Phytochemical Analysis

Cover image for Vol. 28 Issue 5

Early View (Online Version of Record published before inclusion in an issue)

Editor-in-Chief: Satyajit D. Sarker

Impact Factor: 2.292

ISI Journal Citation Reports © Ranking: 2016: 36/76 (Chemistry Analytical); 45/77 (BIOCHEMICAL RESEARCH METHODS); 60/211 (Plant Sciences)

Online ISSN: 1099-1565


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  1. Research Articles

    1. Quantitative Analysis of Ingenol in Euphorbia species via Validated Isotope Dilution Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry

      Tibor Béres, Klaus Dragull, Jiří Pospíšil, Danuše Tarkowská, Martin Dančák, Ondřej Bíba, Petr Tarkowski, Karel Doležal and Miroslav Strnad

      Version of Record online: 7 AUG 2017 | DOI: 10.1002/pca.2711

      Thumbnail image of graphical abstract

      Ingenol is the key precursor for the synthesis of ingenol mebutate (angelate), used to treat actinic keratosis.

      Various species of the Euphorbia genus contain diterpene ingenol and ingenol mebutate (ingenol-3-angelate), a substance found in the sap of the plant Euphorbia peplus and an inducer of cell death. An ultra-high performance liquid chromatography tandem mass spectrometry-based screening method suitable for quantitative analysis of ingenol in 38 species of the Euphorbia genus was developed. The 18O–labelled ingenol analogue was used as an internal standard for ingenol content determination and method validation.

    2. Identification of some Bioactive Metabolites in a Fractionated Methanol Extract from Ipomoea aquatica (Aerial Parts) through TLC, HPLC, UPLC-ESI-QTOF-MS and LC-SPE-NMR Fingerprints Analyses

      Mahmoud Hefny Gad, Emmy Tuenter, Nagwa El-Sawi, Sabry Younes, El-Mewafy El-Ghadban, Kristiaan Demeyer, Luc Pieters, Yvan Vander Heyden and Debby Mangelings

      Version of Record online: 4 AUG 2017 | DOI: 10.1002/pca.2709

      • - Comparison of information from HPLC and HPTLC fingerprints of different Ipomoea aquatica fractions.
      • - Tentative identification of eight compounds in ethyl acetate-methanol fraction using UPLC-QTOF-MS.
      • - Confirmation the chemical structure of rutin and nicotiflorin using LC-SPE-NMR.
    3. Methanol Extracts of 28 Hieracium Species from the Balkan Peninsula – Comparative LC–MS Analysis, Chemosystematic Evaluation of their Flavonoid and Phenolic Acid Profiles and Antioxidant Potentials

      Violeta Milutinović, Marjan Niketić, Ljuboš Ušjak, Dejan Nikolić, Aleksej Krunić, Christian Zidorn and Silvana Petrović

      Version of Record online: 2 AUG 2017 | DOI: 10.1002/pca.2712

      Qualitative and quantitative analysis of flavonoids and phenolic acids in methanol extracts of aerial flowering parts of 28 Hieracium species from the Balkans was performed by LC-MS. Multivariate statistical data analysis included nMDS, UPGMA and PCA. Chemical analysis demonstrated that these metabolites are good indicators of chemosystematic relationships within Hieracium, particularly between non-hybrid species and groups from the same location. The antioxidant potential of the extracts, evaluated using three colorimetric tests, was satisfactory and in accordance with their phenolics composition.

    4. Phytochemical and Bioactive Potential of in vivo and in vitro Grown Plants of Centaurea ragusina L. – Detection of DNA/RNA Active Compounds in Plant Extracts via Thermal Denaturation and Circular Dichroism

      Valerija Vujčić, Sandra Radić Brkanac, Ivana Radojčić Redovniković, Siniša Ivanković, Ranko Stojković, Irena Žilić and Marijana Radić Stojković

      Version of Record online: 25 JUL 2017 | DOI: 10.1002/pca.2708

      Conditions for the most efficient polyphenol extraction from C. Ragusina L. were determined: the 80% EtOH/water solvent system for callus and leaf ex vitro samples and 80 or 96% EtOH for leaf in vivo samples. Significantly higher levels of chlorogenic acid and naringenin were detected in callus tissue than in wild plant. Ethanolic extracts exhibited the significant antibacterial activity against Staphylococcus aureus ATCC 25923. DNA/RNA active compounds in plant extracts were detected by thermal denaturation and circular dichroism methods.

