Development of a triple hyphenated HPLC-radical scavenging detection-DAD-SPE-NMR system for the rapid identification of antioxidants in complex plant extracts

A. Pukalskas, T.A. van Beek, P. de Waard

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86 Citations (Scopus)

Abstract

A rapid method for the simultaneous detection and identification of radical scavenging compounds in plant extracts was developed by combining an HPLC with on-line radical scavenging using DPPH as a model radical and an HPLC¿DAD¿SPE¿NMR system. Using this method a commercial rosemary extract was investigated. All major compounds present in the extract were collected on SPE cartridges after their separation. Advantages of on-line SPE peak trapping are the possibility to perform HPLC with non-deuterated solvents, a concentration effect and being able to record NMR spectra in pure 100% deuterated solvents. After comparing DAD and DPPH scavenging chromatograms, 1H NMR spectra of compounds having radical scavenging activities were recorded. Afterwards all compounds were collected and infused into an ESI-MS. The five main active compounds ¿ carnosol, carnosic acid carnosaldehyde, 12-methoxycarnosic acid and epiisorosmanol ¿ could be identified from the combined UV, NMR and mass spectral data without actually isolating them. It was possible to record on-line an HMBC spectrum of carnosic acid. Also one compound was tentatively identified as epirosmanol methyl ether
Original languageEnglish
Pages (from-to)81-88
JournalJournal of Chromatography. A, Including electrophoresis and other separation methods
Volume1074
Issue number1-2
DOIs
Publication statusPublished - 2005

Fingerprint

Scavenging
Plant Extracts
Complex Mixtures
Antioxidants
High Pressure Liquid Chromatography
Nuclear magnetic resonance
Methyl Ethers
Acids
salvin
Proton Magnetic Resonance Spectroscopy
carnosol

Keywords

  • rosmarinus-officinalis l
  • carnosic acid
  • phenolic diterpenes
  • salvia-officinalis
  • rosemary extracts
  • online detection
  • sage extracts
  • flow-probe
  • constituents
  • oil

Cite this

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title = "Development of a triple hyphenated HPLC-radical scavenging detection-DAD-SPE-NMR system for the rapid identification of antioxidants in complex plant extracts",
abstract = "A rapid method for the simultaneous detection and identification of radical scavenging compounds in plant extracts was developed by combining an HPLC with on-line radical scavenging using DPPH as a model radical and an HPLC¿DAD¿SPE¿NMR system. Using this method a commercial rosemary extract was investigated. All major compounds present in the extract were collected on SPE cartridges after their separation. Advantages of on-line SPE peak trapping are the possibility to perform HPLC with non-deuterated solvents, a concentration effect and being able to record NMR spectra in pure 100{\%} deuterated solvents. After comparing DAD and DPPH scavenging chromatograms, 1H NMR spectra of compounds having radical scavenging activities were recorded. Afterwards all compounds were collected and infused into an ESI-MS. The five main active compounds ¿ carnosol, carnosic acid carnosaldehyde, 12-methoxycarnosic acid and epiisorosmanol ¿ could be identified from the combined UV, NMR and mass spectral data without actually isolating them. It was possible to record on-line an HMBC spectrum of carnosic acid. Also one compound was tentatively identified as epirosmanol methyl ether",
keywords = "rosmarinus-officinalis l, carnosic acid, phenolic diterpenes, salvia-officinalis, rosemary extracts, online detection, sage extracts, flow-probe, constituents, oil",
author = "A. Pukalskas and {van Beek}, T.A. and {de Waard}, P.",
year = "2005",
doi = "10.1016/j.chroma.2005.03.089",
language = "English",
volume = "1074",
pages = "81--88",
journal = "Journal of Chromatography. A, Including electrophoresis and other separation methods",
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T1 - Development of a triple hyphenated HPLC-radical scavenging detection-DAD-SPE-NMR system for the rapid identification of antioxidants in complex plant extracts

AU - Pukalskas, A.

AU - van Beek, T.A.

AU - de Waard, P.

PY - 2005

Y1 - 2005

N2 - A rapid method for the simultaneous detection and identification of radical scavenging compounds in plant extracts was developed by combining an HPLC with on-line radical scavenging using DPPH as a model radical and an HPLC¿DAD¿SPE¿NMR system. Using this method a commercial rosemary extract was investigated. All major compounds present in the extract were collected on SPE cartridges after their separation. Advantages of on-line SPE peak trapping are the possibility to perform HPLC with non-deuterated solvents, a concentration effect and being able to record NMR spectra in pure 100% deuterated solvents. After comparing DAD and DPPH scavenging chromatograms, 1H NMR spectra of compounds having radical scavenging activities were recorded. Afterwards all compounds were collected and infused into an ESI-MS. The five main active compounds ¿ carnosol, carnosic acid carnosaldehyde, 12-methoxycarnosic acid and epiisorosmanol ¿ could be identified from the combined UV, NMR and mass spectral data without actually isolating them. It was possible to record on-line an HMBC spectrum of carnosic acid. Also one compound was tentatively identified as epirosmanol methyl ether

AB - A rapid method for the simultaneous detection and identification of radical scavenging compounds in plant extracts was developed by combining an HPLC with on-line radical scavenging using DPPH as a model radical and an HPLC¿DAD¿SPE¿NMR system. Using this method a commercial rosemary extract was investigated. All major compounds present in the extract were collected on SPE cartridges after their separation. Advantages of on-line SPE peak trapping are the possibility to perform HPLC with non-deuterated solvents, a concentration effect and being able to record NMR spectra in pure 100% deuterated solvents. After comparing DAD and DPPH scavenging chromatograms, 1H NMR spectra of compounds having radical scavenging activities were recorded. Afterwards all compounds were collected and infused into an ESI-MS. The five main active compounds ¿ carnosol, carnosic acid carnosaldehyde, 12-methoxycarnosic acid and epiisorosmanol ¿ could be identified from the combined UV, NMR and mass spectral data without actually isolating them. It was possible to record on-line an HMBC spectrum of carnosic acid. Also one compound was tentatively identified as epirosmanol methyl ether

KW - rosmarinus-officinalis l

KW - carnosic acid

KW - phenolic diterpenes

KW - salvia-officinalis

KW - rosemary extracts

KW - online detection

KW - sage extracts

KW - flow-probe

KW - constituents

KW - oil

U2 - 10.1016/j.chroma.2005.03.089

DO - 10.1016/j.chroma.2005.03.089

M3 - Article

VL - 1074

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EP - 88

JO - Journal of Chromatography. A, Including electrophoresis and other separation methods

JF - Journal of Chromatography. A, Including electrophoresis and other separation methods

SN - 0021-9673

IS - 1-2

ER -