基于UPLC-Q-TOF-MS/MS技术的短管兔耳草化学成分快速识别研究Fast identification of constituents of Lagotis brevituba by using UPLC-Q-TOF-MS/MS method
谢晶;张丽;曾金祥;李敏;王娟;谢雄雄;钟国跃;罗光明;袁金斌;梁健;
XIE Jing;ZHANG Li;ZENG Jin-xiang;LI Min;WANG Juan;XIE Xiong-xiong;ZHONG Guo-yue;LUO Guang-ming;YUAN Jin-bin;LIANG Jian;Research Center of Traditional Chinese Medicine Resources and Minority Medicine,Jiangxi University of Traditional Chinese Medicine;Department of Budget and Finance,Jiangxi University of Traditional Chinese Medicine;
摘要(Abstract):
采用超高效液相色谱-串联四极杆飞行时间质谱(UPLC-Q-TOF/MS)技术快速分析鉴别短管兔耳草的化学成分,为其临床应用提供参考依据,试验采用UPLC-Q-TOF-MS/MS仪器,YMC-Triart C_(18)色谱柱(2.1 mm×100 mm,1.9μm),以乙腈-0.2%甲酸水溶液为流动相梯度洗脱;质谱采用电喷雾(ESI)离子源,在负离子模式下采集数据,通过保留时间、精确分子离子峰和二级质谱裂解碎片,并结合参考文献,对短管兔耳草成分进行鉴定,该实验共鉴别出22个化合物,其中黄酮类化合物11个,苯乙醇苷类化合物6个,环烯醚萜类化合物1个,有机酸类化合物4个。UPLC-Q-TOF-MS/MS方法能快速鉴别短管兔耳草中的各类化学成分,方法简单,快速,可为短管兔耳草的临床应用提供物质依据。
The chemical constituents of Lagotis brevituba were rapidly determined and analyzed by using ultra performance liquid chromatography tandem quadrupole time of flight mass spectrometry( UPLC-Q-TOF-MS/MS) method,providing material basis for the clinical application of L. brevituba. The separation was performed on UPLC YMC-Triart C_(18)(2. 1 mm × 100 mm,1. 9 μm) column,with acetonitrile-water containing 0. 2% formic acid as mobile phase for gradient elution. The flow rate was 0. 4 mL ·min(-1)gradient elution and column temperature was 40 ℃,the injection volume was 2 μL. ESI ion source was used to ensure the data collected in a negative ion mode. The chemical components of L. brevituba were identified through retention time,exact relative molecular mass,cleavage fragments of MS/MS and reported data. The results showed that a total of 22 compounds were identified,including 11 flavones,6 phenylethanoid glycosides,1 iridoid glucosides,and 4 organic acid. The UPLC-Q-TOF-MS/MS method could fast identify the chemical components of L. brevituba,providing valuable information about L. brevituba for its clinical application.
关键词(KeyWords):
短管兔耳草;UPLC-Q-TOF-MS/MS;化学成分;快速鉴别
Lagotis brevituba;UPLC-Q-TOF-MS/MS;chemical constituents;fast identification
基金项目(Foundation): 国家自然科学基金项目(81660648)
作者(Authors):
谢晶;张丽;曾金祥;李敏;王娟;谢雄雄;钟国跃;罗光明;袁金斌;梁健;
XIE Jing;ZHANG Li;ZENG Jin-xiang;LI Min;WANG Juan;XIE Xiong-xiong;ZHONG Guo-yue;LUO Guang-ming;YUAN Jin-bin;LIANG Jian;Research Center of Traditional Chinese Medicine Resources and Minority Medicine,Jiangxi University of Traditional Chinese Medicine;Department of Budget and Finance,Jiangxi University of Traditional Chinese Medicine;
DOI: 10.19540/j.cnki.cjcmm.20170307.012
参考文献(References):
- [1]曹明泽,孔小军,王磊,等.藏药研究概况[J].动物医学进展,2015,36(8):105.
