目的 应用超高效液相色谱-电喷雾/四极杆飞行时间串联质谱(UPLC-ESI-Q-TOF-MS/MS)技术快速鉴定双参药材的化学成分。方法 采用Acquity UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7 μm)分离,以体积分数0.1%甲酸水溶液(A相)-乙腈(B相)为流动相进行梯度洗脱,流速0.4 mL·min-1,采用电喷雾离子源(ESI),在正、负离子模式下采集数据,扫描范围m/z 100~2 000,通过与对照品的保留时间及质谱数据信息对比,并结合精确相对分子质量、质谱裂解规律、质谱数据库(ChemicalBook, ChemSpider, Pubmed等)及相关文献,对双参的化学成分进行快速鉴定。结果 从彝族药双参中共鉴定出59个化合物,其中包括11个环烯醚萜类、23个有机酸类、14个三萜类、4个糖苷、其他类(1个香豆素类、1个生物碱类、2个酯类、1个多酚类、2个核苷类),其中通过与对照品对比鉴定了8个化合物,分别为绿原酸、隐绿原酸、异绿原酸A、异绿原酸B、异绿原酸C、马钱苷、马钱苷酸和樟芽菜苷。结论 该研究首次采用UPLC-Q-TOF-MS/MS技术对彝族药双参的成分进行了研究,为其质量控制、药效物质基础及体内代谢物分析提供可靠的依据。
Abstract
OBJECTIVE To rapidly identify the chemical constituents of Triplostegia glandulifera Wall by ultra-performance liquid chromatography-electrospray/quadrupole time-of-flight tandem mass spectrometry(UPLC-ESI-Q-TOF-MS/MS). METHODS The separation was performed on Waters Acquity UPLC BEH C18(2.1 mm×100 mm, 1.7 μm) column with gradient elution of 0.1% formic acid(A)-acetonitrile(B) at a flow rate of 0.4 mL·min-1.MS data were collected in positive and negative ion modes,the scanning range was m/z100-2 000, and electrospray ionization(ESI) was employed.The chemical constituents of Triplostegia glandulifera Wall were identified by comparing the retention time and the mass data with those of the reference substances,as well as the accurate mass,MS/MS fragment ions,mass spectrometry databases(ChemicalBook, ChemSpider, Pubmed andothers) and related literature. RESULTS Fifty-nine compounds from Triplostegia glandulifera Wall were identified, including 11 iridoids, 23 organic acids, 14 triterpenoids, 4 glycosides and others(one coumarin, one alkaloid, two esters, one phenolic acid and two nucleosides).Among them, eight compounds were identified by comparison with the reference substances, including chlorogenic acid, cryptochlorogenic acid, isochlorogenic acid A, isochlorogenic acid B,isochlorogenic acid C, loganin, ferulic acid and sweroside. CONCLUSION This research is the first one to study the chemical constituents of Yi nationality medicine Triplostegia glandulifera Wall, which provides a reference for the quality control,material basis and in vivo metabolic analysis.
关键词
彝族药 /
双参 /
超高效液相色谱-电喷雾/四极杆飞行时间串联质谱法 /
皂苷 /
环烯醚萜 /
有机酸 /
裂解规律
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Key words
Yi nationality medicine /
Triplostegia glandulifera Wall /
ultra-performance liquid chromatography-electrospray/quadrupole time-of-flight tandem mass spectrometry(UPLC-ESI-Q-TOF-MS/MS) /
saponin /
iridoid /
organic acid /
fragmentation pattern
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中图分类号：
R917
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参考文献
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脚注
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基金
中央引导地方科技发展资金项目资助(206Z2501G);河北省重点研发计划项目资助(20372502D);河北省自然科学基金项目资助(H2019423050)
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