CONTRIBUTION TO THE STUDY OF Himatanthus sucuuba: LATEX MACROMOLECULE, MICROELEMENTS ANDCARBOHYDRATES

ABSTRACT:

The polymeric material in the latex of Himatanthus sucuuba (Spruce) Woodson was identified by spectroscopic methods as cis-polyisoprene (Mn = 192; Mw = 571; Mw/Mn = 2.97). ICP-MS analysis of microelements in the aqueous phase showed the most abundant to be Ca (354 μg/g) and Mg (250 μg/g). Carbohydrate analysis of the aqueous phase by HPLC-PAD showed arabinose, glucose, xylose, rhamnose and galactose to be the predominant saccharides.
KEYWORDS: Apocynaceae, Himatanthus, latex, cis-polyisoprene, microelements, carbohydrates

PDF] CONTRIBUTION TO THE STUDY OF Himatanthus sucuuba : LATEX

Study on Solid Phase Extraction and Spectrophotometric Determinationof Vanadium with 2-(2-Quinolylazo)-5-Diethylaminophenol

A sensitive, selective and rapid method has been developed for the determination μg/L level of vanadium ion based on the rapid reaction of vanadium(V) with 2-(2-quinolylazo)-5-diethylaminophenol (QADEAP) and the solid phase extraction of the colored chelate with C18 cartridge. The QADEAP reacts with V(V) in the presence of citric acid-sodium hydroxide buffer solution (pH = 3.5) and cetyl trimethylammonium bromide (CTMAB) medium to form a violet chelate of a molar ratio 1 : 2 (V(V) to QADEAP). This chelate was enriched by solid phase extraction with C18 cartridge and the enrichment factor of 50 was obtained by elution of the chelates from the cartridge with ethanol. The molar absorptivity of the chelate is 1.28 × 105 L mol−1 cm−1 at 590 nm in the measured solution. Beer’s law is obeyed in the range of 0.01-0.6 μg/mL. The detection limit is 0.04 μg/L in the original samples. This method was applied to the determination of vanadium(V) in water and biological samples with good results.
Key Words : 2-(2-Quinolylazo)-5-diethylaminophenol, Vanadium, Spectrophotometry, Solid phase extraction

PDF] Study on Solid Phase Extraction and Spectrophotometric

SOIL GENESIS ON FELSIC ROCKS IN THE ST. FRANCOIS MOUNTAINS. I. THE ROLE OF SAPROLITE AND ITS INFLUENCE ON SOIL PROPERTIES.

Abstract
One soil profile from Taum Sauk Mountain and two soil profiles from Mudlick Mountain in the St. Francois Mountains of Southeast Missouri were investigated to determine if the soils evolved from the underlying rock unit and to characterize the role of saprolite on soil genesis. Taum Sauk Mountain is composed of rhyolite lava and ash flow of the Van East Group. The rock is quartz and orthoclase phenocrysts in an orthoclase groundmass. Mudlick Mountain consists of rock composed of orthoclase, oligoclase, and a minor amount of quartz phenocrysts in a groundmass of quartz and orthoclase. The shallow Aquic Hapludult formed on the summit of Taum Sauk Mountain shows no evidence of saprolite, whereas the two Typic Paleudalfs formed on Mudlick Mountain rest on a thick layer of saprolite. The presence of minerals in the host rock that weather more easily is largely responsible for the development of the saprolite on Mudlick Mountain. The very strongly acid Typic Paleudalfs have textures ranging from cobbly silt loam to cobbly sandy loam for the eluvial horizons, whereas the argillic and C horizons are generally fine or clayey-skeletal. The extremely acid Aquic Hapludults have a fine-silty texture. The clay mineralogy is mixed, with hydroxy-Al interlayered vermiculite and hydrous mica prominent in the eluvial horizons and kaolinite dominating the Bt and C horizons. The aluminum hydroxide potentials of soil solutions extracted from selected horizons are saturated or slightly supersaturated with respect to kaolinite. Elemental analysis demonstrates that the soil and saprolite originate from the same parent material and that elemental depletion is important to the formation of the saprolite. Iron oxides represent nearly all of the total Fe, and Fe is correlated highly with clay content. The rare earth elements are more abundant in the soil than in the host rock. The weathered thin loess capping is suggested as the source of the rare earth elements.
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Trace element geochemistry in acid rock drainage

INTRODUCTION
Acid rock drainage (ARD) has an impact upon our water, soil and plant quality and fish habitat with regard to trace elements, whether in a toxic or non-toxic, available or non-available form. Its impact will be determined by the type and amount of trace element(s) within the host medium (e.g. mineral assemblage). Prediction of trace element geochemistry is readily determined from standard analytical methods, providing that the sample medium is collected and analyzed in a manner that includes a program of Quality Assurance and Quality Control (QA/QC). The cost of trace element analyses and geochemistry prediction is relatively inexpensive when undertaken as part of an overall ARD study.

