UPLC-Q-TOF-MS法分析防风中香豆素类化学成分
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摘要
目的:分析防风中香豆素类化学成分,为全面解析防风药材的药效物质基础提供参考。方法:采用超高效液相色谱仪联用四级杆串联飞行时间质谱(UPLC-Q-TOF-MS)法。色谱条件:色谱柱为ACQUITY UPLC BEH C18,流动相为0.1%甲酸水-0.1%甲酸乙腈(梯度洗脱),流速为0.3 mL/min,柱温为35℃,进样量为3μL;质谱条件:采用电喷雾离子源(ESI)在正、负离子模式下进行检测,离子喷雾电压ESI+/ESI-为5 500 V/-4 500 V,去簇电压为80～-80 V,辅助加热气压力为55.00 psi,雾化气压力为-55psi,气帘气压力为-35.00 psi,去溶剂温度为550℃,碰撞活化扫描能量为15 eV;碰撞电压为35 psi。通过与相关文献数据及标准品图谱对照,并结合UPLC-Q-TOF-MS提供的化合物准确相对分子质量进行成分分析及鉴定。结果:在ESI+模式下共解析出了135个化学成分,在ESI-模式下共解析出了105个化学成分。并鉴定出了在ESI+模式下的异欧芹素乙、伞形花内酯、东莨菪素、花椒毒素、补骨脂素、Ostenol、秦皮啶、异欧前胡素、5-羟基-8-甲氧基补骨脂素、珊瑚菜素、紫花前胡素等11个香豆素类化学成分。结论:该方法准确、快速,可用于防风中香豆素类化学成分的分析。
OBJECTIVE:To analyze chemical components as coumarin in Saposhnikovia divaricata,and to provide referencefor comprehensive analysis of pharmacodynamic material base in S. divaricata. METHODS:UPLC-Q-TOF-MS method wasadopted. Chromatographic condition:the determination was performed on ACQUITY UPLC BEH C18 column with mobile phaseconsisted of 0.1% formic acid water-0.1% formic acid acetonitrile(gradient elution)at the flow rate of 0.3 mL/min. The columntemperature was 35 ℃,and sample size was 3 μL. MS condition:ESI,in positive and negative ion mode,ESI+/ESI-5 500 V/-4 500 V,declustering potential of 80--80 V,auxiliary heating gas pressure of 55.00 psi,atomizing gas pressure of-55 psi,curtaingas pressure of-35.00 psi,desolvent temperature of 550 ℃,collision activation scanning energy of 15 e V,collision voltage of35 psi. Component analysis was performed by comparing with the related literature data and the standard chromatogram controlcombined with accurate relative molecular mass of compounds provided by UPLC-Q-TOF-MS. RESULTS:Totally 135 chemicalcomponents were analyzed in ESI+mode,and the 105 chemical components were analyzed in ESI-mode. 11 chemical componentsas coumarin were identified in ESI+mode,such as isoimperatorin,umbelliferone,scopolamine,xanthotoxin,psoralen,Ostenol,fraxidin,isoimperatorin,5-hydroxyl-8-methoxypsoralen,phellopterin,decursin. CONCLUSIONS:The method is accurate andrapid,and can be used for the analysis of chemical components as coumarin in S. divaricata.
OBJECTIVE:To analyze chemical components as coumarin in Saposhnikovia divaricata,and to provide referencefor comprehensive analysis of pharmacodynamic material base in S. divaricata. METHODS:UPLC-Q-TOF-MS method wasadopted. Chromatographic condition:the determination was performed on ACQUITY UPLC BEH C18 column with mobile phaseconsisted of 0.1% formic acid water-0.1% formic acid acetonitrile(gradient elution)at the flow rate of 0.3 mL/min. The columntemperature was 35 ℃,and sample size was 3 μL. MS condition:ESI,in positive and negative ion mode,ESI+/ESI-5 500 V/-4 500 V,declustering potential of 80--80 V,auxiliary heating gas pressure of 55.00 psi,atomizing gas pressure of-55 psi,curtaingas pressure of-35.00 psi,desolvent temperature of 550 ℃,collision activation scanning energy of 15 e V,collision voltage of35 psi. Component analysis was performed by comparing with the related literature data and the standard chromatogram controlcombined with accurate relative molecular mass of compounds provided by UPLC-Q-TOF-MS. RESULTS:Totally 135 chemicalcomponents were analyzed in ESI+mode,and the 105 chemical components were analyzed in ESI-mode. 11 chemical componentsas coumarin were identified in ESI+mode,such as isoimperatorin,umbelliferone,scopolamine,xanthotoxin,psoralen,Ostenol,fraxidin,isoimperatorin,5-hydroxyl-8-methoxypsoralen,phellopterin,decursin. CONCLUSIONS:The method is accurate andrapid,and can be used for the analysis of chemical components as coumarin in S. divaricata.
引文
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[14]吴拾保,邓渝,袁铭铭,等.玉屏风口服液1个异黄酮类及3个色原酮类成分的含量测定[J].药物分析杂志,2016,36(12):2221-2225.
