UPLC-Q-TOF-MS分析苗族药红花龙胆化学成分
|
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.
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
[1]贵州省药品监督管理局.贵州省中药材、民族药材质量标准[M].贵阳:贵州科技出版社,2003:184.
[2]国家药典委员会.中华人民共和国药典.一部[M].北京:中国医药科技出版社,2015:151-152.
[3]国家中医药管理局《中华本草》编委会.中华本草.第三十五卷-苗药卷[M].贵阳:贵州科技出版社,2005:328.
[4]陈云,王国凯,武璨,等.红花龙胆化学成分研究[J].中国中药杂志,2013,38(3):362-365.
[5]罗君,卿娟,赵琳珺,等.红花龙胆高效液相指纹图谱[J].中国实验方剂学杂志,2014,20(14):69-72.
[6]赵琳珺,罗君,卿娟,等.红花龙胆血清药物化学初步研究[J].医药导报,2017,36(7):750-752.
[7]康新莉,宋良科,时晓缇,等.红花龙胆及其炮制品中芒果苷的含量测定比较[J].现代中药研究与实践,2016,30(1):39-41.
[8]吴立宏,官海峰,俞丽,等.红花龙胆质量标准研究[J].中国中药杂志,2010,35(16):2099-2102.
[9]刘成松,曹斐华,彭雪晶,等.条纹龙胆的化学成分研究[J].中药材,2012,35(6):908-910.
[10]潘聿.滇龙胆特征成分群指纹图谱评价研究[D].昆明:云南中医学院,2015.
[11]齐静静,苑桂鑫,宋凤瑞,等.龙胆质谱指纹图谱及化学模式识别方法研究[J].质谱学报,2009,30(6):334-339.
[12]杨爱梅,孙静,韩晗,等.藏药线叶龙胆化学成分的研究[J].中成药,2012,34(3):506-508.
[13]覃洁萍,邓家刚,冯钰锜,等.有机质谱分析在芒果苷原料药微量杂质结构鉴定中的应用[J].质谱学报,2008,29(4):218-225.
[14]郑伟,岳跃栋,龚亚君,等.双斑獐牙菜的化学成分研究[J].中草药,2016,47(9):1468-1476.
[15]樊轻亚.农吉利中有效成分的提取分析研究[D].广州:广东药学院,2009.
[16]冯怡,邓远辉,曾星邓,等.液相色谱-串联质谱法测定人血浆中的的龙胆苦苷浓度[J].药物分析杂志,2007,27(2):157-160.
[17]赵莹,冯怡,赵瑞芝.小鼠组织中龙胆苦苷含量的液相色谱-串联质谱测定[J].时珍国医国药,2010,21(7):1580-1582.
[18]刘芳,赵声兰,陈朝银.质谱解析多糖结构的方法学进展[J].药物分析杂志,2011,31(8):1612-1617.
[2]国家药典委员会.中华人民共和国药典.一部[M].北京:中国医药科技出版社,2015:151-152.
[3]国家中医药管理局《中华本草》编委会.中华本草.第三十五卷-苗药卷[M].贵阳:贵州科技出版社,2005:328.
[4]陈云,王国凯,武璨,等.红花龙胆化学成分研究[J].中国中药杂志,2013,38(3):362-365.
[5]罗君,卿娟,赵琳珺,等.红花龙胆高效液相指纹图谱[J].中国实验方剂学杂志,2014,20(14):69-72.
[6]赵琳珺,罗君,卿娟,等.红花龙胆血清药物化学初步研究[J].医药导报,2017,36(7):750-752.
[7]康新莉,宋良科,时晓缇,等.红花龙胆及其炮制品中芒果苷的含量测定比较[J].现代中药研究与实践,2016,30(1):39-41.
[8]吴立宏,官海峰,俞丽,等.红花龙胆质量标准研究[J].中国中药杂志,2010,35(16):2099-2102.
[9]刘成松,曹斐华,彭雪晶,等.条纹龙胆的化学成分研究[J].中药材,2012,35(6):908-910.
[10]潘聿.滇龙胆特征成分群指纹图谱评价研究[D].昆明:云南中医学院,2015.
[11]齐静静,苑桂鑫,宋凤瑞,等.龙胆质谱指纹图谱及化学模式识别方法研究[J].质谱学报,2009,30(6):334-339.
[12]杨爱梅,孙静,韩晗,等.藏药线叶龙胆化学成分的研究[J].中成药,2012,34(3):506-508.
[13]覃洁萍,邓家刚,冯钰锜,等.有机质谱分析在芒果苷原料药微量杂质结构鉴定中的应用[J].质谱学报,2008,29(4):218-225.
[14]郑伟,岳跃栋,龚亚君,等.双斑獐牙菜的化学成分研究[J].中草药,2016,47(9):1468-1476.
[15]樊轻亚.农吉利中有效成分的提取分析研究[D].广州:广东药学院,2009.
[16]冯怡,邓远辉,曾星邓,等.液相色谱-串联质谱法测定人血浆中的的龙胆苦苷浓度[J].药物分析杂志,2007,27(2):157-160.
[17]赵莹,冯怡,赵瑞芝.小鼠组织中龙胆苦苷含量的液相色谱-串联质谱测定[J].时珍国医国药,2010,21(7):1580-1582.
[18]刘芳,赵声兰,陈朝银.质谱解析多糖结构的方法学进展[J].药物分析杂志,2011,31(8):1612-1617.