HPLC-Q-TOF-MS在线筛选鉴定牡丹花中的抗氧化成分

doi:10.3976/j.issn.1002-4026.2022.05.002

摘要/Abstract

摘要：

建立高效液相色谱-四级杆-飞行时间质谱结合在线清除1,1-二甲苯-2-三硝基苯肼模式,实现牡丹花中的抗氧化活性成分的快速筛选与鉴定。采用Waters X-Bridge C₁₈色谱柱,以乙腈-水(0.1%甲酸)为流动相,分别采用电喷雾正、负离子模式对牡丹花进行分析。样品经高效液相色谱分离后与自由基溶液混合发生清除反应,采用飞行时间质谱进行成分的快速鉴定。结果表明,负离子模式下,通过飞行时间质谱获得的精准分子质量对照文献进行推测,从牡丹花中鉴定出15种成分,其中5种抗氧化成分。该方法可以实现对天然产物复杂体系中抗氧化成分的快速定向筛选和鉴定,同时为牡丹花的进一步研究提供科学依据。

关键词: 牡丹花, 抗氧化, 在线筛选, 飞行时间质谱

Abstract:

A high performance liquid chromatography-quadrupole time of flight mass spectrometry (HPLC-Q-TOF-MS) combined with on-line removal of 1,1-diphenyl-2-picrylhydrazyl (DPPH) model was established for the rapid screening and identification of antioxidant active ingredients in peony flowers. Waters X-Bridge C₁₈ chromatographic column was used with acetonitrile-water (0.1% formic acid) as the mobile phase. The peony flower samples were analyzed using electrospray positive and negative ion modes. The samples separated using HPLC were mixed with free-radical solution, and the mixture was entered into HPLC-Q-TOF-MS for rapid identification. In total, 15 ingredients and 5 antioxidant compounds were identified in the negative ion mode. This method is a simple method for rapid screening and identification of antioxidant compounds in a complex system of natural products. Furthermore, it can also provide scientific basis for further studies on peony flower.

Key words: peony flower, antioxidant activity, on-line screening, HPLC-Q-TOF-MS

中图分类号:

O657.72

田璇, 刘宇, 朱文卿, 郑振佳. HPLC-Q-TOF-MS在线筛选鉴定牡丹花中的抗氧化成分[J]. 山东科学, 2022, 35(5): 10-15.

TIAN Xuan, LIU Yu, ZHU Wen-qing, ZHENG Zhen-Jia. Identification of antioxidant components in peony flowers through on-line screening using high performance liquid chromatography-quadrupole time of flight mass spectrometer[J]. Shandong Science, 2022, 35(5): 10-15.

图/表 3

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表1

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序号	选择离子	实验值m/z	分子式	化合物推断结果	参考文献
1	[M-H]^-	331.055 4	C₁₃H₁₆O₁₀	1-没食子酸酰葡萄糖或6-没食子酸酰葡萄糖	[23-24]
2	[M-H]^-	169.007 7	C₇H₆O₅	没食子酸	[29]
3	[M-H]^-	495.124 5	C₂₃H₂₈O₁₂	氧化芍药苷	[27]
4	[M-H]^-	609.111 8	C₂₇H₃₀O₁₆	山奈酚-3,7-二-O-葡萄糖苷或山柰酚3-O-β-D-半乳糖(2→1)-β-D-葡萄糖苷	[25-26]
5	[M-H]^-	525.128 5	C₂₄H₃₀O₁₃	牡丹皮苷-E	[30]
6	[M-H]^-	197.033 5	C₉H₁₀O₅	没食子酸乙酯	[21]
7	[M-H]^-	639.115 6	C₂₈H₃₂O₁₇	异鼠李素-3,7-二-O-葡萄糖	[25]
8	[M-H]^-	653.129 3	—	未知
9	[M-H]^-	447.064 3	C₂₁H₂₀O₁₁	木犀草素-7-O-葡萄糖苷	[25]
10	[M-H]^-	469.021 2	C₂₉H₄₂O₅	11α,12α-epoxy-3β,23-dihydroxy-30-norolean-20(29)-en-28,13β-olide	[22]
11	[M-H]^-	447.064 6	C₂₁H₂₀O₁₁	山奈酚-3-O-β-D-吡喃葡萄糖苷	[27]
12	[M-H]^-	577.118 2	C₂₇H₃₀O₁₄	芹菜素-7-O-新橘皮糖苷或芹菜素-7-O-β-D-葡萄糖-4'-O-α-L-鼠李糖苷	[27-28]
13	[M-H]^-	431.070 1	C₂₁H₂₀O₁₀	芹菜素-7-O-β-D-吡喃葡糖苷	[27]
14	[M-H]^-	545.020 0	—	未知
15	[M-H]^-	349.03 26	—	未知