LC-MS/MS分析人参茎叶提取液中人参皂苷Rg1、Re降解产物

LC-MS/MS Analysis of Degradation Products of Ginsenosides Rg1, Re Aqueous Solution from Ginseng Stem and Leaf

关键词:  人参茎叶  人参皂苷Rg₁  人参皂苷Re  降解产物  液相色谱/离子阱质谱联用

Key words:  stems and leaves of panax ginseng  ginsenosides Rg₁  ginsenosides Re  degradation products  LC-MS/MS

摘要:

目的 研究人参茎叶提取液中人参皂苷Rg₁、Re加热后所产生的降解产物，并分析产物的结构。方法 采用液相色谱/离子阱质谱联用仪对降解产物进行分析，并推测其结构，HPLC的条件为Agilent Extend-C₁₈（250mm×4.6 mm，5 μm）色谱柱，流动相为乙腈-水，梯度洗脱70 min，检测波长203 nm，流速0.4 mL·min^-1，柱温30℃；质谱条件为正离子检测方式，毛细管电压3 000 V，喷雾器15 psi，干燥器流速12.0 L·min^-1，干燥器温度350℃，扫描范围100~1 000 m/z；碎裂器范围4 500~1 500 V。结果 质谱图中有多种化合物，推测人参皂苷Rg₁、Re在人参茎叶提取液的pH值环境下进行加热，会发生脱糖、脱羟基、环合等反应，生成多种降解产物。结论 人参皂苷水溶液在人参茎叶提取液pH环境下加热的时间与温度对人参皂苷的降解非常敏感，说明此方法适用于人参皂苷类化合物的降解与分析。

Abstract:

OBJECTIVE To research the degradation products of ginsenosides Rg₁, Re from ginseng stem and leaf through heated, and analyze the structure of the products. METHODS Degradation products were analyzed by LC-MS/MS, and speculated its structure. HPLC conditions:An Agilent Extend-C₁₈ column(250 mm×4.6 mm, 5 μm) was used with acetonitrile and waters as mobile phase at the flow rate of 0.4 mL·min^-1, and the column temperature was 30℃ and the detection wavelength was 203 nm, gradient elution for 70 min. MS conditions:Positive polarity, capillary 3 000 V, nebulizer 15 psi, dry gas 12.0 L·min^-1, dry temperature 350℃, scan 100-1 000 m/z, ramp range 4 500-1 500 V. RESULTS A variety of compounds in the mass spectra, and predicted its structure. Ginsenosides Rg₁, Re in aqueous solution from Ginseng stem and leaf's chemical environment, during the heat would occur desugared dehydroxylation cyclization reaction, and produce a variety of degradation products. CONCLUSION The heating time and temperature of the ginsenoside aqueous solution under the pH environment of ginseng stem and leaf extract are very sensitive to the degradation of ginsenosides, which indicates that this method is suitable for the degradation and analysis of ginsenosides.