Phytochemical Analysis

Cover image for Vol. 25 Issue 3

May/June 2014

Volume 25, Issue 3

Pages 185–288

  1. Research Articles

    1. Top of page
    2. Research Articles
    1. Determination of Salicinoids by Micro-high-performance Liquid Chromatography and Photodiode Array Detection (pages 185–191)

      K. F. Rubert-Nason, C. J. Hedman, L. M. Holeski and R. L. Lindroth

      Version of Record online: 26 NOV 2013 | DOI: 10.1002/pca.2485

      We demonstrated the use of micro-high-performance liquid chromatography (μHPLC) with photodiode array detection (DAD) for quantification of four salicinoids (salicin, salicortin, hydroxycyclohexen-on-oyl salicortin and tremulacin) in methanolic extracts of Populus. Micro-HPLC can serve as a solvent-conserving alternative to conventional-scale HPLC for quantification of salicinoids.

    2. Stereochemistry of C18 Monounsaturated Cork Suberin Acids Determined by Spectroscopic Techniques Including 1H-NMR Multiplet Analysis of Olefinic Protons (pages 192–200)

      Sara Santos and José Graça

      Version of Record online: 5 DEC 2013 | DOI: 10.1002/pca.2491

      The two C18:1 cork suberin ω-hydroxyacid and α,ω-diacid were proved to have a cis configuration: (Z)-18-hydroxyoctadec-9-enoic acid and (Z)-octadec-9-enedoic acid. Their double bond stereochemistry was elucidated by spectroscopic techniques, namely 1H-NMR and 13C-NMR. The chemical shifts of the olefinic and allylic protons and of the allylic carbons were diagnostic, and the 1H-NMR multiplets of the olefinic protons could only be simulated using 3JHH and long-range 4JHH coupling constants typical of the cis configuration. The revealed stereochemistry of this two major suberin monomers brings a new insight into the mostly unknown suberin macromolecular structure.

    3. Determination of C-glucosidic Ellagitannins in Lythri salicariaeherba by Ultra-High Performance Liquid Chromatography Coupled with Charged Aerosol Detector: Method Development and Validation (pages 201–206)

      Sebastian Granica, Jakub P. Piwowarski and Anna K. Kiss

      Version of Record online: 29 DEC 2013 | DOI: 10.1002/pca.2492

      Lythri herba is a pharmacopoeial plant material. The aim of this study was to develop and validate an efficient UHPLC-CAD method for quantification of four major ellagitannins in Lythri herba and in one commercial preparation.

      Four major ellagitannins were quantified in samples of Lythri herba and in one commercial preparation. The sum of ellagitannins was determined and varied from 30.66 to 48.80 mg/g of raw material and 16.57 mg/capsule for investigated preparation.

    4. Structural Characterisation of Malonyl Flavonols in Leek (Allium porrum L.) Using High-performance Liquid Chromatography and Mass Spectrometry (pages 207–212)

      Leonardo Di Donna, Fabio Mazzotti, Domenico Taverna, Anna Napoli and Giovanni Sindona

      Version of Record online: 28 DEC 2013 | DOI: 10.1002/pca.2493

      The structures of five compounds never reported in leek have been determined by semi-preparative HPLC and high-resolution mass spectrometry. The molecules are mono-hexose, di-hexose and coumaroyl, feruloyl and caffeoyl acylated di-hexose derivatives of kaempferol. The common characteristic of the structures relies on the presence of the malonyl moiety on the primary alcoholic function of the sugar immediately linked to the aglycone. Accurate tandem mass spectrometry experiments and basic hydrolysis treatments reveal the sequence of the acylated glycosidic moieties.

    5. HPLC/UV Analysis of Polyacetylenes, Phenylpropanoid and Pyrrolidine Alkaloids in Medicinally Used Codonopsis Species (pages 213–219)

      Jing-Yu He, Shu Zhu and Katsuko Komatsu

      Version of Record online: 23 JAN 2014 | DOI: 10.1002/pca.2494

      Codonopsis Radix is commonly used as a tonic in traditional Chinese medicine. A HPLC/UV method for simultaneous quantitation of polyacetylenes (lobetyol, lobetyolin, lobetyolinin, cordifolioidyne B), phenylpropanoid (tangshenoside I) and pyrrolidine alkaloids (codonopyrrolidiums A, B) in Codonopsis Radix was established and validated, in which ultrasound-assisted methanol extracts of samples were analysed using reversed phase, gradient elution HPLC monitored at 215 nm. The method enables quality assessment of Codonopsis Radix based on multiple components having potential bioactivities.

    6. Metabolite Profiling of Leek (Allium porrum L) Cultivars by 1H NMR and HPLC–MS (pages 220–228)

      Tuula H. Soininen, Niko Jukarainen, Pasi Soininen, Seppo O. K. Auriola, Riitta Julkunen-Tiitto, Wieslaw Oleszek, Anna Stochmal, Reijo O. Karjalainen and Jouko J. Vepsäläinen

      Version of Record online: 10 JAN 2014 | DOI: 10.1002/pca.2495

      We quantified 17 metabolites from leek cultivars by HPLC–MS and a novel 1H-NMR/CTLS technique. The total concentration of carbohydrates and nine amino acids varied by fourfold in leek juice from different cultivars, while the total concentrations of four organic acids were similar in all cultivars. Threefold differences in flavonol concentrations were detected between cultivars. Different segments of leek exhibited remarkable variation in both number and amount of flavonols.