- [2]刘利敏.藏药短管兔耳草总黄酮抗炎解热镇痛作用研究[D].兰州:兰州大学,2010.
- [3]王燕,张应鹏,马兴铭.短管兔耳草正丁醇提取物诱导胃癌SGC-7901细胞凋亡的研究[J].中成药,2007,29(5):672.
- [4]杨柏龄,侯茜,胡峰,等.短管兔耳草总黄酮降低阿尔茨海默病模型小鼠大脑皮层及海马组织炎性细胞因子的水平[J].细胞与分子免疫学杂志,2016,37(7):881.
- [5]曾金祥,许兵兵,李敏,等.藏药短管兔耳草醇提物降低急性高尿酸血症小鼠血尿酸水平及机制研究[J].中国新药杂志,2015,24(21):2489.
- [6]朱继孝,张红阳,李雪溦,等.两种兔耳草对四氯化碳致肝损伤小鼠保护作用的比较研究[J].中药新药与临床药理,2016,27(2):210.
- [7]苑祥,张莉,赵建强,等.短管兔耳草化学成分研究[J].中草药,2015,46(10):1437.
- [8]Yuan X,Wen H X,Zhao J Q,et al.Phytochemical and chemotaxonomic study on Lagotis brevituba(Scrophulariaceae)[J].Biochem Syst Ecol,2016,66:8.
- [9]Li S L,Song J Z,Qiao C F,et al.A novel strategy to rapidly explore potential chemical markers for the discrimination between raw and processed Radix Rehmanniae by UHPLC-TOF-MS with multivariate statistical analysis[J].J Pharm Biomed Anal,2010,51(4):812.
- [10]Li Z,Song X,Fu Z,et al.Identification of the major constituents in Zhimu-Huangqi herb-pair extract and their metabolites in rats by LCESI-MSn[J].Chromatographia,2013,76(13/14):767.
- [11]Shi Y,Wu C,Chen Y,et al.Comparative analysis of three Callicarpa herbs using high performance liquid chromatography with diode array detector and electrospray ionization-trap mass spectrometry method[J].J Pharm Biomed Anal,2013,75(5):239.
- [12]马志国,杨中林,冯云鹏.大鼠口服松果菊苷粪便中代谢物的HPLC-MSn分析[J].中国天然药物,2008,6(5):387.
- [13]Vallverdú-Queralt A,Alvarenga J F R,Estruch R,et al.Bioactive compounds present in the Mediterranean sofrito[J].Food Chem,2013,141(4):3366.
- [14]罗光明,黄远亮.肉苁蓉松果菊苷药理作用研究进展[J].亚太传统医药,2014,10(17):58.
- [15]孙秀漫.广东紫珠物质基础及其主要活性成分的药代动力学研究[D].广州:广州中医药大学,2015.
- [16]Liu R,Zhang J,Liang M,et al.Simultaneous analysis of eight bioactive compounds in Danning tablet by HPLC-ESI-MS and HPLC-UV[J].J Pharm Biomed Anal,2007,43(3):1007.
- [17]万茵,谢明勇,曾小星.车前子总黄酮的纯化及其成分的液相质谱联用分析[J].食品科学,2008,29(2):328.
- [18]李文兰,白晶,臧宝珊,等.HPLC-ESI-Q-TOF-MS/MS分析肉苁蓉拟雌激素活性部位入血成分[J].质谱学报,2015,36(3):223.
- [19]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.
- [20]王放.基于LC-HR-MSn的苦碟子及血栓通注射剂化学成分研究[D].北京:北京中医药大学,2014.
- [21]潘正.基于ITS2条形码和代谢组技术的藏药独一味品质评价研究[D].成都:成都中医药大学,2015.
- [22]郭盼盼.广金钱草总黄酮纯化工艺优化及总黄酮提取物的抗氧化活性,定性和定量研究[D].石家庄:河北医科大学,2015.
- [23]Barreca D,Bellocco E,Leuzzi U,et al.First evidence of C-and O-glycosyl flavone in blood orange Citrus sinensis(L.)Osbeck juice and their influence on antioxidant properties[J].Food Chem,2014,149(8):244.
