization of Jiweiling freeze-dried powder.