Article

Differential Pulse Polarographic Determination of Trace Amounts of Lead in Alloys and Biological Samples after Column Preconcentration Using Nitroso-S

Abstract:

A highly selective, sensitive, rapid, and economical differential pulse polarographic method has been developed for the determination of trace amounts of lead in various standard alloys and biological samples after the adsorption of its 2-nitroso-l-naphthol-4-sulfonic acid (nitroso-S)—tetradecyldimethylbenzylammonium (TDBA) chloride on microcrystalline naphthalene in the pH range of 8.0–10.5. After filtration, the solid mass is shaken with 9.0 mL of 1 M hydrochloric acid, and lead is determined by differential pulse polarography (DPP). Lead can alternatively be quantitatively adsorbed on 2-nitroso-l-naphthol-4-sulfonic acid-tetradecyldimethylbenzylammonium-naphthalene adsorbent packed in a column and determined similarly. In this case, 1.0 g of lead can be concentrated in a column from 500 mL of an aqueous sample in which its concentration is as low as 2 ng/mL. Characterization of the electroactive process included an examination of the degree of reversibility. Various parameters, such as the pH effect, volume of aqueous phase, HCl concentration, reagent concentration, naphthalene concentration, shaking time, and the interference of a number of metal ions on the determination of lead were studied in detail to optimize the conditions for determination in standard alloys and standard biological samples.
Document Type: Research article
DOI: 10.1023/B:JANC.0000043917.37406.b3
Affiliations: 1: Department of Chemistry, Shahid Bahonar University of Kerman, Kerman, IRAN ma_taher@yahoo.com, Email: ma_taher@yahoo.com
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Recent development of the XANES spectral analysis methods for the structure characterization of metal complexes in solution.

Anal Sci. 2008;24(11):1385-92.
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Recent development of the XANES spectral analysis methods for the structure characterization of metal complexes in solution.

Kurisaki T, Matsuo S, Tóth I, Wakita H.

Department of Chemistry, Faculty of Science, Fukuoka University, Japan.Recent progress of the XANES (X-ray absorption near-edge structure) spectral analysis methods for the structure characterization of metal complexes (MC) in solution is reviewed. Typical examples showing the scheme of the apparatus for XAFS (X-ray absorption fine structure) data collection, preparation and handling of solution samples, data treatment and analysis for XANES spectra, and future of XANES spectroscopy are presented. Detailed examples for the apparatus developed for laboratory scale spectrometers for XANES together with a combined spectral analyses using multi scattering method (MS) and molecular orbital (MO) calculation are discussed.

PMID: 18997363 [PubMed]

Micro-channel chemiluminescence analysis using a peroxyoxalate reaction that works through liquid-liquid interface collapse under laminar-flow conditi

Anal Sci. 2008;24(11):1393-8.
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Micro-channel chemiluminescence analysis using a peroxyoxalate reaction that works through liquid-liquid interface collapse under laminar-flow conditions.

Tsukagoshi K, Hattori Y, Hayashi T, Nakajima R, Yamashita K, Maeda H.

Department of Chemical Engineering and Materials Science, Faculty of Science and Engineering, Doshisha University, Kyotanabe, Kyoto 610-0321, Japan. ktsukago@mail.doshisha.ac.jpAn oxalate reagent-hydrogen peroxide-fluorescent compound chemiluminescence reaction, i.e., peroxyoxalate chemiluminescence, was introduced into micro-channel chemiluminescence analysis (MCCLA) to establish the concept of MCCLA through the direct observation of fluorescence and chemiluminescence using a fluorescence microscope-CCD camera and a microscope-CCD camera. It was confirmed from visual data that chemiluminescence in the MCCLA generated through the liquid-liquid interface collapsed during the course of molecular diffusion in the micro-channel. In addition, the visual data of chemiluminescence were transformed to line drawings on a computer to obtain chemiluminescence profiles. The chemiluminescence profiles were examined in detail at various flow rates and detection points; the relationship between the residence times and the chemiluminescence peak heights, or areas in the profiles, was easily represented as one smoothly changing reaction curve. Furthermore, the fluorescent compounds were detected with high sensitivity and good reproducibility in MCCLA by turning the syringe pumps on and off to produce determinable chemiluminescence signals; a photomultiplier tube was used as a detector. The chemiluminescence intensities in the signals of erythrosine, rhodamine B, Rose Bengal, fluorescein isothiocyanate, and eosin Y were examined; their intensities increased in this order, and eosin Y responded over the range of 1 x 10(-9) - 1 x 10(-6) M with a detection limit of 1 x 10(-9) M (S/N = 3). Introducing of the peroxyoxalate chemiluminescence reaction into MCCLA can extend the analysis system to the analysis of various types of sample and applications incorporating fluorescence labeling techniques.