- [24]Es-Safi N E,Kerhoas L,Ducrot P H.Fragmentation study of globularin through positive and negative ESI/MS,CID/MS,and tandem MS/MS[J].Spectrosc Lett,2007,40(5):695.
- [25]李伟,冯育林,黎田儿,等.UPLC-Q-TOF/MS技术结合诊断离子方法快速分析连钱草中黄酮类化合物[J].质谱学报,2016,37(6):504.
- [26]Li X Q,Sun X H,Cai S,et al.Investigation on the chemical constituents and variation of the flower buds of Lonicera species by UPLC-ESI-MS/MS and principle component analysis[J].Acta Pharm Sin,2009,44(8):895.
- [27]张小平,蒋可志,吕惠卿,等.HPLC-Q-TOF-MS鉴定条叶榕根茎乙酸乙酯提取物中的主要化学成分[J].质谱学报,2015,36(4):310.
- [28]芮雯,冯毅凡,石忠峰,等.不同产地黄芪药材的UPLC-Q-TOFMS指纹图谱研究[J].药物分析杂志,2012,32(4):607.
- [29]钟艳梅,冯毅凡,郭姣.基于UPLC-Q-TOF-MS技术的白术药材化学成分快速识别研究[J].质谱学报,2015,36(1):72.
- [30]黄凯,杨新波,黄正明.金丝桃苷药理作用研究进展[J].医药导报,2009,28(8):1046.
- [31]王伟,张犁.木犀草素抗肿瘤作用的研究进展[J].东南大学学报:医学版,2014,33(2):218.
- [32]牟艳玲,胡志力,周玲,等.木犀草素-7-O-β-D-葡萄糖苷对H2O2诱导乳鼠心肌细胞损伤的保护作用[J].山东中医药大学学报,2009,33(1):63.
- [33]曾金祥,许兵兵,王娟,等.车前子中毛蕊花糖苷及异毛蕊花糖苷降低急性高尿酸血症小鼠血尿酸水平及其机制[J].中成药,2016,38(7):1449.
- [34]Deng M,Zhao J Y,Tu P F,et al.Echinacoside rescues the SHSY5Y neuronal cells from TNFα-induced apoptosis[J].Eur J Pharmacol,2004,505(1):11.
- [35]宁强,彭大颖,高志安.原儿茶酸调控PPARγ通路对小鼠胆总管梗阻肠屏障损伤的保护作用[J].中药药理与临床,2013,29(4):27.
- 短管兔耳草
- UPLC-Q-TOF-MS/MS
- 化学成分
- 快速鉴别
Lagotis brevituba - UPLC-Q-TOF-MS/MS
- chemical constituents
- fast identification
- 谢晶
- 张丽
- 曾金祥
- 李敏
- 王娟
- 谢雄雄
- 钟国跃
- 罗光明
- 袁金斌
- 梁健
XIE Jing- ZHANG Li
- ZENG Jin-xiang
- LI Min
- WANG Juan
- XIE Xiong-xiong
- ZHONG Guo-yue
- LUO Guang-ming
- YUAN Jin-bin
- LIANG Jian
- Research Center of Traditional Chinese Medicine Resources and Minority Medicine
- Jiangxi University of Traditional Chinese Medicine
- Department of Budget and Finance
- Jiangxi University of Traditional Chinese Medicine
- 谢晶
- 张丽
- 曾金祥
- 李敏
- 王娟
- 谢雄雄
- 钟国跃
- 罗光明
- 袁金斌
- 梁健
XIE Jing- ZHANG Li
- ZENG Jin-xiang
- LI Min
- WANG Juan
- XIE Xiong-xiong
- ZHONG Guo-yue
- LUO Guang-ming
- YUAN Jin-bin
- LIANG Jian
- Research Center of Traditional Chinese Medicine Resources and Minority Medicine
- Jiangxi University of Traditional Chinese Medicine
- Department of Budget and Finance
- Jiangxi University of Traditional Chinese Medicine