基于UPLC-Q-TOF/MS的连桂宁心汤体外与入血成分分析及鉴定  

Analysis and Indentification of Chemical Components and Blood Components of Liangui Ningxin Decoction(连桂宁心汤)by UPLC-Q-TOF/MS

作　　者：陈金红 陈涵 叶雨佳 黄冰慧 李晓凤[3] 杜武勋[3] 刘志超 CHEN Jinhong;CHEN Han;YE Yujia;HUANG Binghui;LI Xiaofeng;DU Wuxun;LIU Zhichao(School of Rehabilitation Medicine,Shandong Second Medical University,Weifang 261053,Shandong,China;Gaoqiao Community Health Service Center in Yinhu Street of Fuyang District,Hangzhou 311400,Zhejiang,China;Second Affiliated Hospital of Tianjin University of Traditional Chinese Medicine,Tianjin 300250,China)

机构地区：[1]山东第二医科大学康复医学院,山东潍坊261053 [2]杭州市富阳区银湖街道高桥社区卫生服务中心,浙江杭州311400 [3]天津中医药大学第二附属医院,天津300250

出　　处：《辽宁中医杂志》2024年第6期138-143,I0006,共7页Liaoning Journal of Traditional Chinese Medicine

基　　金：国家自然科学基金项目(82004329);山东省医药卫生科技项目(202303011361);山东省中医药科技项目(Q-2023006);潍坊市科技发展计划项目(医学类)(2022YX044,2022YX045)。

摘　　要：目的采用超高效液相色谱-四级杆-飞行时间质谱(ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry,UPLC-Q-TOF-MS)对连桂宁心汤化学成分和入血成分进行分析,初步阐明其可能的药效物质基础。方法采用ACQUITYTM UPLC BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm),流动相为A(0.1%甲酸的水溶液)-B(0.1%甲酸的乙腈溶液),梯度洗脱,柱温为45℃,进样量为5μL。采用电喷雾离子源,正/负离子双模式检测,离子源温度120℃,脱溶剂和雾化气为高纯N_(2),锥孔N_(2)反吹流量50 L/h,锥孔电压30 V;毛细管电压3.0 kV(正)/2.0 kV(负);脱溶剂温度450℃,流量800 L/h;分子量范围50~1200 Da。结果结合文献报道和一级MS、二级MS/MS高分辨质谱数据,在连桂宁心汤水煎液中鉴定出68个成分,以黄酮类、生物碱类、三萜类为主,在给药大鼠血浆样本中鉴定出33个成分,以黄酮类、生物碱类、三萜类、挥发油类为主,其中黄酮类及生物碱类鉴定出的成分数量及丰度较体外明显降低。结论UPLC/Q-TOF MS/MS技术是鉴定中药复方成分的有效手段,结合连桂宁心汤化学成分及其入血成分,初步阐明连桂宁心汤的药效物质基础,为探讨其作用机制及其质量控制提供了有效的科学依据。Objective To analyze the chemical components and blood components of Liangui Ningxin Decoction(连桂宁心汤),and preliminarily clarify its possible medicinal substances basis by ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF-MS).Methods An ACQUITY UPLC BEH C_(18)column(2.1 mm×100 mm,1.7μm)was used,with A(0.1%formic acid aqueous solution)-B(0.1%formic acid acetonitrile solution)for gradient elution under column temperature of 45℃.The injection volume was 5μL.The electrospray ion source was used for scanning in positive and negative ion modes.Ion source temperature was 120℃.The desolvention and atomized gas were high purity N_(2),the cone N 2 backflush flow was 50L/h,and the cone voltage was 30 V.The capillary voltage was 3.0 kV(Positive)/2.0 kV(Negative).The desolventing temperature was 450℃,and the flow rate was 800L/h.Molecular weight range was 50-1200 Da.Results Combined with literature reports and primary MS and secondary MS/MS high resolution mass spectrometry data,68 components were identified in the decoction liquid of Liangui Ningxin Decoction,mainly flavonoids,alkaloids and triterpenoids,and 33 components were identified in the plasma samples of administered rats,mainly flavonoids,alkaloids,triterpenoids and volatile oils,of which the number and abundance of components identified by flavonoids and alkaloids were significantly reduced compared with in vitro.Conclusion UPLC/Q-TOF-MS is an effective method to identify the components of traditional Chinese medicine compound.Combined with the analysis of the chemical components and blood components of Liangui Ningxin Decoction,the medicinal substances basis of Liangui Ningxin Decoction was preliminarily elucidated,which provided an effective scientific basis for exploring its mechanism of action and its quality control.

关 键 词：连桂宁心汤 UPLC-Q-TOF/MS 化学成分 入血成分 药效物质基础 

分 类 号：R284[医药卫生—中药学]