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[用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱分析桑寄生乙酸乙酯提取物的化学成分并筛选潜在的黄嘌呤氧化酶抑制剂]

[Analysis of chemical constituents in ethyl acetate extract of Taxilli Herba by UPLC-Q-Exactive-MS and screening of potential xanthine oxidase inhibitors].

作者信息

Liang Yuan, Li Li, Cai Yi, Xu Li-Ba, Xie Feng-Feng, Liang Da-Long, Chen Fu-Lai

机构信息

Guangxi University of Chinese Medicine Nanning 530200, China.

Guangxi University of Chinese Medicine Nanning 530200, China Chengdu University of Traditional Chinese Medicine Chengdu 611137, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2022 Feb;47(4):972-979. doi: 10.19540/j.cnki.cjcmm.20210914.201.

Abstract

The present study analyzed and identified the chemical constituents from ethyl acetate(EA) extract of Taxilli Herba with UPLC-Q-Exactive-MS and screened active xanthine oxidase(XO) inhibitors with HPLC. The analysis was performed on an Hypersil GOLD C_(18) reversed-phase column(2.1 mm×50 mm, 1.9 μm), with the mobile phase of water containing 1% formic acid(A) and methanol(B) under gradient elution, the flow rate of 0.3 mL·min(-1), and the injection volume of 5 μL. ESI source was used for MS and the compounds were collected in positive and negative ion modes. Xcalibur 4.1 was used to analyze the retention time, accurate relative molecular weight, and fragmentation of the compounds. The inhibitory activity of some known compounds on XO was screened by HPLC. Thirty chemical constituents were identified, including phenolic acids and flavonoids by experimental data combined with information of standards, data reported previously, and databases, such as MzCloud and ChemSpider. The activities of 10 chemical components were screened. Gallic acid and naringenin chalcone had strong inhibitory activities on XO with IC_(50) of 57 μg·mL(-1) and 108 μg·mL~(-1). UPLC-Q-Exactive-MS allows the accurate, rapid, and comprehensive identification of main chemical constituents from Taxilli Herba. Gallic acid and naringenin chalcone may be the active components of XO inhibitors.

摘要

本研究采用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UPLC-Q-Exactive-MS)对桑寄生乙酸乙酯提取物中的化学成分进行分析和鉴定,并采用高效液相色谱法筛选活性黄嘌呤氧化酶(XO)抑制剂。分析在Hypersil GOLD C₁₈反相色谱柱(2.1 mm×50 mm,1.9 μm)上进行,流动相为含1%甲酸的水(A)和甲醇(B),梯度洗脱,流速为0.3 mL·min⁻¹,进样量为5 μL。采用电喷雾离子源(ESI)进行质谱分析,化合物在正离子和负离子模式下采集。使用Xcalibur 4.1分析化合物的保留时间、精确相对分子量和碎片。通过高效液相色谱法筛选了一些已知化合物对XO的抑制活性。结合标准品信息、先前报道的数据以及MzCloud和ChemSpider等数据库,通过实验数据鉴定出30种化学成分,包括酚酸类和黄酮类化合物。筛选了10种化学成分的活性。没食子酸和柚皮素查尔酮对XO具有较强的抑制活性,IC₅₀分别为57 μg·mL⁻¹和108 μg·mL⁻¹。UPLC-Q-Exactive-MS能够准确、快速、全面地鉴定桑寄生中的主要化学成分。没食子酸和柚皮素查尔酮可能是XO抑制剂的活性成分。

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