Phytochemical Analysis

Cover image for Vol. 25 Issue 2

March/April 2014

Volume 25, Issue 2

Pages 97–184

  1. Research Articles

    1. Top of page
    2. Research Articles
    1. Characterisation of the Metabolism of Pogostone In Vitro and In Vivo Using Liquid Chromatography with Mass Spectrometry (pages 97–105)

      Yucui Li, Ziren Su, Shuhai Lin, Chuwen Li, Ya Zhao, Xiang Gao, Yongquan Lai, Xiaoli Wu, Hanzhi Wu, Zongwei Cai and Xiaoping Lai

      Article first published online: 26 NOV 2013 | DOI: 10.1002/pca.2471

      The metabolic profile of pogostone in vitro and in vivo was studied by using LC -MS techniques. In total, three mono-hydroxylated, one di-hydroxylated, one mono-oxygenated, one di-oxygenated metabolite, one hydrolysis and one hydroxy conjugated metabolites were found. And hydroxylation was demonstrated to be a major metabolic pathway of pogostone.

    2. HPLC Profiling with At-line Microdilution Assay for the Early Identification of Anti-fungal Compounds in Plants from French Polynesia (pages 106–112)

      Samuel Bertrand, Charlotte Petit, Laurence Marcourt, Raimana Ho, Katia Gindro, Michel Monod and Jean-Luc Wolfender

      Article first published online: 23 SEP 2013 | DOI: 10.1002/pca.2473

      An anti-fungal at-line HPLC profiling was devised for the rapid and efficient localisation of anti-Candida compounds in crude plant extracts. The approach is based on HPLC microfractionation with a microdilution assay a 96-well plates. This format is also compatible for MS and NMR dereplication of the active compounds. It was applied to the search for anti-Candida compounds in five plants from French Polynesia and lead to the rapid identification of betulinic acid as the active compound from Alphitonia zizyphoides.

    3. Identification of Nuclear Factor-κB Inhibitors and β2 Adrenergic Receptor Agonists in Chinese Medicinal Preparation Fuzilizhong Pills Using UPLC with Quadrupole Time-of-flight MS (pages 113–121)

      Linyi Dong, Binfeng Cheng, Yi Luo, Ning Zhang, Hongquan Duan, Min Jiang, Yiming Wang, Gang Bai and Guoan Luo

      Article first published online: 23 SEP 2013 | DOI: 10.1002/pca.2474

      Fuzilizhong Pills, a famous prescription in Treatise on Febrile Diseases for treating dyspnea and pulmonary oedema, was analysed using UPLC-Q-TOF MS combined with dual-bioactive (NF-κB and β2-adrenergic receptor) luciferase reporter assay systems to identify anti-inflammatory and spasmolytic constituents. Two β2-adrenergic receptor agonists and three terpenoidal analogues of NF-κB inhibitors were characterised. This strategy clearly demonstrated that dual bioactivity-integrated fingerprinting is a powerful tool for the improved screening and identification of potential dual-target lead compounds in complex herbal medicines.

    4. Quantitative Analysis of Amygdalin and Prunasin in Prunus serotina Ehrh. using 1H-NMR Spectroscopy (pages 122–126)

      Lúcia P. Santos Pimenta, Menno Schilthuizen, Robert Verpoorte and Young Hae Choi

      Article first published online: 23 SEP 2013 | DOI: 10.1002/pca.2476

      Prunasin and amygdalin were quantified by 1H-NMR in Prunus serotina leaves using the signal of the –CHCN groups, which are well resolved between δ 5.5 and δ 6.0. Trimethylsilylpropionic acid sodium salt-d4 was added as internal standard. The NMR-based protocol allowed the rapid, simple and direct quantification of amygdalin and prunasin in dried P. serotina leaves.

    5. Preparative Isolation of six Anti-Tumour Biflavonoids from Selaginella Doederleinii Hieron by High-Speed Counter-Current Chromatography (pages 127–133)

      Shaoguang Li, Meifeng Zhao, Yuxiang Li, Yuxia Sui, Hong Yao, Liying Huang and Xinhua Lin

      Article first published online: 23 SEP 2013 | DOI: 10.1002/pca.2478

      A bioassay-guided method is developed for isolation of antitumor biflavones. mg level of six antitumor biflavones were obtained from S. doederleinii by HSCCC. Antitumor biapigenin and binaringenin were found at first time in this herb. The cytotoxicities of the 2'', 3''-dihydro-3', 3'''-biapigenin and 3', 3'''-binaringenin were studied originally. It provides method references for preparation of active biflavones from herbs.

    6. Extraction Yields and Anti-oxidant Activity of Proanthocyanidins from Different Parts of Grape Pomace: Effect of Mechanical Treatments (pages 134–140)

      M. de Sá, V. Justino, M. I. Spranger, Y. Q. Zhao, L. Han and B. S. Sun

      Article first published online: 3 OCT 2013 | DOI: 10.1002/pca.2479

      More total polyphenols can be extracted from milled skins than from its entire form. Seeds present the highest total phenol, oligomeric and polymeric proanthocyanidin content, and similar extraction yield was found between milled and squashed tissues. HPLC analysis showed no difference in extraction yield of low-molecular-weight proanthocyanidins between milled and entire stems. The use of entire stems and squashed seeds makes manipulation simpler and cost-efficient. Antioxidant activity showed positive correlation with total phenol content, galloylated oligomers and polymeric proanthocyanidins.

