目的 建立超高效液相色谱-四极杆-静电场轨道阱串联质谱(UHPLC-Q-Exactive Orbitrap MS/MS)技术对川乌中生物碱类化学成分进行快速鉴定的方法。方法 采用ACQUITY UHPLC BEH C18柱(2.1 mm×100 mm, 1.7 μm)色谱柱,以0.1%氨水(A)-乙腈(B)为流动相;洗脱程序为0~3 min,0~15% B;3~10 min,15%~40% B;10~16 min,40%~70% B;16~20 min,70%~90%进行梯度洗脱,柱温35 ℃,流速为0.3 mL·min-1,进样量2 μL,正离子模式扫描。结果 最终从川乌中鉴定了141种生物碱类成分。其中单酯型生物碱37种,双酯型生物碱21种,三酯型生物碱2种,醇胺型生物碱80种及其他类生物碱1种。结论 该研究所建立的定性分析方法可系统快速地识别川乌中生物碱类化学成分,并为川乌的作用机制研究和产业开发提供一定的参考依据。
Abstract
OBJECTIVE To establish a method for rapid identificalion of akaloides in Radix Aconitum by Ultrahigh performance liquid chromatography-quadrupole Orbitrap tandem mass spectrometry (UHPLC-Q-ExactiveOrbitrap MS/MS) to rapidly identify the alkaloids in Radix Aconitum. METHODS An ACQUITY UHPLC BEH C18 (2.1 mm×100 mm, 1.7 μm) column was used with 0.1% ammonia (A)-acetonitrile (B) as mobile phases.The elution procedure was 0-3 min, 0-15%B;3-10 min, 15%-40% B;10-16 min, 40%-70% B.The column temperature was maintained at 35 ℃, the flow rate was 0.3 mL·min-1, the sample volume was 2 μL and the scanning mode was positive ion. RESULTS A total of 141 alkaloids were identified from Radix Aconitum. 37 kinds of monoester alkaloids,21 kinds of diester alkaloids,2 kinds of triester alkaloids,80 alkaloids of alcoholamine type and 1 other kind of alkaloids. CONCLUSION The qualitative analysis method established in this paper can be used to identify alkaloid chemical constituents systematically and quickly, and provide a certain reference for the study of action mechanism and industrial development of Radix Aconitum.
关键词
川乌 /
超高效液相色谱-四级杆-静电场轨道阱串联质谱 /
生物碱 /
化学成分分析
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Key words
Radix Aconitum /
UHPLC-Q-ExactiveOrbitrap MS/MS /
alkaloid /
chemical constituent analysis
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中图分类号：
R917
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基金
山东省泰山学者青年专家项目资助(tsqn202103110);山东省中药材及饮片标准研究课题资助(2020-246);山东省青创人才引育团队项目资助(10073004);中国食品药品检定研究院中青年基金资助项目资助(2022A2);中药配方颗粒质量识别与控制关键技术研究及产业化应用项目资助(2021CXGC010511);烟台市省级以上领军人才配套支持计划项目资助
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