机构地区:[1]贵州中医药大学药学院/药食两用资源应用与开发研究中心/中药材开发技术研究中心,贵阳550025 [2]贵州省药食同源植物资源开发工程技术研究中心,贵阳550025
出 处:《中国药房》2021年第4期443-452,共10页China Pharmacy
基 金:国家重点研发计划项目(No.2018YFC1708100);贵州省科技计划项目(No.黔科合平台人才〔2019〕5407);贵州省高层次创新型人才培养项目(No.黔科合人才〔2015〕4032号);贵州中医药大学2018年度学术新苗培养及创新探索专项项目(No.黔科合平台人才〔2018〕5766号-9);贵阳中医学院博士启动基金项目(No.2019)。
摘 要:目的:鉴定并分析不同基原八爪金龙药材中黄酮及香豆素类成分。方法:采用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法(UPLC-QE-HF-MS/MS)。色谱柱为Zorbax Eclipse-C18,流动相为乙腈-0.1%甲酸水溶液(梯度洗脱),柱温为30℃,流速为0.3 mL/min,自动进样器温度为4℃,进样量为2μL。离子源为电喷雾离子源,扫描模式为正、负离子模式,加热器温度为325℃,鞘气压力为45 arb,辅助气压力为15 arb,吹扫气压力为1 arb,电喷雾电压为3.5 kV,毛细管温度为330℃,透镜电压为55%,扫描模式为一级全扫描(m/z 100~1500)、数据依赖性二级质谱扫描(dd-MS2,Top N=10),分辨率为70000(一级质谱)、17500(二级质谱),碰撞模式为高能量碰撞解离。通过参考ChemSpider、mzCloud、mzVault、PubChem等国内外专业数据库,同时结合相关文献和对照品数据对化合物结构进行鉴定并比较含量。结果与结论:从朱砂根、百两金、红凉伞等3种不同基原的八爪金龙药材中共分离47个成分,鉴定出17个黄酮类化合物,包括9个黄酮醇类(槲皮素3-O-鼠李糖苷7-O-葡糖苷、杨梅素、芦丁、毛里求斯排草素、山柰酚、槲皮素、异鼠李素、槲皮苷、美恩西汀)、3个黄烷-3-醇类(表棓儿茶素、儿茶素、表没食子儿茶素没食子酸酯)、2个二氢黄酮类(黄颜木素、圣草酚)及3个其他类{3-(2,3-二氢苯并[1,4]二噁英-6-基)-7-羟基-2-三氟甲基-4-酮、墨沙酮、Oriciacridone F},10个香豆素类化合物{岩白菜素、[(7-羟基-4-甲基-2-氧代-2H-色烯-6-基)氧基]乙酸、[7-(羧基甲氧基)-4-甲基-2-氧-2-羟色基-3-基]乙酸、4,9-二羟基7H-呋喃并[3,2-g]色烯-7-酮、6,7-二羟基-4-甲基香豆素、七叶内酯、秦皮素、7,8-二羟基-4-甲基香豆素、4-甲基伞形酮葡萄糖醛酸、二十烷酮}。含量分析结果显示,黄酮、香豆素类化合物中,3种不同基原八爪金龙药材中共有5个共有成分,分别为岩白菜素(2号峰)、[7-(羧基OBJECTIVE:To identify and analyze the flavonoids and coumarins in Radix Ardisiae from different sources.METHODS:UPLC-QE-HF-MS/MS was adopted.The determination was performed on Zorbax Eclipse-C18 column with mobile phase consisted of acetonitrile-0.1%formic acid solution(gradient elution)at the flow rate of 0.3 mL/min.The column temperature was 30℃,and the temperature of injector was 4℃.The sample size was 2μL;ESI source was applied in negative and positive scanning ion mode,the heater temperature was 325℃,the sheath gas pressure was 45 arb,the auxiliary gas pressure was 15 arb,the purge gas pressure was 1 arb,the electrospray voltage was 3.5 kV,the capillary temperature was 330℃,S-lens RF level was 55%,scan mode was first-order full scan m/z 100-1500,data-dependent secondary mass spectrometry scanning(dd-MS2,Top N=10),the resolution was 70000(first mass spectrometry),17500(secondary mass spectrometry),the collision mode was high-energy collision dissociation.Through retrieving foreign and domestic databases as ChemSpider,mzCloud,mzVault,PubChem,the structure of the compound was identified on the basis of related literatures and reference data,and the contents were compared.RESULTS&CONCLUSIONS:A total of 47 components were separated from Radix Ardisiae of 3 kinds of sources as Ardisia crenata Sims,A.crispa(Thunb.)A.DC.,A.crenata Sims var.bicolor(Walk)C.Y.Wu et C.Chen.A total of 17 flavonoids were identified,including 9 flavonols(quercetin 3-O-rhamnoside-7-O-glucoside,myricetin,rutin,mauritanin,kaempferol,quercetin,isorhamnetin,quercetin,mearnsitrin),3 flavan-3-ols[(-)-epigallocatechin,catechin,epigallocatechin gallate)2 dihydroflavonoids[fustin,eriodictyol]and 3 other types[3-(2,3-dihydro-benzo[1,4]dioxin-6-yl)-7-hydroxy-2-trifluoromethyl-chromen-4-one,methadone,oriciacridone F],10 coumarins{bergenin,[(7-hydroxy-4-methyl-2-oxo-2H-chromen-6-yl)oxy]acetic acid,[7-(carboxymethoxy)-4-methyl-2-oxo-2hydroxychromo-3-yl]acetic acid,4,9-dihydroxy-7H-furo[3,2-g]chromen-7-one,6,7-dihydroxy-4-methylcoumarin,esculetin
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...