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目的研究白英化学成分,建立HPLC-ELSD法测定白英中碱苷A[3-O-β-D-glucopyranosyl-(1→2)-β-D-glucopyranosyl-(1→4)-β-D-galactopyranoside-(25ξ)-solanidan-3β,23β-diol]的含量的方法。方法采用硅胶、ODS柱色谱进行分离纯化。运用NMR数据及理化性质鉴定单体化合物的结构。色谱柱为Elite-ODS C18(200 mm×4.6 mm,5μm),流动相为乙腈-体积分数为0.02%三乙胺水溶液(体积比为56∶44),检测器漂移管温度为95℃,氮气流速2.3 L.min-1。结果从白英提取物中分离得到碱苷A。碱苷A在0.4~4.0μg线性关系良好(r=0.999 6),平均回收率为99.6%(RSD=2.0%)。结论HPLC-ELSD法可用于白英中碱苷A的测定。
OBJECTIVE: To study the chemical constituents of Bletilla striata and establish HPLC-ELSD method for the determination of alkaloid glycoside A[3-O-β-D-glucopyranosyl-(1→2)-β-D-glucopyranosyl-(1→4)-β-D- Method of content of galactopyranoside-(25ξ)-solanidan-3β, 23β-diol]. The method was separated and purified by silica gel and ODS column chromatography. The structure of the monomeric compounds was identified using NMR data and physicochemical properties. The column was Elite-ODS C18 (200 mm×4.6 mm, 5 μm). The mobile phase consisted of acetonitrile-0.02% triethylamine aqueous solution (56:44 volume ratio). The detector drift tube temperature was 95°C. Flow rate 2.3 L.min-1. As a result, an alkali glycoside A was isolated from the white English extract. Alkaline glycoside A had good linearity in the range of 0.4-4.0 μg (r=0.999 6) and the average recovery was 99.6% (RSD=2.0%). Conclusion HPLC-ELSD method can be used for the determination of alkaloid glycoside A in Bai Ying.