    7. Simultaneous Determination of Sulphoraphane and Sulphoraphane Nitrile in Brassica Vegetables using Ultra-Performance Liquid Chromatography with Tandem Mass Spectrometry (pages 141–146)

      Laura Alvarez-Jubete, Thomas J. Smyth, Juan Valverde, Dilip K. Rai and Catherine Barry-Ryan

      Article first published online: 16 OCT 2013 | DOI: 10.1002/pca.2480

      The objective of this study was to develop and validate an UPLC-MS/MS method for the simultaneous analysis of sulphoraphane and sulphoraphane nitrile from broccoli. The retention times for sulphoraphane and sulphoraphane nitrile were 0.4 and 0.6 min respectively and total run time was 3 min. The validated UPLC-MS/MS method for simultaneous detection of sulphoraphane and sulphoraphane nitrile was shown to be applicable to broccoli plants and is expected to be applicable to other cruciferous sources.

    8. Identification and Anti-oxidant Capacity Determination of Phenolics and their Glycosides in Elderflower by On-line HPLC–CUPRAC Method (pages 147–154)

      S. Esin Çelik, Mustafa Özyürek, Kubilay Güçlü, Esra Çapanoğlu and Reşat Apak

      Article first published online: 10 JAN 2014 | DOI: 10.1002/pca.2481

      An on-line HPLC–CUPRAC assay with a post-column derivatization system was applied for screening phenolic antioxidants and their glycosides in elderflower. Separated components on the HPLC column were derivatized by Cu(II)-Nc reagent in the reaction coil and post-column detection of the reduction product, Cu(I)-Nc, equivalent to anti-oxidant constituents was monitored at 450 nm by measuring the increase in absorbance. The phenolic compounds in elderflower extract were identified and quantified with much better sensitivities than those of on-line HPLC–DPPH assay. In contrast to the widely used on-line HPLC–ABTS assay, post-column identification of flavonol glycosides (kaempferol derivatives) and calculation of their contribution to the total anti-oxidant capacity of a complex mixture could be made with the on-line HPLC–CUPRAC assay.

    9. A Thin-layer Chromatography Autographic Method for the Detection of Inhibitors of the Salmonella PhoP–PhoQ Regulatory System (pages 155–160)

      Mario O. Salazar, Gaston Viarengo, Mariela I. Sciara, Pablo M. Kieffer, Eleonora Garcia Vescovi and Ricardo L. E. Furlan

      Article first published online: 4 NOV 2013 | DOI: 10.1002/pca.2482

      A bioautographic assay suitable for the localisation of inhibitors of the PhoP–PhoQ regulatory system activity in Salmonella enterica serovar Typhimurium present in a complex matrix is described. This bioactivity was detected by coupling the β-galactosidase-catalysed production of a blue product to the activity of the PhoP–PhoQ system. The assay was used to analyse several hydrolysed extracts, detecting linolenic, linoleic and palmitoleic acids as the first naturally occurring organic compounds that act as inhibitory input signals of the PhoP–PhoQ system.

    10. Chemometric Discrimination of Different Tomato Cultivars Based on Their Volatile Fingerprint in Relation to Lycopene and Total Phenolics Content (pages 161–169)

      Sonia A. Socaci, Carmen Socaciu, Crina Mureşan, Anca Fărcaş, Maria Tofană, Simona Vicaş and Adela Pintea

      Article first published online: 21 NOV 2013 | DOI: 10.1002/pca.2483

      ITEX/GC-MS technique was used to fingerprint the volatile composition of ten different tomato cultivars. Principal component analysis revealed that the tomato cultivars can be easily discriminated based on their characteristic volatile composition. The chemometric approach also showed that total phenolic content, which is highly correlated with phenotypic and biochemical differences between tomato cultivars, plays a crucial role in their discrimination.

    11. Comparative Study of the Methodology Used in the Extraction of Isoflavones from Legumes Applying a Modified QuEChERS Approach (pages 170–177)

      Myriam Bustamante-Rangel, Lara Pérez-Martín and M. Milagros Delgado-Zamarreño

      Article first published online: 2 DEC 2013 | DOI: 10.1002/pca.2487

      A study of five different agitation techniques, using QuEChERS methodology, for the extraction of isoflavones from legume samples was made. Separation and quantification were carried out using LC-MS/MS. The main advantages of the proposed extraction procedures were their simplicity, speed, reliability and low cost. The use of thermostatted shaking tray for the extraction of chickpeas and white beans and ultrasound probe for lentil samples were proposed. The importance of the agitation mode in the extraction of analytes should be noted.

    12. Dynamic Ultrasonic Nebulisation Extraction Coupled with Headspace Ionic Liquid-based Single-drop Microextraction for the Analysis of the Essential Oil in Forsythia suspensa (pages 178–184)

      Jinjuan Yang, Hongmin Wei, Xiane Teng, Hanqi Zhang and Yuhua Shi

      Article first published online: 18 DEC 2013 | DOI: 10.1002/pca.2490

      Ionic liquids have attracted much attention as an extraction solvent in single-drop microextraction. However, it is difficult to couple with GC. Thus, a new injection technique was described. The extracts in ionic liquid were evaporated through a thermal desorption unit, while ionic liquid was removed out of GC injector. The proposed method was environmentally friendly, time saving, with high efficiency and low consumption. It would extend the application range of HS-SDME and would be useful for aromatic plants analysis.