结肠炎奇效颗粒中化学成分的UPLC-Q-TOF/MSE分析

Analysis of Chemical Constituents in Jiechangyan Qixiao Granules Based on UPLC-Q-TOF/MS

目的:为了系统分析复方中药结肠炎奇效颗粒的化学组成,采用超高效液相色谱-四极杆-飞行时间串联质谱法(UPLC-Q-TOF/MSE)对该制剂中主要化学成分进行了快速鉴定和归属。方法:色谱条件采用ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.8μm),流动相0.1%甲酸水溶液(A)-乙腈(B)进行梯度洗脱(0~2 min,5%B;2~16 min,5%~21%B;16~30 min,21%~95%B;30~33 min,95%B;33~34 min,95%~5%B;34~37 min,5%B),流速0.3 mL·min-1,柱温30℃,进样量2μL。质谱分析使用电喷雾离子源(ESI),正、负离子模式扫描,扫描范围m/z 60~1 200,MSE模式采集数据。通过与对照品、参考文献和自建数据库信息比对后对各离子峰进行鉴定。结果:从结肠炎奇效颗粒中共分离和鉴定出102个化学成分,包括有机酸类、黄酮及其苷类、三萜类、苯乙醇苷类、鞣质类、环烯醚萜苷类等,其中黄酮及其苷类主要来源于骨碎补和山楂,苯乙醇苷类和环烯醚萜苷类来源于车前子,三萜类和鞣质类主要来源于山楂和诃子,且已鉴定化学成分包含骨碎补中成分28个,车前子中成分31个,诃子肉中成分53个以及山楂中成分58个。结论:建立的UPLC-Q-TOF/MSE能全面快速地分析结肠炎奇效颗粒中的化学成分,初步阐明了该颗粒剂的化学成分轮廓,可为其药效物质基础及质量控制研究奠定基础。

Objective: In order to systematically clarify the chemical composition of Jiechangyan Qixiao granules,the main chemical components in this preparation were rapidly identified and assigned by ultraperformance liquid chromatography-quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF/MSE).Method: ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.8 μm)was employed for UPLC analysis with the mobile phase of 0.1% formic acid aqueous solution(A)-acetonitrile(B)for gradient elution(0-2 min,5%B;2-16 min,5%-21%B;16-30 min,21%-95%B;30-33 min,95%B;33-34 min,95%-5%B;34-37 min,5%B). The flow rate was 0.3 mL·min-1,the column temperature was 30 ℃,and the volume of sample injection was 2 μL. Electrospray ionization(ESI)was applied for scanning under positive and negative ion modes with the scanning range of m/z 60-1 200. MSEmode was used to collect mass spectral data. The ion peaks were identified by comparing with the information of control substances,literature references and self-built database.Result: A total of 102 chemical components were separated and identified in Jiechangyan Qixiao granules,including organic acids,flavonoids and its glycosides,triterpenes,phenylethanoid glycosides,tannins,iridoid glycosides and other components,among which flavonoids and its glycosides were from Drynariae Rhizoma and Crataegi Fructus,phenylethanoid glycosides and iridoid glycosides were from Plantaginis Semen,triterpenoids and tannins were from Crataegi Fructus and Chebulae Fructus. Among the identified chemical constituents,there were 28 from Drynariae Rhizoma,31 from Plantaginis Semen,53 from Chebulae Fructus and 58 ingredients from Crataegi Fructus. Conclusion: The established UPLC-Q-TOF/MSEcan comprehensively and rapidly analyze the chemical constituents in Jiechangyan Qixiao granules,and preliminarily elucidates the chemical composition profile of this granules,which can lay a foundation for further research on the pharmacodynamic material basis and quality control of Jiechangyan Qixiao granules.