液相色谱-质谱联用法分析葡萄籽提取物中的5种多酚类成分

目的：应用液相色谱-质谱联用法对葡萄籽提取物中的组成成分进行测定。方法：采用Zobax SB-C₁₈色谱柱（250 mm×4.6 mm，5 μm），流动相为乙腈（A）-水（1%甲醇+0.1%甲酸）（B），梯度洗脱，流速为1.0 mL·min^-1，柱温为40℃，进样体积10 μL；电喷雾电离（ESI），毛细管温度300℃，碎裂能量30%，离子源电压4.5 kV，毛细管电压12.7 V，对葡萄籽提取物中的组分定性分析。结果：应用LC-MS法明确了葡萄籽提取物的组分主要为单体和原花青素低聚体，并分析二级质谱碎片推测出了原花青素的裂解规律。结论：应用液相色谱-质谱联用技术可以较好地对葡萄籽提取物中没食子酸、儿茶素、表儿茶素等组分进行测定。

Objective: To apply an LC-MS method for determination of components in grape seed extract. Methods: Chromatographic separation was performed on an Agilent zobax SB -C₁₈ column (4.6 mm×250 mm,5 μm),the mobile phase was acetonitrile-water(1% methanol+0.1% methanoic acid) with the gradient elution at a flow rate of 1.0 mL·min^-1;the column temperature was maintained at 40℃,and the injection volume was 10 μL. The qualitative analysis of grape seed extract components was carried out by electrospray ionization (ESI) under the following condition:capillary temperature was at 300℃,the fracture energy was 30%,ion source voltage was 4.5 kV,and capillary voltage was 12.7 V. Results: The application of LC-MS proved the composition of grape seed extract mainly as monomers,oligomers and procyanidins and secondary mass spectrometry analysis of debris infer the pyrolysis regularity of procyanidins. Conclusion: Gallic acid,catechin and epicatechin components in grape seed extract can be better determined by the application of LC-MS.

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