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引用本文:李晶,张屏.HPLC-Q-Exactive-MS/MS法快速分析蒙药材悬钩子木中的化学成分[J].中国现代应用药学,2024,41(11):47-55.
lijing,zhangping.Rapid analysis of chemical constituents in Rubus sachalinensis Leveille by HPLC-Q-Exactive-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2024,41(11):47-55.
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HPLC-Q-Exactive-MS/MS法快速分析蒙药材悬钩子木中的化学成分
李晶, 张屏
内蒙古医科大学药学院
摘要:
摘要:目的:采用高效液相色谱串联四极杆-静电场轨道阱高分辨质谱(HPLC-Q-Exactive-MS/MS)法快速分析蒙药材悬钩子木化学成分。方法:采用 CAPCELL PAK MGII C18(4.6?250 mm, 5 μm)色谱柱,以乙腈(A)- 0.1%甲酸水溶液(B)为流动相进行梯度洗脱,体积流量1.0 mL?min-1,进样体积20 μL,柱温30℃,热电喷雾(HESI)质谱离子源,在负离子模式下采集数据。结果:依据精确质量数和Chemspider、Pubchem数据库确定化合物分子式及结构式,通过比较对照品及文献报道的保留时间、一级质谱以及二级碎片离子,结合此类化合物的裂解规律,从悬钩子木中共鉴定出71个化学成分,包括30个有机酸类、22个黄酮类、7个三萜皂苷类、5个香豆素类、1个木质素类、1个没食子鞣质和2个芳香族化合物。结论:该方法可快捷、准确的鉴定悬钩子木中复杂化学成分,为悬钩子木的药效物质基础研究提供科学依据。
关键词:  悬钩子木  HPLC-Q-Exactive-MS/MS  化学成分  成分归属
DOI:
分类号:
基金项目:国家自然科学基金项目
Rapid analysis of chemical constituents in Rubus sachalinensis Leveille by HPLC-Q-Exactive-MS/MS
lijing, zhangping
College of Pharmacy,Inner Mongolia Medical University
Abstract:
ABSTRACT: OBJECTIVE To rapidly analyze the chemical constituents of Rubus sachalinensis Leveille by HPLC-Q-Exactive-MS/MS. METHODS Chromatographic separation was carried out on an CAPCELL PAK MGII C18(4.6?250 mm, 5 μm)at the temperature of 30℃. The mobile phase was 0.1% formic acid and acetonitrile by gradient elution, with a flow rate at 1.0 mL?min-1, and the injection volume of 20 μL. The MS spectrum was acquired in negative ion modes using HESI ion source. RESULTS The molecular and structural formulae of the compounds were determined based on the exact mass number and Chemspider and Pubchem databases. By comparing the retention times of the corresponding reference standards and those reported in the literature, primary mass spectra, and secondary mass spectrometry pyrolysis fragments, combined with fragmentation regularity of such compounds, a total of 71 compounds were identified from Rubus sachalinensis Leveille, including 30 organic acids, 22 flavonoids, 7 triterpenoid saponins, 5 coumarins, 1 lignan, 1 gallotannin and 2 aromatic compounds. CONCLUSION This method can quickly and accurately identify the complex chemical constituents in Rubus sachalinensis Leveille, and provide scientific basis for the basic research on the medicinal substances of Rubus sachalinensis Leveille.
Key words:  Rubus sachalinensis Leveille  HPLC-Q-Exactive-MS/MS  chemical constituents  compositional attribution
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