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目的建立制备型高效液相色谱(PHPLC)分离竹叶黄酮中异荭草苷和荭草苷的方法。方法竹叶黄酮经AB-8树脂吸附洗脱纯化后,采用PHPLC分离异荭草苷和荭草苷,制备色谱条件:流动相为甲醇-0.3%乙酸水溶液(32∶68),体积流量为5 mL/min,柱温为20℃,检测波长330 nm,进样体积为400μL,上样质量浓度为15.3 mg/mL。结果 HPLC检测表明,异荭草苷的质量分数>99%,荭草苷的质量分数>93%,加样回收率分别为(92.7±2.92)%和(85.1±3.45)%。单体结构通过核磁共振碳谱和氢谱鉴定,确定为异荭草苷和荭草苷。结论该法分离效果较好,低毒,回收率高,可用于竹叶黄酮中2种黄酮苷的分离制备。
OBJECTIVE To establish a preparative high performance liquid chromatography (HPLCLC) method for isolating isorientin and tirriolide from bamboo leaf flavonoids. Methods After the bamboo leaves flavonoids were purified by adsorption on AB-8 resin, iso-triterpenoid glycosides and triclucan were separated by PHPLC. The chromatographic conditions were as follows: the mobile phase was methanol-0.3% acetic acid solution (32:68), the volume flow rate was 5 mL / min, the column temperature was 20 ℃, the detection wavelength was 330 nm, the injection volume was 400 μL, and the loading mass concentration was 15.3 mg / mL. Results The results of HPLC showed that the content of isoorientin was more than 99% and the content of toxins was more than 93%. The average recoveries were (92.7 ± 2.92)% and (85.1 ± 3.45)%, respectively. The monomer structure was identified by 1H NMR and 1H NMR spectra and identified as isoorientin and xyloside. Conclusion The method has good separation effect, low toxicity and high recovery rate. It can be used for the separation and preparation of two flavonoid glycosides in bamboo leaf flavonoids.