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本文建立了分离纯化鉴定拳卷地钱中芹菜素 -7- O- β- D- 葡萄糖醛酸甙的硅胶柱色谱 /RP- HPLC/LC- ESI- MS方法。拳卷地钱叶经过 80 %乙醇提取后 ,减压蒸馏 ,得粗提物。拳卷地钱叶粗提物用甲醇溶解后上硅胶柱 ,用不同浓度的甲醇 氯仿溶液洗脱 ,各洗脱液进行RP- HPLC分析 ,较纯的洗脱液进行LC- ESI- MS分析 ,为制备分离黄酮类化合物单体提供指导。氯仿与甲醇配比为 5 :4的洗脱液经过RP- HPLC分析为单一组分 ,tR为 12 1min ,与对照品芹菜素 - 7 -O-β -D 葡萄糖醛酸甙共注射进行RP HPLC实验 ,发现峰高增加 ,tR为 12 . 1min,UV(λmax为 336 /2 96 (sh) /2 6 7nm)和IR光谱与芹菜素 - 7 -O -β- D 葡萄糖醛酸甙基本一致。LC ESI MS测定结果表明 ,与对照品芹菜素 -7 -O- β- D -葡萄糖醛酸甙的分子量相同为 4 4 6。由此可以鉴定该洗脱组分为芹菜素 -7 -O -β- D- 葡萄糖醛酸甙。
In this paper, a silica gel column chromatography/RP-HPLC/LC-ESI-MS method was developed for the separation and purification of apigenin-7-O-β-D-glucuronidate from Marquis. After the box leaf was extracted with 80% ethanol, it was distilled under reduced pressure to obtain a crude extract. The crude extract of the money leaf was dissolved in methanol and then loaded onto a silica gel column and eluted with different concentrations of methanol in chloroform. The eluents were analyzed by RP-HPLC, and the pure eluent was analyzed by LC-ESI-MS. Provide guidance for the preparation of separation of flavonoid monomers. The eluate with chloroform:methanol ratio of 5:4 was analyzed by RP-HPLC as a single component, with a tR of 121 min, and co-injection with the control apigenin-7-O-β-D glucuronide for RP HPLC. Experiments showed that the peak height increased, tR was 12.1 min, UV (λmax was 336 / 2 96 (sh) / 267 nm) and the IR spectrum was basically consistent with that of apigenin-7-O-β-D glucuronide. The results of LC ESI MS indicated that the molecular weight of apigenin-7-O-β-D-glucuronide was the same as that of the reference product, 4 46 . From this, it was identified that the eluted fraction was apigenin-7-O-β-D-glucuronide.