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目的 :建立分离纯化鉴定拳卷地钱中芹菜素 -7-O -β -D -葡萄糖醛酸苷的硅胶柱色谱 /RP -HPLC/LC -ESI -MS方法。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 ,用甲醇 -氯仿配比为 2 5∶1,2 5∶2 ,2 5∶3…… 2∶2 5 ,1∶2 5混合溶液洗脱 ,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。结果 :氯仿与甲醇配比为 2 5∶15、2 5∶16、2 5∶ 17、2 5∶18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 -葡萄糖醛酸苷共注射进行RP -HPLC实验 ,发现峰高增加 ,tR 为12 1min ,UV[λmax为 3 3 6/ 2 96(sh) / 2 67nm]和IR光谱与芹菜素 -7-O -β -D -葡萄糖醛酸苷基本一致。LC -ESI -MS测定结果表明 ,与对照品芹菜素 -7-O -β -D -葡萄糖醛酸苷的分子量相同为 44 6。结论 :由此可以鉴定该洗脱组分为芹菜素 -7-O -β -D -葡萄糖醛酸苷。
Objective : To establish a method for the separation and purification of apigenin-7-O-β-D-glucuronide by column chromatography and RP-HPLC/LC-ESI-MS. Methods : After 80% ethanol extraction, the money leaves of Curl Curl was distilled under reduced pressure to obtain crude extract. The crude extract of the box leaf was dissolved in methanol and then applied to a silica gel column. The methanol-chloroform ratio was 2:5:1, 25:2, 25:3,... 2:25, 1:2 5 mixed solution. Elution, RP-HPLC analysis of each eluent, LC-ESI-MS analysis of pure eluent, to provide guidance for the preparation of separation of flavonoids monomers. Results: The eluents of chloroform and methanol in the ratios of 25:15, 25:16, 25:17, and 2.5:18 were analyzed by RP-HPLC as a single component, tR was 12 1min, and the control was celery The co-injection of prime-7-O-β-D-glucuronide for RP-HPLC experiments revealed an increase in peak height with tR of 12 1min, UV[λmax of 3 3 6 / 2 96(sh) / 2 67 nm] and IR spectrum is basically consistent with apigenin-7-O-β-D-glucuronide. The LC-ESI-MS determination showed that the molecular weight of the apigenin-7-O-β-D-glucuronide was 44 6 . Conclusion : This can be identified as apigenin-7-O-β-D-glucuronide.