Phytochemical Analysis

Cover image for Vol. 25 Issue 4

Special Issue: Pre-analytical Methods in Plant Metabolomics: Sample Preparation and Extraction

July/August 2014

Volume 25, Issue 4

Pages 289–388

Issue edited by:

  1. Editorial

    1. Top of page
    2. Editorial
    3. Special Issue Reviews
    4. Special Issue Articles
    1. You have free access to this content
      Metabolomics: What You See is What You Extract (pages 289–290)

      Young Hae Choi and Robert Verpoorte

      Version of Record online: 17 JUN 2014 | DOI: 10.1002/pca.2513

  2. Special Issue Reviews

    1. Top of page
    2. Editorial
    3. Special Issue Reviews
    4. Special Issue Articles
    1. Extraction for Metabolomics: Access to The Metabolome (pages 291–306)

      Mian Yahya Mushtaq, Young Hae Choi, Robert Verpoorte and Erica G. Wilson

      Version of Record online: 13 FEB 2014 | DOI: 10.1002/pca.2505

      Extraction is a very critical step in metabolomics studies. This article provides an overview of the most used methods and their applications, revealing how the choice of different techniques and solvents affects the type and amount of metabolites extracted. Diverse pre-extraction treatments and their effects on the metabolite profile are also discussed. Finally, we introduce a method developed by our group (comprehensive extraction method), which is especially suited to overcome the problem of extracting chemically diverse metabolites.

    2. Laser Microdissection: a Sample Preparation Technique for Plant Micrometabolic Profiling (pages 307–313)

      Jingjing Fang and Bernd Schneider

      Version of Record online: 23 SEP 2013 | DOI: 10.1002/pca.2477

      This review provides an introduction to laser microdissection, a powerful sampling technique to harvest plant material for micrometabolic profiling. It is described step-by-step, how LMD can be used to sample homogeneous cell types or microscopic tissue pieces from different plant organs, such as leaves, stems, and seeds. This review also summarizes studies, indicating the wide application of LMD for high-resolution plant metabolite analysis. Finally, the future of LMD in plant metabolites analysis is discussed.

    3. Sample Preparation for Liquid Chromatographic Analysis of Phytochemicals in Biological Fluids (pages 314–330)

      Ju-Hee Oh and Young-Joo Lee

      Version of Record online: 2 DEC 2013 | DOI: 10.1002/pca.2484

      This review discusses sample preparation methods for quantification of phytochemicals in biological matrices such as plasma, bile, urine, faeces and tissues that are applicable to pharmacokinetics studies of herbal medicines and natural products. Protein precipitation, liquid–liquid extraction and solid-phase extraction are used primarily in the context of wide applications as well as to increase processing efficiency. Sample preparation methods critically condition the quality of data in spite of extraordinary developments in analytical equipment such as the MS detector.

    4. An Overview of Plant Volatile Metabolomics, Sample Treatment and Reporting Considerations with Emphasis on Mechanical Damage and Biological Control of Weeds (pages 331–341)

      John J. Beck, Lincoln Smith and Nausheena Baig

      Version of Record online: 18 DEC 2013 | DOI: 10.1002/pca.2486

      Plant emitted volatiles are an important component for understanding plant-plant, plant-insect, or plant-microbe interactions. In situ collection methods and gas chromatography coupled to mass spectroscopy have allowed for the efficient detection of plant volatile metabolites, which provide important clues as to the biochemical processes of a plant. The emerging field of plant volatile metabolomics was reviewed and the example of its potential use toward biological control of weeds discussed.

  3. Special Issue Articles

    1. Top of page
    2. Editorial
    3. Special Issue Reviews
    4. Special Issue Articles
    1. An Easy, Convenient Cell and Tissue Extraction Protocol for Nuclear Magnetic Resonance Metabolomics (pages 342–349)

      Nicolas Matheus, Sylvain Hansen, Eric Rozet, Paul Peixoto, Erik Maquoi, Vincent Lambert, Agnès Noël, Michel Frédérich, Denis Mottet and Pascal de Tullio

      Version of Record online: 23 JAN 2014 | DOI: 10.1002/pca.2498

      The visualisation of the metabolites contained in cells, tissues or organs could be a powerful tool to understand local metabolism. For this purpose, extraction is a necessary step to obtain samples adapted for the appropriate analytical tools. These work-ups are often the most labour-intensive and rate-limiting steps in metabolomics. In the search for a simplified, fast and NMR-compatible protocol, we assessed the use of sonication to disrupt cell membranes and tissue structures.