    7. Simultaneous Characterisation of Fifty Coumarins from the Roots of Angelica dahurica by Off-line Two-dimensional High-performance Liquid Chromatography Coupled with Electrospray Ionisation Tandem Mass Spectrometry (pages 229–240)

      Bin Li, Xu Zhang, Juan Wang, Le Zhang, Bowen Gao, Shepo Shi, Xiaohui Wang, Jun Li and Pengfei Tu

      Version of Record online: 30 JAN 2014 | DOI: 10.1002/pca.2496

      A method using off-line two-dimensional high-performance liquid chromatography coupled with electrospray tandem mass spectrometry (off-line 2D-HPLC–ESI/MSn) was developed for the simultaneous characterization of coumarins in the roots of Angelica dahurica. In total 50 coumarins, including 32 linear-type furanocoumarins, 16 bifuranocoumarins and two non-furanocoumarins, were identified. The MS fragmentation pathways of these coumarins were proposed. The method described here allows rapid and convenient identification of the coumarins in A. dahurica, and may be applied to other linear-type furanocoumarins-riched herbal medicines.

    8. Rapid Separation of Free Fatty Acids in Vegetable Oils by Capillary Zone Electrophoresis (pages 241–246)

      Renata Takabayashi Sato, Renata de Jesus Coelho Castro, Patrícia Mendonça de Castro Barra and Marcone Augusto Leal de Oliveira

      Version of Record online: 23 JAN 2014 | DOI: 10.1002/pca.2499

      Introduction – Free fatty acids in olive oils results in lipid deterioration.

      Objective – Free fatty acids determination by capillary zone electrophoresis.

      Method – 15 mm NaH2PO4-Na2HPO4 at pH ~6.86, 4.0 mm of sodium dodecybenzenesulphonate, 8.3 mm of Brij 35®, 45% v/v of acetonitrile and 2.1% of 1-octanol.

      Results – Determination of free fatty acids in olive oils and soybean oil.

      Conclusion – The method make possible the determination of individual amount of the free fatty acids in real samples.

    9. Sensitive and Selective Determination of Phenolic Compounds from Aromatic Plants Using an Electrochemical Detection Coupled with HPLC Method (pages 247–254)

      Alberto Cantalapiedra, Mª Jesús Gismera, Mª Teresa Sevilla and Jesús R. Procopio

      Version of Record online: 23 JAN 2014 | DOI: 10.1002/pca.2500

      The simultaneous determination of thymol, vainillin, eugenol and carvacrol in different samples is successfully performed by RP-HPLC using spectrophotometric, amperometric and coulometric detection. The highest sensitive responses and the lowest LOD were obtained in coulometric detection mode. Both electrochemical detection modes permit to obtain more selective responses and lower background signals than the observed with the diode-array detector. The low LODs obtained make this methodology very competitive and adequate for quality control of these phenolic compounds.

    10. Tandem Solid-Phase Extraction Followed by HPLC–ESI/QTOF/MS/MS for Rapid Screening and Structural Identification of Trace Diterpenoids in Flowers of Rhododendron molle (pages 255–265)

      Hong-Yan Zou, Jun Luo, De-Ran Xu and Ling-Yi Kong

      Version of Record online: 23 JAN 2014 | DOI: 10.1002/pca.2501

      Tandem solid phase extraction (PA and C18E) followed by HPLC-ESI/QTOF/ MS/MS was applied to enrich and detect the trace diterpenoids from the flowers of Rhododendron molle G. Don (a Traditional Chinese Medicine named ‘Naoyanghua’) for the first time. A total of 14 diterpenoids was detected, and eight ones were identified by comparison with references and other six based on fragmentation analysis. This technique will facilitate qualitative research analysis of these kinds of diterpenoids from herbal medicines of genus Rhododendron.

    11. Thin-layer Chromatographic Identification of Chinese Propolis Using Chemometric Fingerprinting (pages 266–272)

      Tie-xin Tang, Wei-yan Guo, Ye Xu, Si-ming Zhang, Xin-jun Xu, Dong-mei Wang, Zhi-min Zhao, Long-ping Zhu and De-po Yang

      Version of Record online: 4 FEB 2014 | DOI: 10.1002/pca.2502

      TLC identification of Chinese propolis using chemometric fingerprinting.

    12. Chemometric Resolution Approaches in Characterisation of Volatile Constituents in Plantago ovata Seeds using Gas Chromatography–Mass Spectrometry: Methodology and Performance Assessment (pages 273–281)

      Hooman Seifi, Saeed Masoum, Soodabe Seifi and Ebrahim Haghir Ebrahimabadi

      Version of Record online: 23 JAN 2014 | DOI: 10.1002/pca.2503

      GC-MS combined with chemometric resolution method such as multivariate curve resolution-alternating least squares (MCR-ALS), provides a perfectly way for rapid and accurate analysis of the volatile components of Plantago ovata. Results of this study show that the 71 constituents that are qualitatively recognized represent 94.53% of the total relative content of constituents from Plantago ovata oil, whereas without applying the chemometric methods only 51 constituents were identified by direct searching utilising a mass database.

    13. One-step Separation and Purification of Two Chromones and One Pyrone from Aloe barbadensis Miller: a Comparison Between Reversed-phase Flash Chromatography and High-speed Counter Current Chromatography (pages 282–288)

      Jia-Sheng Zhong, Jin-Zhi Wan, Wen-Jing Ding, Xiao-Fang Wu and Zhi-Yong Xie

      Version of Record online: 5 FEB 2014 | DOI: 10.1002/pca.2504

      Two efficient, low-cost and high-yield methods – reversed-phase flash chromatography (RP-FC) and high-speed counter current chromatography (HSCCC) – were successfully developed for the one-step separation and purification of two chromones and one pyrone from Aloe barbadensis Miller. A comparison in performance between the two selected methods was also performed. Both methods would afford sufficient amounts of high-purity compounds for chromatographic purposes and pharmacological activity screening.

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