Biphasic electrospray ionization for the study of interfacial complexes.

Anal Sci. 2008;24(11):1399-404.
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Biphasic electrospray ionization for the study of interfacial complexes.

Prudent M, Méndez MA, Girault HH.

Laboratoire d'Electrochimie Physique et Analytique, Ecole Polytechnique Fédérale de Lausanne.Biphasic electrospray ionization (BESI) mass spectrometry is achieved by using a dual-channel microsprayer, where channels filled with different immiscible phases meet at the Taylor cone. Two types of interfacial complexation reactions have been studied: the interfacial complexation of aqueous lead ions by thioether crown molecules, and the interfacial complexation of an aqueous dipeptide by dibenzo-18-crown-6 as ionophore. The mass spectra also give valuable information on the stoichiometry of the complexation reaction.

PMID: 18997365 [PubMed]

Bioluminescent indicators for Ca2+ based on split Renilla luciferase complementation in living cells.

Anal Sci. 2008;24(11):1405-8.
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Bioluminescent indicators for Ca2+ based on split Renilla luciferase complementation in living cells.

Kaihara A, Umezawa Y, Furukawa T.

Department of Bio-Informational Pharmacology, Medical Research Institute, Tokyo Medical and Dental University, Chiyoda, Tokyo 101-0062, Japan. kaihara.bip@mri.tmd.ac.jpGenetically encoded bioluminescent indicators for intracellular Ca2+ are described here with CaM-M13 interaction-induced complementation of split Renilla luciferase. The Ca2+-induced interaction between CaM and M13 leads to complementation of the N- and C-terminal halves of split Renilla luciferase in living cells. This intramolecular interaction results in the spontaneous and simultaneous emission of bioluminescence split Renilla luciferase. This is how intracellular Ca2+ is illuminated with the intramolecular complementation of split Renilla luciferase. The Ca2+-dependent spontaneous and simultaneous emission of bioluminescence promises to reveal Ca2+ dynamics in living cells, and also in vivo using the present indicators.

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997366 [PubMed - indexed for MEDLINE]

Polymeric membrane sensors for the selective determination of dextromethorphan in pharmaceutical preparations.

Anal Sci. 2008;24(11):1409-14.
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Polymeric membrane sensors for the selective determination of dextromethorphan in pharmaceutical preparations.

El-Naby EH.

Narcotic Department, National Center for Social and Criminal Research, P. O. Zamalek Post, 11561, Cairo, Egypt. emanhasab@gmail.comThe construction and electrochemical response characteristics of poly(vinyl chloride) matrix ion-selective electrodes (ISEs) for dextromethorphan (DXM) hydrobromide are described. The membranes incorporate ion-association complexes of DXM with reineckate salt {[Cr(NH3)2(SCN)4]NH4} or phosphomolybdic acid [H3(PMo12O40)], as electroactive materials and dioctylphthalate or dibutylsebacate as a plasticizing solvent mediator. The sensors display a fast, stable and linear response with slopes of 54.4 to 59.5 mV/decade at pH 2.5-6.5 and a detection limit of 1.0 x 10(-6) M. Moreover, the sensors exhibit very good selectivity for DXM over opiate alkaloids, as well as organic and inorganic cations. The sensors proved to be useful for the determination of 5.0 x 10(-5)-1.0 x 10(-3) M DXM hydrobromide in pure as well as in dosage forms by direct potentiometry and standard addition methods. Determination of 5.0 x 10(-4) M DXM using the standard addition method and a sensor based on phosphomolybdate and dioctylphthalate shows an average recovery of 99.8% and a relative standard deviation (RSD) of 0.4%.

Publication Types:
Evaluation Studies

PMID: 18997367 [PubMed - indexed for MEDLINE]

Application of polyammonium cations to enzyme-immobilized electrode: application as enzyme stabilizer for bilirubin oxidase.

Anal Sci. 2008;24(11):1421-4.
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Application of polyammonium cations to enzyme-immobilized electrode: application as enzyme stabilizer for bilirubin oxidase.