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[22]嵇扬,曾国钱,芮耀诚.欧芹素乙和异欧芹素乙对小鼠腹腔巨噬细胞体外释放肿瘤坏死因子的抑制作用[J].第二军医大学学报,1994,15(6):511-513.
[23]李斌,陈钰妍,李顺祥.飞蛾藤属植物化学成分和药理作用研究进展[J].科技导报,2013,31(11):74-79.
[24]鲁亚奇,张晓,王金金,等.补骨脂化学成分及药理作用研究进展[J].中国实验方剂学杂志,2018,24(20):132-141.
[25]王梦月,贾敏如,马逾英,等.白芷中四种线型呋喃香豆素类成分药理作用研究[J].天然产物研究与开发,2010,22(3):485-489.
[26]李莉,杜纪坤,邹丽宜,等.朝鲜当归源紫花前胡素对LPS损伤THP-1细胞的研究[J].广州化工,2015,43(16):88-90.
[2]赵博,杨鑫宝,杨秀伟,等.防风化学成分的研究[J].中国中药杂志,2010,35(12):1569-1572.
[3]赵常英.中药防风栽培品与野生品药材性状显微组织差异对比[J].中医临床研究,2017,9(25):19-20.
[4]黄彧,吴桐,刘春明,等.防风中色原酮类化学成分的分离及鉴定[J].时珍国医国药,2018,29(7):1558-1561.
[5]李阳,王旭,李壮壮,等.防风化学成分分离鉴定[J].中国实验方剂学杂志,2017,23(15):60-64.
[6]刘亚娟,任晓蕾,霍金海,等.防风色原酮类化学成分的UPLC-Q-TOF/MS分析[J].中国中医药科技,2018,25(3):355-361.
[7]刘双利,姜程曦,赵岩,等.防风化学成分及其药理作用研究进展[J].中草药,2017,48(10):2146-2152.
[8]杨景明,姜华,王紫玮,等.防风多糖的提取分离与含量测定方法研究[J].吉林中医药,2016,36(5):513-516.
[9]王紫玮,杨景明,姜华,等.多糖对抽薹防风药效及其药动学的影响[J].中成药,2015,37(11):2392-2397.
[10]王鹏军.两种不同来源的中药材:防风的鉴别[J].北方药学,2016,13(8):12-13.
[11]王文祎,徐佳,刘杰,等.不同生长方式防风色原酮物质含量测定及差异性分析[J].世界中医药,2015,10(9):1410-1412,1415.
[12]项瑞.高效液相色谱法测定防风中色原酮的含量[J].首都医药,2014,21(18):75-77.
[13]杨景明,姜华,孟祥才.中药防风质量评价的现状与思考[J].中药材,2016,39(7):1678-1681.
[14]吴拾保,邓渝,袁铭铭,等.玉屏风口服液1个异黄酮类及3个色原酮类成分的含量测定[J].药物分析杂志,2016,36(12):2221-2225.
[15]宗亚丽,林玉萍,丁琼娥,等.竹叶防风地上部分的化学成分研究[J].中药材,2007,30(1):42-44.
[16]刘双利.防风类药材的质量评价研究[D].长春:吉林农业大学,2007.
[17]曾丽君.防风质量标准研究及其资源开发[D].沈阳:沈阳药科大学,2008.
[18] RYOSUKE M,ALEXANDRE O,LEXANDRE. Molecu-lar evolution of parsnip(Pastinaca sativa)membrane-bound prenyltransferases for linear and/or angular furano-coumarin biosynthesis[J]. NPH,2016,211(1):332-344.
[19]姜超.防风中有效成分的提取及对实验性肝损伤保护作用的研究[D].长春:吉林农业大学,2013.
[20]阎玉凝,丁书风,郭彦文.防风地区习惯用药的研究Ⅰ:川防风、竹节防风的生药与化学成分[J].西北药学杂志,1988,3(1):31-34.
[21]汪丹,蔡甜,吴志军,等. HPLC-ESI-Q-TOF-MS法分析金钱草颗粒的化学成分[J].中国药房,2016,27(12):1651-1654.
[22]嵇扬,曾国钱,芮耀诚.欧芹素乙和异欧芹素乙对小鼠腹腔巨噬细胞体外释放肿瘤坏死因子的抑制作用[J].第二军医大学学报,1994,15(6):511-513.
[23]李斌,陈钰妍,李顺祥.飞蛾藤属植物化学成分和药理作用研究进展[J].科技导报,2013,31(11):74-79.
[24]鲁亚奇,张晓,王金金,等.补骨脂化学成分及药理作用研究进展[J].中国实验方剂学杂志,2018,24(20):132-141.
[25]王梦月,贾敏如,马逾英,等.白芷中四种线型呋喃香豆素类成分药理作用研究[J].天然产物研究与开发,2010,22(3):485-489.
[26]李莉,杜纪坤,邹丽宜,等.朝鲜当归源紫花前胡素对LPS损伤THP-1细胞的研究[J].广州化工,2015,43(16):88-90.