    5. Application of NIR Spectroscopy Coupled with PLS Regression for Quantification of Total Polyphenol Contents from the Fruit and Aerial Parts of Citrullus colocynthis

      Tania S. Rizvi, Fazal Mabood, Liaqat Ali, Mohammed Al-Broumi, Hamida K.M. Al Rabani, Javid Hussain, Farah Jabeen, Suryyia Manzoor and Ahmed Al-Harrasi

      Version of Record online: 25 JUL 2017 | DOI: 10.1002/pca.2710

      Citrulluscolocynthis is extensively used to treat various human ailments due to the presence of phytochemical constituents responsible for interesting biological activities. In an attempt to quantify the polyphenolic phytochemicals of fruit and aerial parts of the title plant, NIR spectroscopy was used successfully in connection with the multivariate analysis.

    6. Integrating High-Resolution and Solid-State Magic Angle Spinning NMR Spectroscopy and a Transcriptomic Analysis of Soybean Tissues in Response to Water Deficiency

      Isabel D. Coutinho, Tiago Bueno Moraes, Liliane Marcia Mertz-Henning, Alexandre Lima Nepomuceno, Willian Giordani, Juliana Marcolino-Gomes, Silvia Santagneli and Luiz Alberto Colnago

      Version of Record online: 19 JUL 2017 | DOI: 10.1002/pca.2702

      This study revealed the potential of integrating NMR-MAS and transcriptomic data. The primary metabolites were up-regulated by water deficiency and were properly assigned in the 1H HR-MAS spectrum, rigid and semi-rigid polysaccharides were readily observed using CP-MAS and mobile components were observed by SPE-MAS during the SSNMR analysis. In addition, multiple copies of the genes involved in the biosynthesis of the compounds affected by the water deficiency were identified in the soybean genome.

    7. Screening of Hallucinogenic Compounds and Genomic Characterisation of 40 Anatolian Salvia Species

      Seda Damla Hatipoglu, Burhanettin Yalcinkaya, Muslum Akgoz, Turan Ozturk, Ahmet C. Goren and Gulacti Topcu

      Version of Record online: 19 JUL 2017 | DOI: 10.1002/pca.2703

    8. Supercritical CO2 Extraction of Lavandula angustifolia Mill. Flowers: Optimisation of Oxygenated Monoterpenes, Coumarin and Herniarin Content

      Igor Jerković, Maja Molnar, Senka Vidović, Jelena Vladić and Stela Jokić

      Version of Record online: 14 JUL 2017 | DOI: 10.1002/pca.2705

      SC-CO2 extraction of lavender flowers was performed under different parameters determined by Box-Behnken design. The interaction between the pressure and CO2 flow rate as well as between the temperature and CO2 flow rate showed statistically significant influence on the yield. The optimum extraction conditions for higher monoterpenes and lower coumarin content were at 10 MPa, 41°C and CO2 flow rate 2.3 kg/h, and at 30 MPa, 50°C and CO2 flow rate 3 kg/h for higher monoterpenes and coumarin content.

    9. Screening for Ptaquiloside in Ferns: Using Herbarium Specimens for Qualitative Mapping Purposes

      Lars Holm Rasmussen and Henrik Ærenlund Pedersen

      Version of Record online: 13 JUL 2017 | DOI: 10.1002/pca.2707

      Thumbnail image of graphical abstract
    10. Isolation of Three Triterpene Saponins, Including Two New Oleanane Derivatives, from Soldanella alpina and Hydrophilic Interaction Liquid Chromatography–Evaporative Light Scattering Detection of these Three Saponins in Four Soldenella Species

      Julia Haller, Stefan Schwaiger, Hermann Stuppner, Frank Gafner and Markus Ganzera

      Version of Record online: 12 JUL 2017 | DOI: 10.1002/pca.2706

      The phytochemical investigation of different Soldanella species resulted in the isolation of three oleanane-type saponins, two being new natural products, and the development of an HPLC method for their separation. For the latter Hydrophilic Interaction Liquid Chromatography and Evaporative Light Scattering Detection were used. Method validation confirmed that the assay meets all respective requirements, and quantitative results revealed a total saponin content ranging from 1.09 % (S. montana leaves) to 5.14 % (S. alpina roots).

    11. Flavonoid Composition of Tarocco (Citrus sinensis L. Osbeck) Clone Lempso and Fast Antioxidant Activity Screening by DPPH-UHPLC-PDA-IT-TOF

      Eduardo Sommella, Francesco Pagano, Giacomo Pepe, Carmine Ostacolo, Michele Manfra, Marcello Chieppa, Rosa Di Sanzo, Sonia Carabetta, Pietro Campiglia and Mariateresa Russo

      Version of Record online: 7 JUL 2017 | DOI: 10.1002/pca.2701

      The flavonoid pattern of a typical Citrus sinensis variety, an original product of the Calabria region, namely Tarocco Lempso, has been investigated thoroughly. The qualitative/quantitative profiling was performed using a UHPLC-PDA-IT-TOF platform. Moreover, a precolumn DPPH assay coupled to UHPLC-PDA was developed as a fast antioxidant screening method. The entire protocol takes only 50 min per sample, comprising of reaction and analysis. The developed method highlighted higher amount of flavanones and a better antioxidant activity of Lempso clone, in comparison with other Citrus varieties.

