基于UPLC-Q-Exactive Orbitrap-MS的固公果根指纹图谱分析及DPPH抗氧化谱效关系研究

康荣, 程显隆, 姚令文, 李明华, 余坤子, 魏锋, 马双成

中国药学杂志 ›› 2023, Vol. 58 ›› Issue (18) : 1664-1670.

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中国药学杂志
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中国药学杂志 ›› 2023, Vol. 58 ›› Issue (18) : 1664-1670. DOI: 10.11669/cpj.2023.18.006
动植物来源药品质量控制研究

基于UPLC-Q-Exactive Orbitrap-MS的固公果根指纹图谱分析及DPPH抗氧化谱效关系研究

  • 康荣, 程显隆, 姚令文, 李明华, 余坤子, 魏锋*, 马双成*
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Quality Analysis of Rosa odorata Sweet var. gigantean Root Based on UPLC-Q-Exactive Orbitrap-MS Fingerprint and Antioxidant Effect of DPPH Spectrum-Effect Relationship

  • KANG Rong, CHENG Xianlong, YAO Lingwen, LI Minghua, YU Kunzi, WEI Feng*, MA Shuangcheng*
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摘要

目的 建立固公果根药材的超高效液相色谱串联四极杆-静电场轨道阱质谱(UPLC-Q-Exactive Orbitrap-MS)指纹图谱,并研究其与自由基清除活性的谱效关系。方法 采用UPLC-Q-Exactive Orbitrap-MS建立固公果根的指纹图谱,评价指纹图谱相似度,结合热图分析,对其中的19个共有峰进行指认;使用1,1-二苯基-2-三硝基苯肼(DPPH)法评价固公果根的抗氧化活性,结合灰色关联度分析(grey relational analysis,GRA)研究谱效关系。结果 建立了固公果根的UPLC-Q-Exactive Orbitrap-MS指纹图谱,选择峰面积>1%的19个色谱共有峰,通过对照品比对法、数据库、参考文献等方法鉴定前述色谱峰。19个色谱峰的热图分析和DPPH抗氧化灰色关联度结果显示,面积颜色变动较大峰为2、4、8、14、15、17,谱效关系表明11、18、17、19、8、6、16、12、1、5、7、15号峰是与抗氧化活性关联较大的正相关峰。各取排名前五相交得以下9个化学成分作为质量评价指标:峰2(儿茶素)、峰4(表儿茶素)、峰8[(+)-喹色亭酚-(4β,8)-表儿茶素]、峰11(鞣花酸)、峰14(野蔷薇苷)、峰15(刺梨苷)、峰17(委陵菜酸)、峰18(蔷薇酸)和峰19(皂皮酸)。结论 固公果根抗氧化活性是酚类和三萜皂苷类等多成分联合效应的结果,为药材质量控制提供更全面的参考。

Abstract

OBJECTIVE To establish the UPLC-Q-Exactive Orbitrap-MS fingerprint of Rosa odorata Sweet var. gigantean root and study the spectrum-effect relationship of its free radical scavenging activity. METHODS The fingerprint of Rosa odorata Sweet var. gigantean root was established by UPLC-Q-Exactive Orbitrap-MS method, the similarity of the fingerprint was evaluated, and 19 common peaks were evaluated by heat map analysis. The antioxidant activity of Rosa odorata Sweet var. gigantean root was evaluated by1,1-diphenyl-2-trinitrophenylhydrazine (DPPH) method, and the spectrum-effect relationship was studied by grey correlation analysis (grey relational analysis, GRA). RESULTS The UPLC-Q-Exactive Orbitrap-MS fingerprint of Rosa odorata Sweet var. gigantean root was established, and 19 common chromatographic peaks with Area %>1% were selected, and the chromatographic peaks were identified by reference method, database and reference. According to the heat map analysis of 19 peaks and the grey correlation degree of DPPH oxidation resistance, the heat map analysis of 19 peaks showed that the peaks with large area color changes were 2, 4, 8, 14, 15, 17. The spectrum-effect relationship showed that peaks 11, 18, 17, 19, 8, 6, 16, 12, 1, 5, 7 and 15 were positively correlated with antioxidant activity. The following nine peaks were selected from the top five as quality evaluation indexes, Peak 2 (catechin), Peak 4 (epicatechin), Peak 8 [(+)-fisetinidol-(4β, 8)-epicatechin], Peak 11 (ellagic acid), Peak 14 (rosamultin), Peak 15 (kaji-ichigoside F1), Peak 17 (2α, 3β, 19α-trihydroxyurs-12-en-28-oic acid), Peak 18 (euscaphic acid), Peak 19 (quillaic acid). CONCLUSION The antioxidant activity of Rosa odorata Sweet var. gigantean root is the result of the combined effect of multi-components such as phenols and triterpenoid saponins, which provides a more comprehensive reference for the quality control of medicinal materials.

关键词

固公果根 / 超高效液相色谱串联四极杆-静电场轨道阱质谱 / 指纹图谱 / 1,1-二苯基-2-三硝基苯肼抗氧化活性 / 谱效关系

Key words

Rosa odorata Sweet var. gigantean root / UPLC-Q-Exactive Orbitrap-MS / fingerprint pectrum / DPPH antioxidant activity / spectrum-effect relationship

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康荣, 程显隆, 姚令文, 李明华, 余坤子, 魏锋, 马双成. 基于UPLC-Q-Exactive Orbitrap-MS的固公果根指纹图谱分析及DPPH抗氧化谱效关系研究[J]. 中国药学杂志, 2023, 58(18): 1664-1670 https://doi.org/10.11669/cpj.2023.18.006
KANG Rong, CHENG Xianlong, YAO Lingwen, LI Minghua, YU Kunzi, WEI Feng, MA Shuangcheng. Quality Analysis of Rosa odorata Sweet var. gigantean Root Based on UPLC-Q-Exactive Orbitrap-MS Fingerprint and Antioxidant Effect of DPPH Spectrum-Effect Relationship[J]. Chinese Pharmaceutical Journal, 2023, 58(18): 1664-1670 https://doi.org/10.11669/cpj.2023.18.006
中图分类号： R282   

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基金

国家重点研发计划项目资助(2019YFC1711500);中国食品药品检定研究院中青年发展研究基金课题资助(2022A5-1020052210205)

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