Katano H, Tatsumi H, Hibi T, Ikeda T, Tsukatani T.

Department of Bioscience, Fukui Prefectural University, Japan. hajime@fpu.ac.jpBilirubin oxidase was stored in the solutions containing polyammonium salts for a given time at 30 degrees C, and the activity was assayed. The enzyme catalyzes the reaction: 4[Fe(CN)6]4- + 4H+ + O2 --> 4[Fe(CN)6]3- + 2H2O, and the activity can be measured by the absorbance at the wavelength for the absorption maxima of [Fe(CN)6)]3-. The results show that polyammonium cations comprising quaternary ammonium in the main chain and hydrophilic groups, such as hydroxyl and amide groups, stabilize the enzyme in solution. These polyammonium cations may act like a protective colloid. The membrane-covered electrode containing the polyammonium cations, the enzyme, and [Fe(CN)6]4-/3- in the internal solution phase was constructed. The electrode gave a well-defined current-potential curve with a steady state limiting current due to the polycation-[Fe(CN)6]4-/3- complex-mediated bioelectrocatalytic current for the reduction of O2. The time-dependent decrease of the limiting current indicates again the stabilizing effect of the polyammonium cations on the enzyme.

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997369 [PubMed - indexed for MEDLINE]

An amperometric glucose biosensor based on titania sol-gel/Prussian Blue composite film.

Anal Sci. 2008;24(11):1425-30.
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An amperometric glucose biosensor based on titania sol-gel/Prussian Blue composite film.

Liang R, Jiang J, Qiu J.

Department of Chemistry, Nanchang University, Nanchang 330031, China. rpliang@ncu.edu.cnAn improved amperometric glucose biosensor was constructed by immobilizing glucose oxidase (GOD) in a titania sol-gel film, which was prepared by a vapor deposition method, on a Prussian Blue (PB)-modified electrode. The method combined the merits of immobilizing biomolecules in the titania sol-gel film by vapor deposition method and the synergic catalysis effects of PB and GOD molecules. Results showed that the fabricated titania sol-gel/PB membrane possessed high surface area, good mechanical stability, and good hydrophilicity, which provided a biocompatible microenvironment for maintaining the bioactivity of the immobilized enzyme and prevented the enzyme from leaking out of the film. Therefore, the present biosensor exhibited fast response time (10 s), high sensitivity (12.74 muA cm(-2) mM(-1)), long-term operational stability, good suppression of interference, and a wide linear range from 0.02 to 15 mM with a low detection limit of 5 muM for the detection of glucose. In addition, this simple and controllable method could fabricate biosensors in batches with a very small amount of enzyme.

Publication Types:
Evaluation Studies Research Support, Non-U.S. Gov't

PMID: 18997370 [PubMed - indexed for MEDLINE]

Detection of cytochrome c at biocompatible nanostructured Au-lipid bilayer-modified electrode.

Anal Sci. 2008;24(11):1431-6.
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Detection of cytochrome c at biocompatible nanostructured Au-lipid bilayer-modified electrode.

Liu Y, Wei W.

State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Changsha 410082, P. R. China.The present work describes the dectection of cytochrome c (cyt c) at biocompatible aurum (Au) nanoparticle-structured supported bilayer lipid membrane (sBLM) modified with anionic sites. Au nanoparticles were directly deposited through sBLM modified with lauric acid (LA) to build a hybrid device of nanoscale electrode array via potential cycling in 10 mM HAuCl4 solution containing 0.1 M KCl. The properties of Au nanoparticle-doped sBLM composite were then characterized by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM). Results indicated that Au nanoparticles grew in voids of the sBLM with size around 20 - 30 nm. With SWV, after optimization, the results of the experiments indicate that the currents of cyt c were linear functions of its concentrations over the range from 1.0 x 10(-7) to 3.2 x 10(-6) M and the limit of detection (LOD, S/N = 3) was 5 x 10(-8) M. The influences of several common base pairs, amino acids and metal ions on determination of cyt c via this Au nanoparticle-doped sBLM composite were relatively low in experiments, suggesting the excellent biocompatibility of this detection method.

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997371 [PubMed - indexed for MEDLINE]

Electrochemical and spectroscopic investigations of protonated ferrocene-DNA intercalation.

Anal Sci. 2008;24(11):1437-41.
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Electrochemical and spectroscopic investigations of protonated ferrocene-DNA intercalation.

Shah A, Qureshi R, Janjua NK, Haque S, Ahmad S.

