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[摘要]
目的 利用UPLC-Q-Exactive四极杆-静电场轨道阱高分辨质谱仪联用技术,对粗茎秦艽块根中的化学成分快速识别和鉴定。方法 以100%甲醇作为提取液制备供试液,采用ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm)分离,以乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,质谱采用正负离子监测模式、全扫描及自动触发二级质谱扫描的功能,快速识别和鉴定粗茎秦艽中的化学成分。结果 通过高分辨数据共鉴定34个化学成分,包括环烯醚萜类13个、黄酮类5个、酯类5个、三萜类3个、有机酸类2个、苯丙素类1个、其他类5个,其中12个成分经与对照品比对而准确鉴定,15个化学成分为首次从该植物中分得。结论 UPLC-Q-Exactive四极杆-静电场轨道阱高分辨质谱联用技术可以快速鉴定粗茎秦艽中的化学成分,为粗茎秦艽化学成分的提取分离及其药效物质基础提供科学依据。
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[Abstract]
Objective An ultra-high performance liquid chromatography coupled with hybrid quadrupole-orbitrap mass spectrometry(UPLC-hybrid quadrupole-orbitrap MS) method was developed to rapidly analyze and identify the chemical constituents from the roots of Gentiana crasicaulis.Methods The 100% methanol extract was separated on an ACQUITY UPLC BEH C18 column(100 mm×,2.1 mm,1.7 μm),and eluted with a gradient of methanol-water containing 0.1% formic acid.Constituents in the roots of G.crasicaulis were identified by HRMS in the positive and negative ion modes using both full scan and two-stage threshold-triggered mass modes.Results A total of 34 compounds,including 13 iridoids,5 flavonoids,5 esters,3 triterpenoids,2 organic acids,1 phenylpropanoid,and 5 others compounds were identified.Among them,12 compounds were unambiguously identified by comparing with reference standards.Fifteen compositions wre reported for the first time in the roots of G.crasicaulis.Conclusion Chemical constituents in the roots of G.crasicaulis were identified fast with UPLC-Q-Exactive hybrid quadrupole-orbitrap mass spectrometer technology to provide the scientific basis for the study on the material basis of the separation and crassicaulis chemical constitents.
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[基金项目]
国家留学基金委青年骨干教师出国研修项目(CSC201500850007);四川省科技支撑计划(2014SZ0131);四川省科技厅基础研究项目(2015JY0009);西南民族大学研究生创新型科研项目(CX2015SZ033);西南民族大学大学生创新训练项目(X201610656298