    12. Liquid Chromatographic Method for the Determination of Caffeoylquinic Acid Derivates in Hieracium pilosella L

      Larisa Borisova-Jan, Dick Fransson, Per Claeson and Robert Burman

      Version of Record online: 2 JUL 2017 | DOI: 10.1002/pca.2704

      An HPLC method for quantification of caffeoylquinic acid derivatives in Hieracium pilosella has been developed and validated. Samples of H. pilosella were prepared by extraction of dried plant material with methanol. Individual substances in the methanol extract were identified by analyses of UV-MS/MS spectra and verified by comparisons with authentic reference substances. The content of caffeoylquinic acid derivatives was determined and expressed as chlorogenic acid. In analyses of 12 batches of H. pilosella contents of caffeoylquinic acid derivatives ranging from 0.7 to 1.9% were found.

    13. Structural Characterisation of Acetogenins from Annona muricata by Supercritical Fluid Chromatography Coupled to High-Resolution Tandem Mass Spectrometry

      Laurent Laboureur, Natacha Bonneau, Pierre Champy, Alain Brunelle and David Touboul

      Version of Record online: 19 JUN 2017 | DOI: 10.1002/pca.2700

      A new method for the structural elucidation of Annonaceous acetogenins was based on supercritical fluid chromatography coupled to high resolution tandem mass spectrometry, including lithium post-column cationisation. This method appeared as sensitive as classical liquid chromatography coupled to the same mass spectrometer but significantly improved the chromatographic resolution and thus allowed the annotation of a new group of isomers of montanacin-D.

    14. Mass Spectrometry Imaging of low Molecular Weight Compounds in Garlic (Allium sativum L.) with Gold Nanoparticle Enhanced Target

      Maria Misiorek, Justyna Sekuła and Tomasz Ruman

      Version of Record online: 13 JUN 2017 | DOI: 10.1002/pca.2696

      The distribution of organosulphur, organoselenium compounds as well as several low molecular weight compounds such as amino acids, peptides and fatty acids within sprouted garlic clove cross-section was studied using a mass spectrometry imaging (MSI) method with gold nanoparticle enhanced target (AuNPET). Ions of endogenous compounds of interest were characterised in order to assess their distribution in garlic tissue and biological function of their precursors and metabolic properties were also discussed.

    15. Phlorotannin Composition of Laminaria digitata

      Anne M. Vissers, Augusta Caligiani, Stefano Sforza, Jean-Paul Vincken and Harry Gruppen

      Version of Record online: 13 JUN 2017 | DOI: 10.1002/pca.2697

      Phlorotannins in Laminaria digitata were characterised. 13C NMR spectroscopy revealed a fucol-to-phlorethol linkage type ratio of 1:26. Quantitative 1H NMR spectroscopy allowed determination of the response factors required for colorimetric quantification by the DMBA-assay. Mass fragmentation data and 13C NMR spectroscopy (an average number of 1.5 hydrogen atoms per benzene ring) data indicated the presence of branched phlorotannin isomers. MALDI-TOF-MS analysis showed the presence of oligomeric phlorotannins up to DP27.

    16. One-Step Extraction and Hydrolysis of Flavonoid Glycosides in Rape Bee Pollen Based on Soxhlet-Assisted Matrix Solid Phase Dispersion

      Xijuan Tu, Shuangqin Ma, Zhaosheng Gao, Jing Wang, Shaokang Huang and Wenbin Chen

      Version of Record online: 9 JUN 2017 | DOI: 10.1002/pca.2699

      Thumbnail image of graphical abstract

      A modified matrix solid phase dispersion (MSPD) methodology was developed for analysing flavonoid aglycones in rape bee pollen. The method comprises a MSPD procedure using silica gel as sample disruptor, followed by packing into the column of constant pressure funnel. By refluxing with acid aqueous ethanol solution, the extraction and hydrolysis were accomplished in one step. Compared with already available methods, the present work showed advantages of time and labor saving, higher extraction efficiency and less consumption of acid catalyst.

    17. High-Speed Counter-Current Chromatography with an Online Storage Technique for the Preparative Isolation and Purification of Dihydroflavonoids from Sophora alopecuroides L.

      Zhong-Lin Sun, Jian-Ming He, Jiang-Er Lan and Qing Mu

      Version of Record online: 6 JUN 2017 | DOI: 10.1002/pca.2698

      1. HSCCC combined with an on-line storage recycling (OSR) elution technique was employed.
      2. Reverse elution mode was used for decreasing the isolation cost ultimately.
      3. Six natural stilbene-dihydroflavonoids were non-stop isolated from a Sophora herb by running OSR-HSCCC.


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