Department of Chemistry, Quaid-i-Azam University, 45320 Islamabad, Pakistan. afzal_toru@yahoo.comThe interaction of protonated ferrocene (PF) with chicken blood DNA (CB-DNA) has been investigated in vitro by cyclic voltammetry (CV) and UV-Vis spectroscopy as well as viscosity measurements under stomach pH and body temperature. The peak potentials shift in CV, hyperchromism in UV absorption titration, an increase in the viscosity of DNA and the results of the effect of ionic strength on the binding constant strongly support the intercalation of PF into the DNA double helix. The diffusion coefficients of PF in the presence and absence of DNA were 9.54 x 10(-11) and 1.34 x 10(-10) m2/s, respectively. The binding constant of the PF-DNA complex and the number of binding sites on a DNA molecule were calculated as being 3.07 x 10(2) M(-1) and 2.96, with the help of the Scatchard equation. An expression by Carter et al. was used for determining the binding site size (0.17 bp). The binding constant was also determined by UV absorption titration.

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997372 [PubMed - indexed for MEDLINE]

Square wave voltammetry in the determination of Ni2+ and Al3+ in biological sample.

Anal Sci. 2008;24(11):1443-7.
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Square wave voltammetry in the determination of Ni2+ and Al3+ in biological sample.

Paulino AT, Vargas AM, Santos LB, Nozaki J, Muniz EC, Tambourgi EB.

Universidade Estadual de Campinas, Departamento de Sistemas Químicos, Faculdade de Engenharia Química, Campinas-São Paulo, Brazil. atpaulino10@gmail.comIn this contribution, the amounts of Ni (nickel) and Al (aluminum) in tilapias (Oreochromis niloticus) were determined using square wave voltammetry (SWV) with glassy carbon working microelectrode with a mercury thin film, platinum counter electrode, and Ag/AgCl reference electrode. Ni was studied through the formation of the dimethylglyoxime-Ni (Ni-DMG) complex, while Al was studied through the formation of the Alizarin R-Al complex. The detection limit found for Ni-DMG and Alizarin R-Al complexes were 1.70 x 10(-7) and 1.0 x 10(-8) mol L(-1), respectively. The voltammetric anodic curves for the Alizarin R-Al complex were recorded over the potential range from -0.8 to -0.05 V while the voltammetric cathodic curve for the Ni-DMG complex was recorded over the potential range from -0.7 to -1.2 V. These methods detected low concentrations of Ni and Al in biological samples efficiently.

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997373 [PubMed - indexed for MEDLINE]

Determination of losartan and triamterene in pharmaceutical compounds and urine using cathodic adsorptive stripping voltammetry.

Anal Sci. 2008;24(11):1449-54.
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Determination of losartan and triamterene in pharmaceutical compounds and urine using cathodic adsorptive stripping voltammetry.

Ensafi AA, Hajian R.

Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran. Ensafi@cc.iut.ac.irA square-wave voltammetric procedure for the electroanalytical determination of losartan and triamterene in Britton-Robinson buffer (pH 3.0, 0.1 mol L(-1)) as a supporting electrolyte containing 30 ng mL(-1) of copper ions was developed. Opposite to the case of triamterene, losartan can not be reduced at a mercury electrode alone, but a new peak appears at -0.25 V in the presence of copper due to the formation of a complex between copper(II) and losartan. An accumulation potential of -0.30 V during 80 s for the prior adsorption of losartan-copper(II) and triamterene on the electrode surface was used. The response of the system was found to be linear in the range of 30.0 - 270.0 nmol L(-1) for losartan and two linear dynamic ranges containing 0.5-200.0 and 200.0-400.0 nmol L(-1) of triamterene. The limits of detections were 9.7 and 0.3 nmol L(-1) for losartan and triamterene, respectively. The relative standard deviations for five replicate analyses of 100.0 and 10.0 nmol L(-1) losartan and triamterene were 5.5%. Applicability to assay the drugs in urine and pharmaceutical formulations was illustrated with satisfactory results. The direct-current polarography of triamterene indicates that the reduction of a related drug is strongly dependent on the pH of the solution. A linear segment was found with slope value of -63.6 mV pH(-1) in the pH range of 2.0 - 6.0. The stoichiometry and complex formation constant (beta) for losartan-Cu(II), number of transfer electrons (n), transfer coefficients (alpha) and number of proton transfers were also estimated.

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997374 [PubMed - indexed for MEDLINE]

Membrane solubilization technique for spectrophotometric determination of trace formaldehyde in rainwater.

Anal Sci. 2008;24(11):1455-9.
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Membrane solubilization technique for spectrophotometric determination of trace formaldehyde in rainwater.

