University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf

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Amines, poly

Citations 5

"Multi-enzyme-containing Tissue-based And Ferrocene-mediated Bioelectrode For The Determination Of Polyamines"
Electroanalysis 1992 Volume 4, Issue 5 Pages 521-525
Meng Shan Lin, Minoru Hare, Garry A. Rechnitz

Abstract: Ground oat seedling tissue (which contains polyamine oxidase and peroxidase) was mixed with 2 to 9% (w/w) of graphite - mineral oil (3:2) paste containing 2% of ferrocene, and the mixture was firmly packed into the cavity of a flow cell electrochemical detector or, for steady-state experiments, into the end of a tubular electrode (3 mm i.d.). The electrode tip was smoothed on paper. Polyamine oxidase catalyses the oxidation of polyamines, O as co-substrate is reduced to H2O2, and the peroxidase then oxidizes ferrocene to ferricinium at the expense of H2O2; the signal is monitored reductively at 0.0 V vs. Ag - AgCl. Steady-state amperometric and cyclic voltammetric experiments were carried out in conjunction with a Pt-wire counter electrode; for a working electrode containing 7% of oat seedling tissue, response to spermidine or spermine in 0.1 M phosphate buffer of pH 7 was rectilinear up to 15 or 7.5 µM, respectively, and the corresponding detection limits were 0.19 and 1.15 µM. In the flow injection analyzes, carried out with the same buffer, the Ag - AgCl reference electrode was placed in a compartment downstream of the flow cell, with a stainless steel auxiliary electrode downstream of this, and PTFE tubing was used. Response to spermidine or spermine was rectilinear up to 20 or 15 µM, respectively. The electrodes did not respond to injections of 0.1 µM-ascorbic acid, uric acid, histamine, 4-aminobutyric acid or agmatine.
Sensor Electrode Interferences

"Chromatography, Flow Injection Analysis And Electrophoresis In Computer Assisted Comparative Biochemistry: Its Application And Possibilities In Clinical Research. Preliminary Studies On Crohns Disease"
J. Chromatogr. A 1988 Volume 440, Issue 1 Pages 261-273
V. R. Villanueva and M. Mardon

Abstract: A computer-assisted multicomponent analytical system, developed for comparative biochemical studies, was used for a clinical study of Crohn's disease in which 73 subjects, of comparable age and sex distribution, were considered: 40 with Crohn's disease, 16 with ulcerative colitis and 17 healthy volunteers as controls. Blood samples (5 ml) were taken to recover plasma and red cells. After extraction and fractionation of low- and high-molecular weight substances, the samples were analyzed by ion-exchange chromatography and electrophoresis. The contents of amino acids, sugars, polyamines and proteins in the plasma and the red cells from the three groups of individuals were compared using statistical (means, variance, principal components analysis) and graphical profile methods. The first results indicate that the content of red cells, in comparison with plasma, allows the best differentiation of the three groups of subjects considered. In particular, the amino acids (Asp, Thr, Ser, Glu, Gly, Ala and Leu), the polyamines (spermidine and spermine) and glucose, show the most significant differences. The methodology followed and the results obtained, together with possible uses of this computer-assisted multicomponent analytical system in problems concerning clinical research, are discussed.
Blood Plasma Clinical analysis HPIC Electrophoresis Computer Chemometrics Multicomponent

"High Performance Liquid Chromatographic Determination Of Polyamines In Selected Vegetables With Post-column Fluorimetric Derivatization"
J. Chromatogr. A 1993 Volume 628, Issue 2 Pages 199-204
Hideaki Ohta, Yuko Takeda, Koh-Ichi Yoza and Yoichi Nogata

Abstract: A method is described for the HPLC analysis of the aliphatic polyamines agmatine, putrescine, cadaverine, spermidine and spermine in vegetables. Sample (1 g) was homogenised with 7 mL of 5% perchloric acid, cooled for 1 h at 0°C, and centrifuged. The supernatant was analyzed on a column (3.5 cm x 6 mm) of Polyaminepak (strong cation-exchange resin, 5 µm) with a mobile phase (0.65 mL min-1) of 1.0 M sodium citrate (pH 5.4) - acetonitrile (9:1). Post-column derivatization with phthalaldehyde (details given) and subsequent fluorescent detection was used.
Vegetable HPLC Fluorescence Post-column derivatization

"Monitoring Of The Uptake And Metabolism Of Amino-oxy-analogues Of Polyamines In Cultured Cells By High Performance Liquid Chromatography"
J. Chromatogr. B 1992 Volume 574, Issue 1 Pages 17-21
Tapani Hyvönen* and Tuomo A. Keinänen, Alex R. Khomutov, Radii M. Khomutov, Terho O. Eloranta

Abstract: Cultured kidney cells were disrupted in cold 5% sulfosalicylic acid solution, and the polyamine amino-oxy-analogues were derivatized with acetone or ethyl methyl ketone in phosphate-buffered medium (pH 7.4) for 1 h. The resulting solution was analyzed by HPLC at 37°C on a column (10 cm x 2.1 mm) of Hypersil ODS (5 µm), which was pre-equilibrated with buffer A [8 mM octanesulfonate and 0.1 mM EDTA in 0.1 M potassium phosphate (pH 2.5) - acetonitrile (49:1)]. Elution was effected (at 0.5 mL min-1) with buffer A for 5 min, followed by a linear gradient to 75% of buffer B [8 mM octanesulfonate in 0.2 M potassium phosphate (pH 3.1) - acetonitrile (7:3)] over 15 min and, after 5 min, return to the starting conditions in 3 min. The analytes were then derivatized with phthalaldehyde (details given) for fluorimetric detection at 425 nm (excitation at 340 nm). The ketone used for the first derivatization depended on the separation required. The detection limit was 20 to 30 pmol and response (based on peak area) was rectilinear up to 4 nmol. The method was used to measure the stability of amino-oxy-analogues of putrescine and spermidine.
Cell HPLC Fluorescence Post-column derivatization

"Analysis Of Polyamines In Chinese Caterpillar Fungus"
Zhongcaoyao 1993 Volume 24, Issue 2 Pages 71-72
Zhu, C.;Aratsu, M.

Abstract: Identification and determination of polyamines (e.g., propane-1,3-diamine, putrescine, spermidine, spermine, cadaverine and homospermidine) present in Chinese caterpillar fungus (Cordyceps sinensis Sacc.) was carried out by HPLC, GC and GC - MS. Powdered sample (10 g) was treated with 1 M HClO4 and separated on columns of Dowex-50 W-X8 (4 cm x 2 cm) and CM-Cellulose (0.8 cm x 0.5 cm). The resulting solution was analyzed by HPLC on a 62110 FK column (8 cm x 4.6 mm) with post-column derivatization (details given); elution was effected with a mobile phase of KCl - K citrate solution (37.275:108.137) and fluorescence detection was at 450 nm (excitation at 365 nm). For determination, the resulting solution was acylated with heptafluorobutyric anhydride, before analysis by GC and GC - MS on a column of 3% SE-30 and 70-eV MS detection. Results were tabulated.
Caterpillar Fungus Mass spectrometry GC Fluorescence Post-column derivatization