    2. Sample Preparation Issues in NMR-based Plant Metabolomics: Optimisation for Vitis Wood Samples (pages 350–356)

      Maria Halabalaki, Samuel Bertrand, Anna Stefanou, Katia Gindro, Sarantos Kostidis, Emmanuel Mikros, Leandros A. Skaltsounis and Jean-Luc Wolfender

      Version of Record online: 4 FEB 2014 | DOI: 10.1002/pca.2497

      The aim of the study was the investigation of different sample preparation methods and establishment of an optimised protocol for untargeted NMR-based metabolomics of Vitis vinifera wood. Two reference cultivars were selected and different extraction protocols and deuterated solvents systems for NMR acquisition were evaluated. The optimal extract concentration, chemical shift stability and peak area repeatability were also investigated. Attention should be paid to sample preparation procedures prior NMR analysis to perform an extensive metabolomic survey of the specific matrix.

    3. Ultrasound-assisted Extraction with LC–TOF/MS Identification and LC–UV Determination of Imazamox and its Metabolites in Leaves of Wheat Plants (pages 357–363)

      Antonia M. Rojano-Delgado, Feliciano Priego-Capote, Rafael De Prado and María Dolores Luque de Castro

      Version of Record online: 10 AUG 2013 | DOI: 10.1002/pca.2467

      A method based on ultrasound-assisted sample preparation and liquid chromatography-ultraviolet absorption detection for simultaneous determination of imazamox and its metabolites in plants is proposed. Identification and confirmatory analysis of the presence of imazamox and its metabolites in extracts from treated plants was performed by LC-TOF/MS. The metabolites were quantified using a surrogate approach based on imazamox standard as there are not commercial standards for them. The method make is recommendable to evaluate metabolism of Imazamox in plants.

    4. Efficiency of Different Solvents on the Extraction of Bioactive Compounds from the Amazonian Fruit Caryocar villosum and the Effect on its Antioxidant and Colour Properties (pages 364–372)

      Renan Campos Chisté, Marta de Toledo Benassi and Adriana Zerlotti Mercadante

      Version of Record online: 26 NOV 2013 | DOI: 10.1002/pca.2489

      Caryocar villosum extracts were obtained by extraction using safe solvents with different polarities. The goal of this research was to obtain extracts with high levels of bioactive compounds, with both antioxidant and colour properties. As a conclusion, ethanol:water, water and ethanol are the most promising solvents to obtain Caryocar villosum extracts with high contents of bioactive compounds, peroxyl radical scavenging capacity and protection against singlet oxygen. These extracts may be potentially used against oxidative damage in foods or biological systems.

    5. Extraction-free In situ Derivatisation of Timosaponin AIII Using Direct Analysis in Real Time TOF/MS (pages 373–377)

      Hye Jin Kim, Se Ri Park and Young Pyo Jang

      Version of Record online: 5 DEC 2013 | DOI: 10.1002/pca.2488

      In situ permethylation with tetramethylammonium hydroxide was successfully employed in DART-TOF-MS analysis of hydrophilic glycoside directly from plant tissue. Timosaponin III was anlayzed from Anemarrhena Rhizoma raw material with LOD range of a few nanogram scale which was not detected by normal DART-MS analysis. Broader spectrum of natural products can be analyzed with DART-MS directly from the tissues by this in situ derivatization.

    6. Species-specific Standardisation of Licorice by Metabolomic Profiling of Flavanones and Chalcones (pages 378–388)

      Charlotte Simmler, Tristesse Jones, Jeffrey R. Anderson, Dejan C. Nikolić, Richard B. van Breemen, Djaja D. Soejarto, Shao-Nong Chen and Guido F. Pauli

      Version of Record online: 13 NOV 2013 | DOI: 10.1002/pca.2472

      UHPLC-based quantitative metabolomic profiling of two widely used licorice species, Glycyrrhiza glabra and Glycyrrhiza uralensis, identified characteristic flavanone (F) and chalcone (C) glycoside patterns and F:C proportions as suitable measures for botanical quality control and species-specific standardisation. The F–C compositions reflect the metabolic flux of liquiritigenin to isoliquiritigenin glycosides in each species. The conclusions were validated by analysing a panel of three different hydro-alcoholic extracts obtained from each of the three accessions per species.

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