白芍化学成分的高效液相色谱-电喷雾质谱研究

Determination of chemical compositions in extract of Radix Paeoniae Alba by liquid chromatography-electrospray ionization mass spectrometry

目的：采用高效液相色谱-电喷雾质谱联用技术（LC-ESI/MS）对白芍乙醇提取物中的化学成分进行分析鉴定。方法：选用反相C18色谱柱,以0.02%醋酸溶液（A）-甲醇（B）作为液相色谱流动相,梯度洗脱（0~2 min,13%B,2~120 min,13%B→100%B）,流速0.8 mL·min-1,检测波长270 nm,柱温30℃,进样量10μL。利用二极管阵列检测器（PDA）和电喷雾质谱（ESI-MS）正离子模式和负离子模式在线检测化学成分,扫描范围m/z 50~1000;离子阱条件：喷雾电压4.5 kV,鞘气辅助气为氮气,金属毛细管温度250℃,金属毛细管电压20 V。结果：共鉴定出8个化学成分,分别为芍药内酯苷、异芍药苷、芍药苷亚硫酸酯、没食子酰基芍药苷、芍药苷、苯甲酰芍药苷、氧化芍药苷和苯甲酰氧芍药苷。结论：利用液质联用技术对白芍中化学成分进行分析可以快速分析鉴定白芍中的化合物并提供结构信息。

Objective：To analyze and identify the chemical compositions from crude extracts of Radix Paeoniae A1- ba by liquid chromatography coupled with electrospray ionization mass spectrometry （ LC - ESI/MS）. Methods ： The analysis was processed by means of a reversed phase C1s column and a binary mobile phase system consisting of 0.02 % acetic acid aqueous （A） and methanol （ B ） under a gradient condition （0 - 2 rain, 13 % B, 2 - 120 rain, 13 % B→100% B）with the flow rate of O. 8 mL · min-1, the detection wavelength of 270 nm, the column temperature of 30 ℃ and the injection volume of 10 μL. A photodiode array detector（PDA） and an electrospray ionization mass spectrometry（ESI - MS） under the both positive and negative ion modes were used to detect the chemical constitu- ents at the same time. The full scan of ions ranged from m/z 50 to 1000 ;the mass spectrometer conditions were as follows. The spray voltage was 4.5 kV, the sheath gas was nitrogen, the capillary voltage was set at 20 V and the temperature of metal capillary tube was controlled at 250 ℃. Results：The main chemical compositions from Radix Paeoniae Alba crude extracts were glycosides, and eight major peaks including isopaeoniflorin, albiflorin, galloylpae- oniflorin, paeoniflorin, benzoylpaeoniflorin, oxypaeoniflorin, benzoyloxypaeoniflorin and paeoniflorin sulfonate were respectively separated and detected. Conclusion：The technique of HPLC - MS can quickly analyze and identify the compositions in Radix Paeoniae Alba and provide structural information.