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Efficient counter-current chromatographic isolation and structural identification of phenolic compounds from sweet potato leaves

机译:甘薯叶中酚类化合物的高效逆流色谱分离和结构鉴定

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High-speed counter-current chromatography was successfully applied to separate and purify bioactive ingredients from sweet potato leaves. Four caffeoylquinic acid derivatives and a mixture of two flavonoids were successfully obtained in one step. The caffeoylquinic acid derivatives were 3-O-caffeoylquinic acid (1), 4,5-di-O-caffeoylquinic acid (4), 3,5-di-O-caffeoylquinic acid (5), and 3,4-di-O-caffeoylquinic acid (6). The two-phase solvent system was composed of n-hexaneethyl acetateethanolwater acetic acid (1:5:2:4:0.1, v/v). The upper layer was used as the stationary phase, and the lower layer was used as the mobile phase. The flow rate was 1.5mL/min, the revolution speed was 850rpm, and the injection volume was 280mg. The mixture of flavonoids was separated by preparative high-performance liquid chromatography into quercetin-3-O-β-D-galactopyranoside (2) and quercetin-3-O-β-D-glucoside (3). The purities of compounds 1-6 were 95.8% (5.4mg), 99.5% (6.1mg), 98.7% (15.1mg), 97.8% (14.5mg), 96.2% (10.3mg), and 96.8% (7.8mg), respectively, as determined by HPLC with a pulsed amperometric detector. The chemical structures were identified by electrospray ionization-tandem mass spectrometry and nuclear magnetic resonance imaging. The results showed the efficiency of the method in purifying bioactive compounds from sweet potato leaves, and compound 2 was separated from sweet potato for the first time.
机译:高速逆流色谱法已成功应用于从甘薯叶中分离和纯化生物活性成分。一步即可成功获得四种咖啡酰奎尼酸衍生物和两种类黄酮的混合物。咖啡酰奎尼酸衍生物是3-O-咖啡酰奎尼酸(1),4,5-二-O-咖啡酰奎尼酸(4),3,5-二-O-咖啡酰奎尼酸(5)和3,4-二-邻咖啡酰奎尼酸(6)。两相溶剂系统由正己烷乙酸乙酯乙醇水乙酸(1:5:2:4:0.1,v / v)组成。上层用作固定相,下层用作流动相。流速为1.5mL / min,转速为850rpm,注射量为280mg。通过制备型高效液相色谱将类黄酮混合物分离为槲皮素-3-O-β-D-吡喃半乳糖苷(2)和槲皮素-3-O-β-D-D-葡萄糖苷(3)。化合物1-6的纯度为95.8%(5.4mg),99.5%(6.1mg),98.7%(15.1mg),97.8%(14.5mg),96.2%(10.3mg)和96.8%(7.8mg)分别由HPLC和脉冲安培检测器测定。化学结构通过电喷雾串联质谱和核磁共振成像鉴定。结果表明该方法从甘薯叶中纯化生物活性化合物是有效的,化合物2首次从甘薯中分离出来。

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