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,5μm),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 m L·min^-1,柱温为40℃,进样体积10μL;电喷雾电离(ESI),毛细管温度300℃,碎裂能量30%,离子源电压4.5 k V,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 μ m ), 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 μ L. The qualitative analysis of grape seed extract components was carried out by electrospray ionization ( ESI )under the following condition: capillary temperature was at 3ou u, me ractuly was 4.5 kV, and capillary voltage was 12.'7 Y. 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.