LC-MS/MS profiling of polyphenol-enriched leaf, stem and root extracts of Korean Humulus japonicus Siebold & Zucc and determination of their antioxidant effects

Biomed Chromatogr. 2018 May;32(5):e4171. doi: 10.1002/bmc.4171. Epub 2018 Jan 10.

Abstract

Polyphenols from ethyl acetate extracts from the leaves, stems and roots of Korean Humulus japonicus were comprehensively profiled using liquid chromatography-electrospray ionization-tandem mass spectrometry. A total of 36 polyphenols were detected, of which 26 were structurally characterized based on their [M - H]- peak, tandem mass spectrometry fragmentation pattern, UV-vis absorption and published data. Validation data provided satisfactory results for the evaluated parameters. The determination coefficients were ≥0.9812. The limits of detection and quantification were 0.017-0.573 and 0.056-1.834 mg/L, respectively, indicating good performance limits. The accuracy (expressed as percentage recovery) at 50 and 100 mg/L was 71.4-99.7 and 75.1-105.1%, with precisions (expressed as relative standard deviation) of 1.5-7.3 and 0.8-4.1%, respectively, indicating acceptable accuracy and precision values. The leaves were rich in total polyphenols (3089.9 ± 6.4 mg/kg of fresh sample) followed by the stems (1313.9 ± 6.4 mg/kg of fresh sample) and roots (655.2 ± 2.7 mg/kg of fresh sample). Antioxidant activity, determined by α,α-diphenyl-β-picrylhydrazyl, 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) scavenging activity and ferric reducing antioxidant power assay, revealed the lowest EC50 value for the leaf extracts, indicating a higher scavenging activity in this tissue followed by the roots and stems. Overall, the results indicated that H. japonicus is rich in polyphenols and could be a potential alternative to Humulus lupulus (hop plant) in the brewery industry.

Keywords: Humulus japonicus; antioxidant activity; high-performance liquid chromatography; polyphenols; tandem mass spectrometry.

MeSH terms

  • Antioxidants / analysis*
  • Antioxidants / chemistry
  • Antioxidants / metabolism
  • Benzothiazoles / analysis
  • Benzothiazoles / metabolism
  • Biphenyl Compounds / analysis
  • Biphenyl Compounds / metabolism
  • Chromatography, High Pressure Liquid / methods*
  • Humulus / chemistry*
  • Limit of Detection
  • Linear Models
  • Picrates / analysis
  • Picrates / metabolism
  • Plant Extracts / chemistry*
  • Polyphenols / analysis*
  • Polyphenols / chemistry
  • Polyphenols / metabolism
  • Reproducibility of Results
  • Sulfonic Acids / analysis
  • Sulfonic Acids / metabolism
  • Tandem Mass Spectrometry / methods*

Substances

  • Antioxidants
  • Benzothiazoles
  • Biphenyl Compounds
  • Picrates
  • Plant Extracts
  • Polyphenols
  • Sulfonic Acids
  • 2,2'-azino-di-(3-ethylbenzothiazoline)-6-sulfonic acid
  • 1,1-diphenyl-2-picrylhydrazyl