摘要
目的:利用超高效液相色谱-电喷雾质谱联用技术(UPLC-Q-TOF-MS)对苗药红花龙胆95%乙醇提取物的正丁醇萃取部位化学成分进行分析鉴定。方法:采用Waters BEH-C18色谱柱(2. 1 mm×50 mm,1. 7μm);流动相0. 01%甲酸水-0. 01%甲酸乙腈,梯度洗脱;柱温30℃;流速0. 4 m L·min~(-1)。质谱使用ESI离子源,正负离子模式下采集数据,结合龙胆属相关文献以及对照品信息进行数据分析。结果:从红花龙胆中共鉴定出化合物33个,包括环烯醚萜类10个,酚酸类6个,黄酮类5个,三萜类6个,苯甲酸碳苷类1个,吡喃酮类1个,其他类4个。其中24个化合物为首次从红花龙胆中发现,分别为阿魏酸,去甲基雏菊叶龙胆酮,3S,5R,6R,9S-tetrahydroxymegas-tigmane,雏菊叶龙胆酮,龙胆二糖,当药苷,secoxyloganin,α-香树脂醇或β-香树脂醇,28-羟基-α-香树脂醇(28-羟基-β-香树脂醇或24-羟基-羽扇豆醇),去甲-当药苷,槲皮素-3-O-β-D葡萄糖苷,3-O-乙酰氧基熊果醇,2'-(2,3-二羟基苯甲酰)-龙胆苦苷,龙胆三糖,gmephiloside,异荭草苷-4'-O-葡萄糖苷或异荭草苷-4'-O-葡萄糖苷,rindoside,macophyllosides A,macophyllosides B,rhodanthenone,secologanoside,gentiside F,gentiside G和花色素。结论:UPLC-Q-TOF-MS技术能够快速准确地鉴定红花龙胆的化学成分,为其质量评价和应用开发提供了参考。
Objective: To analyze and identify the chemical compositions of n-butyl alcohol fraction from Gentiana rhodantha 95% ethanol extract by using ultra-performance liquid chromatography with quadrupole-time-offlight mass spectrometry(UPLC-Q-TOF-MS). Method: The separation was performed on Waters BEH C18(2. 1 mm × 50 mm,1. 7 μm) with 0. 01% formic acid solution-0. 01% acetonitrile formate as mobile phase for gradient elution. The column temperature was 30 ℃,the flow rate was 0. 4 m L·min~(-1). ESI ion source was used in the mass spectrometry,and the data were collected in positive and negative ion modes for data analysis by referring to relevant literature of G. rhodantha and comparing with the control product information. Result: The 33 chemical compounds were identified from the plant,including 10 iridoids,6 phenolic acids,5 flavonoids,6 triterpenoids,1 benzoic acid carboxylate,1 pyranone and 4 other types. 24 compounds among them were detected from this species for the first time, namely ferulic acid, demethylbellidifolin, 3 S, 5 R, 6 R, 9 S-tetrahydrox-ymegastigmane, lbellidifolin, gentiobiose, chiratin, secoxyloganin, α-amyrin or β-amyrin, 28-hydroxy-α-amyrin(28-hydroxy-β-amyrin or 24-hydroxy-lupeol), norswertianolin, quercetin-3-O-β-glucoside,3-O-acetoxy-uvao,2'-(2,3-dihyd-roxybenzoyl)-gentiopicroside, gentianose,gmephiloside,isoorientin-4'-O-glucoside,rindoside,macophyllosides A,macophyllosides B and rhodanthenone respectively,secologanoside,gentiside F,gentiside G and anthocyanidin. Conclusion: UPLC-Q-TOF-MS technology can be used to identify the chemical compositions of G. rhodantha quickly and accurately,providing references for its quality evaluation and application development.
引文
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