Murai K, Okano M, Kuramitz H, Hata N, Kawakami T, Taguchi S.

Graduate School of Science and Engineering (Science Div.), University of Toyama, Toyama 930-8555, Japan.A simple and sensitive spectrophotometry for formaldehyde in water by membrane solubilization technique was proposed. Formaldehyde was converted into a blue cationic dye with 3-methyl-2-benzothiazolinone hydrazone, and the dye was retained on a membrane filter as an ion-associate with tetraphenylborate anion. The filter retaining the blue dye was dissolved in 2-methoxyethanol containing sulfuric acid, and the absorbance of the solution was measured at 670 nm against the reagent blank. The formaldehyde from 0.007 to 0.2 mg L(-1) was determined with an RSD of less than 5%, and the detection limit was 0.002 mg L(-1). The proposed method was very simple and rapid. Twenty minutes was sufficient for the entire analytical procedure. When the method was applied to rainwater, the analytical results were in good agreement with those obtained by GC/MS.

Publication Types:
Evaluation Studies

PMID: 18997375 [PubMed - indexed for MEDLINE]

Characterization of fluorophores released from three kinds of lake phytoplankton using gel chromatography and fluorescence spectrophotometry.

Anal Sci. 2008;24(11):1461-7.
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Characterization of fluorophores released from three kinds of lake phytoplankton using gel chromatography and fluorescence spectrophotometry.

Aoki S, Ohara S, Kimura K, Mizuguchi H, Fuse Y, Yamada E.

Department of Chemistry and Material Technology, Kyoto Institute of Technology, Kyoto 606-8585, Japan.Three kinds of phytoplankton were cultivated, and the contribution of dissolved organic matter (DOM) released from the phytoplankton was examined to clarify the cause of organic pollution of Lake Biwa. Microcystis aeruginosa, Staurastrum dorcidentiferum, and Cryptomonas ovata were evaluated with regard to cultivation. A significant peak (M(w): <3000> Microcystis aeruginosa > Staurastrum dorcidentiferum. These results suggest that the increase of the refractory organic matter in Lake Biwa may be attributed to a change of the predominant phytoplankton.

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997376 [PubMed - indexed for MEDLINE]

Simultaneous determination of L-glutamate, acetylcholine and dopamine in rat brain by a flow-injection biosensor system with microdialysis sampling.

Anal Sci. 2008;24(11):1469-73.
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Simultaneous determination of L-glutamate, acetylcholine and dopamine in rat brain by a flow-injection biosensor system with microdialysis sampling.

Yao T, Okano G.

Department of Applied Chemistry, Graduate School of Engineering, Osaka Prefecture University, Naka, Sakai, Osaka 599-8531, Japan.A flow-injection biosensor system with an on-line microdialysis sampling system is proposed for the simultaneous detection of neurotransmitters (L-glutamate, acetylcholine and dopamine) released from rat brain cells. The dialysate collected in the sample loop from the microdialysis probe was automatically injected into the flow-injection line with a triple electrode arranged perpendicular to the flow direction. The triple electrode was constructed by hybridizing a poly(1,2-diaminobenzene) film to two enzyme sensing-parts which respond to L-glutamate and acetylcholine, and by coating a Nafion film on a remaining sensing part which responds to dopamine, respectively, without any cross-reactivity. The three sensing parts of the triple electrode responded linearly to the concentrations of L-glutamate and acetylcholine in the range of 0.002-5 mM and to that of dopamine in the range of 0.002-20 mM, respectively, without any interference from oxidizable species present in the dialysate. The proposed flow-injection analytical method could be applied to an in vivo assay of these neurotransmitters released from rat-brain cells by the continuous KCl stimulation.

PMID: 18997377 [PubMed - indexed for MEDLINE]

Production and characterization of a monoclonal antibody to capture proteins tagged with lithocholic acid.

Anal Sci. 2008;24(11):1475-80.
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Production and characterization of a monoclonal antibody to capture proteins tagged with lithocholic acid.

Ikegawa S, Yamamoto T, Miyashita T, Okihara R, Ishiwata S, Sakai T, Chong RH, Maeda M, Hofmann AF, Mitamura K.

