基于UHPLC-Q-Exactive Orbitrap MS技术的正心降脂片化学成分研究

Chemical Constituents of Zhengxin Jiangzhi Tablets Based on UHPLC-Q-Exactive Orbitrap MS

目的建立一种快速鉴定中药复方制剂正心降脂片的高分辨质谱分析方法,系统阐明其化学成分组成。方法采用超高效液相色谱静电场轨道阱高分辨质谱(UHPLC-Q-Exactive Orbitrap MS)对正心降脂片成分进行分析,色谱柱为Thermo Accucore aQ RP18(2.1 mm×150 mm,2.6μm),流动相采用乙腈(A)-0.1%甲酸水(B)进行梯度洗脱,流速0.3 mL·min^(-1)。采用加热电喷雾离子源,正、负离子同时扫描模式采集数据。根据一级准分子离子精确质荷比、二级质谱碎片离子信息、文献报道和对照品比对鉴定正心降脂片的化学成分。结果共鉴定了正心降脂片中105个化学成分,包括21个有机酸、59个黄酮类化合物(黄酮氧苷类37个,黄酮碳苷类10个,多甲氧基黄酮类化合物12个)、19个醌类化合物(11个蒽醌类和8个菲醌类)、3个二苯乙烯类化合物及3个其他类型化合物。其中29个化合物采用对照品比对进行了鉴定,并对各成分的药材来源进行了归属。结论对正心降脂片的化学成分进行了系统、全面地分析,为其药效物质基础、质量控制及作用机制研究奠定了基础。

OBJECTIVE To clarify the chemical constituents of Zhengxin Jiangzhi tablets systematically and establish a rapid a-nalysis method for this traditional Chinese medicine preparation.METHODS UHPLC-Q-exactive orbitrap MS was used to analyze the compounds of Zhengxin Jiangzhi tablets.The chromatographie separation was performed on a Thermo AccucoreaQ RP18(2.1 mm×150 mm,2.6μm)column with gradient elution using acetonitrile(A)-0.1%formic acid-water(B)as the mobile phase.The flow rate was 0.3 mL·min^(-1) A heated electrospray ion source was used to ionize compounds.The MS and MS^(2) data was collected in positive and negative ion modes simulaneously.The chemical constituents of Zhengxin Jiangzhi tablets were idenified based on accurate MS data,fragmentation characteristics of MS^(2),published literature,and reference standards.RESULTS A total of 105 chemical constituents from Zhengxin Jiangzhi tablets were identifed,including 21 organic acids,59 flavones(37 flavone O-glycosides,10 flavone C-glyco-sides,12 polymethoxy flavones),19 quinones(11 anthraquinones and 8 phenanthraquinones),3 stilbenes,and 3 other types of com-pounds.29 compounds were identifed by comparison with reference standards,and the herb sources of each compound were assigned.CONCLUSION The chemical constituents of Zhengxin Jiangzhi tablets are characterized systematically,which lays a foundation for the study of its pharmacodynamic material basis,quality control,and action mechanism.