HPLC-ESI-MS法同时测定虎杖提取物中的17种成分

Simultaneous analysis of 17 compounds from the extract of Giant knotweed R. by HPLC-ESI-MS

目的采用HPLC和电喷雾质谱联用技术并结合核磁共振和紫外光谱技术分析测定虎杖复合酶提取物中的化学成分。方法液相色谱条件为色谱柱:Agilent C18色谱柱(250 mm×4.6 mm,5μm),流动相:质量分数为0.2%的醋酸溶液(A)-乙腈(B)进行梯度洗脱,流速为0.8 mL.min-1;检测波长为254 nm,以Thermo-LCQ-FLEET多级离子阱质谱仪进行检测。结果采用HPLC-ESI-MS法检测了中药虎杖中17个化学成分,分别为芦丁(rutin)、大黄酚(chrysophanol)、6-OH-大黄素(6-OH-emodin)、大黄素(emodin)、金丝桃苷(hyperoside)、异槲皮素(isoquercetin)、三叶豆苷(trifolin)、紫云英苷(astragalin)、何首乌乙素(polygonimitin B)、大黄酚(chrysophanol)、大黄素-8-葡萄糖苷(emodin-8-glucoside)、新芒果苷(neomangiferin)、芒果苷(mangiferin)、槲皮素(quercetin)、山奈酚(kaempferol)、I3-II8双芹菜苷元(I3-II8-biapigenin)和芹菜素(apigenin)。结论 HPLC-EST-MS法可用于虎杖提取物中的17种成分的含量测定。

Objective To apply HPLC-ESI-MS combining with NMR and UV technique for the analysis of the major constituents of the extract of Giant knotweed R. Methods The separation was performed on the Agilent C18 （250 mm×4.6mm,5μm）column. The mobile phase was composed of 0.2% （w）acetic acid in aqueous solution （A）and acetonitrile（ B ）, and the flow rate was 0.8 mL. min-1. The wavelength of the UV detector was set at 254 nm. The MS spectrometer was Thermo LCQ Fleet mass spectrometer. Results Seventeen compounds including of rutin, chrysophanol, 6-OH-emodin, emodin, hyperoside, isoquercetin, trifolin, austragalin, polygonimitin B, chrysophanol, emodin-8-O-glucoside, neomangiferin, mangiferin quercetin, kaempferol I3-II8-biapigenin and apigenin from Giant knotweed R. were detected by HPLC-MS. Conclusions The method of complex enzyme extraction combined with the analysis by HPLC-ESI-MS has been proved to be effective, sensitive and intuitionistic. It can be used to analyze the micro constituent in G. knotweed. This method can provide the reference for the analysis and study of other Chinese medicine.