Faculty of Pharmaceutical Sciences, Kinki University, 3-4-1 Kowakae, Higashi-osaka 577-8502, Japan. ikegawa@phar.kindai.ac.jpReactive metabolic-modified proteins have been proposed to play an important role in the mechanism(s) of the hepatotoxicity and colon cancer of lithocholic acid (LCA). To identify cellular proteins chemically modified with LCA, we have generated a monoclonal antibody that recognizes the 3alpha-hydroxy-5beta-steroid moiety of LCA. The spleen cells from a BALB/c mouse, which was immunized with an immunogen in which the side chain of LCA was coupled to bovine serum albumin (BSA) via a succinic acid spacer, was fused with SP2/0 myeloma cells to generate antibody-secreting hybridoma clones. The resulting monoclonal antibody (gamma2b, kappa) was specific to LCA-N(alpha)-BOC-lysine as well as the amidated and nonamidated forms of LCA. The immunoblot enabled the detection of LCA residues anchored on BSA and lysozyme. The antibody will be useful for monitoring the generation, localization, and capture of proteins tagged with LCA, which may be the cause of LCA-induced toxicity.

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997378 [PubMed - indexed for MEDLINE]

Direct observation of dispersion and mixing processes in microfluidic systems

Anal Sci. 2008;24(11):1481-5.
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Direct observation of dispersion and mixing processes in microfluidic systems.

Takabayashi Y, Fujino T, Korenaga T.

Department of Chemistry, Graduate School of Science and Engineering, Tokyo Metropolitan University, 1-1 Minami-Ohsawa, Hachioji, Tokyo 192-0397, Japan.The diffusion phenomena, dispersion and mixing processes of the sample solute (Basic Blue 3 dye and KMnO4 aqueous solutions) were directly observed in laminar flow in glass microchannels. Quasi steady-state UV-visible absorption spectrometry was carried out using CCD camera images of the colored sample dispersion and mixing processes, and the absorbance change (DeltaAbs) was discussed based on the dimensionless parameter, tau which represents the flow time renormalized to the diffusion coefficient and the channel cross section. It was found that DeltaAbs showed almost the same tau dependence, even though the solutions and the microchannel sizes differed in laminar flow, if the microchannel fabrication method was the same. On the basis of this fundamental result, the total microchannel length required for the reaction of 2,3-diaminonaphthalene (DAN) and NO2- at a flow rate of 2 microL min(-1) was calculated, and the obtained value ( approximately 100 mm) showed very good agreement with our previous microchip research. It was concluded that both results were useful for designing the microchannel width, depth and length to control the chemical reaction time in recent microfluidic systems.

PMID: 18997379 [PubMed]

Direct observation of dispersion and mixing processes in microfluidic systems.

Anal Sci. 2008;24(11):1481-5.
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Direct observation of dispersion and mixing processes in microfluidic systems.

Takabayashi Y, Fujino T, Korenaga T.

Department of Chemistry, Graduate School of Science and Engineering, Tokyo Metropolitan University, 1-1 Minami-Ohsawa, Hachioji, Tokyo 192-0397, Japan.The diffusion phenomena, dispersion and mixing processes of the sample solute (Basic Blue 3 dye and KMnO4 aqueous solutions) were directly observed in laminar flow in glass microchannels. Quasi steady-state UV-visible absorption spectrometry was carried out using CCD camera images of the colored sample dispersion and mixing processes, and the absorbance change (DeltaAbs) was discussed based on the dimensionless parameter, tau which represents the flow time renormalized to the diffusion coefficient and the channel cross section. It was found that DeltaAbs showed almost the same tau dependence, even though the solutions and the microchannel sizes differed in laminar flow, if the microchannel fabrication method was the same. On the basis of this fundamental result, the total microchannel length required for the reaction of 2,3-diaminonaphthalene (DAN) and NO2- at a flow rate of 2 microL min(-1) was calculated, and the obtained value ( approximately 100 mm) showed very good agreement with our previous microchip research. It was concluded that both results were useful for designing the microchannel width, depth and length to control the chemical reaction time in recent microfluidic systems.

PMID: 18997379 [PubMed]

Simultaneous determination of Fe(III) and Fe(II) ions via complexation with salicylic acid and 1,10-phenanthroline in microcolumn ion chromatography.

Anal Sci. 2008;24(11):1487-92.
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Simultaneous determination of Fe(III) and Fe(II) ions via complexation with salicylic acid and 1,10-phenanthroline in microcolumn ion chromatography.

Oktavia B, Lim LW, Takeuchi T.

