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Volume 28 Number 6
November – December 2017
Aims & Scope
Phytochemical Analysis is devoted to the publication of original articles concerning the development, improvement, validation
and/or extension of application of analytical methodology in the plant sciences. The spectrum of coverage is broad, encompassing
methods and techniques relevant to the detection (including bio-screening), extraction, separation, purification, identification and
quantification of compounds in plant biochemistry, plant cellular and molecular biology, plant biotechnology, the food sciences,
agriculture and horticulture. The Journal publishes papers describing significant novelty in the analysis of whole plants (including
algae), plant cells, tissues and organs, plant-derived extracts and plant products (including those which have been partially or
completely refined for use in the food, agrochemical, pharmaceutical and related industries). All forms of physical, chemical,
biochemical, spectroscopic, radiometric, electrometric, chromatographic, metabolomic and chemometric investigations of
plant products (monomeric species as well as polymeric molecules such as nucleic acids, proteins, lipids and carbohydrates) are
included within the remit of the Journal. Papers dealing with novel methods relating to areas such as data handling /data mining
in plant sciences will also be welcomed.
Phytochemical Analysis is intended to serve as a major resource for information on analytical and instrumental methodology in
the plant sciences. Together with original articles and accelerated communications, all of which will be both timely and of interest
to a wide readership, short review articles describing recent advances in specific areas of plant analysis will be published. Reviews
are by invitation only, but the Editor-in-Chief welcomes suggestions for new review topics from potential authors.
Research articles
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.
Mass Spectrometry Imaging
of Low Molecular Weight
Compounds In Garlic (Allium
sativum L.) with Gold
Nanoparticle Enhanced Target
M. Misiorek, J. Sekuła and T. Ruman
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.
Phlorotannin Composition of
Laminaria digitata
HSCCC combined with an on-line storage recycling (OSR) elution technique
was employed. Reverse elution mode was used for decreasing the isolation
cost ultimately. Six natural stilbene-dihydroflavonoids were non-stop
isolated from a Sophora herb by running OSR-HSCCC.
High‐Speed Counter‐Current
Chromatography with an
Online Storage Technique for
the Preparative Isolation and
Purification of Dihydroflavonoids
from Sophora alopecuroides L.
A. M. Vissers, A. Caligiani, S. Sforza,
J.‐P. Vincken and H. Gruppen
Z.‐L. Sun, J.‐M. He, J.‐E. Lan and Q. Mu
Contents continued
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.
One‐Step Extraction and Hydrolysis
of Flavonoid Glycosides in Rape
Bee Pollen Based on Soxhlet‐
Assisted Matrix Solid Phase
X. Tu, S. Ma, Z. Gao, J. Wang, S. Huang
and W. Chen
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.
Structural Characterisation
of Acetogenins from Annona
muricata by Supercritical Fluid
Chromatography Coupled to
High‐Resolution Tandem Mass
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.
Flavonoid Composition Of Tarocco
(Citrus sinensis L. Osbeck) Clone
“Lempso” and Fast Antioxidant
Activity Screening by DPPH‐
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 semirigid 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.
Integrating High‐Resolution
and Solid‐State Magic Angle
Spinning NMR Spectroscopy
and a Transcriptomic Analysis of
Soybean Tissues in Response to
Water Deficiency
This article is the first report of screening 40 Salvia species according to their
psychoactive constituents, salvinorin A and salvinorin B and their genomic
structures. Very few of the Salvia species (S. recognita, S. cryptantha and
S. glutinosa) contained relatively high levels of salvinorin A. The sequences
of 5S -rRNA gene of 40 different Salvia species were presented and it was
found that none of the Salvia species had similar DNA sequence to Salvia
divinorum plant.
Screening of Hallucinogenic
Compounds and Genomic
Characterisation of 40 Anatolian
Salvia Species
L. Laboureur, N. Bonneau, P. Champy,
A. Brunelle and D. Touboul
E. Sommella, F. Pagano, G. Pepe,
C. Ostacolo, M. Manfra, M. Chieppa,
R. Di Sanzo, S. Carabetta, P. Campiglia
and M. Russo
I. D. Coutinho, T. B. Moraes, L. M. Mertz‐Henning,
A. L. Nepomuceno, W. Giordani,
J. Marcolino‐Gomes, S. Santagneli
and L. A. Colnago
S. D. Hatipoglu, B. Yalcinkaya, M. Akgoz,
T. Ozturk, A. C. Goren and G. Topcu
Contents continued
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.
Liquid Chromatographic
Method for the Determination of
Caffeoylquinic Acid Derivates in
Hieracium pilosella L
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.
Supercritical CO2 Extraction
of Lavandula angustifolia
Mill. Flowers: Optimisation of
Oxygenated Monoterpenes,
Coumarin and Herniarin Content
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).
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
L. Borisova‐Jan, D. Fransson, P. Claeson
and R. Burman
I. Jerković, M. Molnar, S. Vidović, J. Vladić
and S. Jokić
J. Haller, S. Schwaiger, H. Stuppner,
F. Gafner and M. Ganzera
Highlights for review
• Brackens (Pteridium sp.) is classified by WHO/IARC as “… possibly
carcinogenic to humans”.
• Bracken and ptaquiloside cause cancer in the urinary bladder among cattle.
• Other ferns cause similar cancers and contain ptaquiloside.
• A novel HPLC-DAD method for screening of ptaquiloside and metabolite
pterosin B was validated.
• A novel experimental approach using herbarium specimens for screening
purposes was tested.
• Ptaquiloside and pterosin B were only found in Bracken among the screened species.
• Herbarium specimens up to 50 years old can be used for qualitative screening surveys.
Screening for Ptaquiloside in Ferns:
Using Herbarium Specimens for
Qualitative Mapping Purposes
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.
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
L. H. Rasmussen and H. Æ. Pedersen
V. Vujčić, S. Radić Brkanac, I. Radojčić
Redovniković, S. Ivanković, R. Stojković,
I. Žilić and M. Radić Stojković
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