Department of Chemistry, Faculty of Engineering, Gifu University, 1-1 Yanagido, Gifu 501-1193, Japan.Fe(III) and Fe(II) ions were separated and determined via in-column and post-column reactions with salicylic acid and 1,10-phenanthroline by microcolumn ion chromatography with UV-Vis detection. The separation could be achieved on a silica microcolumn using an aqueous ethanol solution of salicylic acid as eluent. The effluent from the column was then mixed with aqueous ethanol solution of 1,10-phenanthroline and detected at 518 nm. Fe(III) ion was detected as the complex with salicylic acid, whereas Fe(II) ion was detected as the complex with 1,10-phenanthroline. The detection limits with 0.25 microL injection volume at S/N = 3 were 0.21 and 0.10 mg L(-1) for Fe(III) and Fe(II), respectively. Increasing the injection volume of sample, e.g., 5.1 microL, improved the sensitivity; the detection limits at S/N = 3 were 12 and 9.2 microg L(-1) for Fe(III) and Fe(II), respectively. The present system was applied to the determination of iron in a local well water sample.

Publication Types:
Evaluation Studies

PMID: 18997380 [PubMed - indexed for MEDLINE]

Ethyl chloroformate as a derivatizing reagent for the gas chromatographic determination of isoniazid and hydrazine in pharmaceutical preparations.

Anal Sci. 2008;24(11):1493-6.
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Ethyl chloroformate as a derivatizing reagent for the gas chromatographic determination of isoniazid and hydrazine in pharmaceutical preparations.

Khuhawar MY, Zardari LA.

Dr. M. A. Kazi Institute of Chemistry, University of Sindh Jamshoro, Pakistan. liaquat_zardari@yahoo.comEthyl chloroformate was examined as a precolumn derivatizing reagent for the gas chromatographic (GC) determination of isoniazid (INH) and hydrazine (HZ). Phenylhydrazine (PHZ) was used as an internal standard. GC separation was carried out on an HP-5 column (30 m x 0.32 mm i.d.) with flame ionization detection. The elution was carried out at an initial column temperature of 150 degrees C for 1 min at a heating rate of 10 degrees C/min up to 250 degrees C, nitrogen flow rate of 4 ml/min and a split ratio of 10:1, v/v. The linear calibration ranges for INH and HZ were observed between 3.5-37.5 and 3.5-35 microg/ml with corresponding detection limits of 0.18 and 0.17 ng reaching the detector. The method was subsequently applied to the determination of INH and HZ in pharmaceutical preparations, achieving a relative standard deviation (RSD) of 3.8-5.8%. The recovery percentage of INH from isoniazid syrup was 98% with an RSD of 5.2%.

Publication Types:
Evaluation Studies
Research Support, Non-U.S. Gov't

PMID: 18997381 [PubMed - indexed for MEDLINE]

Suppression of matrix-related ions using cyclodextrin in MALDI mass spectrometry.

Anal Sci. 2008;24(11):1497-500.
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Suppression of matrix-related ions using cyclodextrin in MALDI mass spectrometry.

Yamaguchi S, Fujita T, Fujino T, Korenaga T.

Department of Chemistry, Graduate School of Science and Engineering, Tokyo Metropolitan University, 1-1 Minami-Osawa, Hachioji, Tokyo 192-0397, Japan.An effective technique for the suppression of matrix-related ions in matrix-assisted laser desorption/ionization (MALDI) mass spectrometry have been developed. Using typical organic matrices such as THAP (2,4,6-trihydroxyacetophenone) and CHCA (alpha-cyano-4-hydroxycinnamic acid) in a cyclodextrin cavity, we successfully measured the mass peaks of only protonated matrix ions and significantly suppressed their intensities and fragmentation. In addition, it became possible to analyze the mass peak of the analyte molecules (substance P and adenosine) without any interference from the matrix. We believe that this technique could be a powerful tool for MALDI mass spectrometry, particularly for low-molecular-weight compounds.

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997382 [PubMed - indexed for MEDLINE]

Isotopic analysis of calcium in blood plasma and bone from mouse samples by multiple collector-ICP-mass spectrometry.

Anal Sci. 2008;24(11):1501-7.
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Isotopic analysis of calcium in blood plasma and bone from mouse samples by multiple collector-ICP-mass spectrometry.

Hirata T, Tanoshima M, Suga A, Tanaka YK, Nagata Y, Shinohara A, Chiba M.

Laboratory for Planetary Sciences, Tokyo Institute of Technology, 2-12-1 O-okayama, Meguro, Tokyo 152-8551, Japan. hrt1@geo.titech.ac.jpThe biological processing of Ca produces significant stable isotope fractionation. The level of isotopic fractionation can provide key information about the variation in dietary consumption or Ca metabolism. To investigate this, we measured the 43Ca/42Ca and 44Ca/42Ca ratios for bone and blood plasma samples collected from mice of various ages using multiple collector-ICP-mass spectrometry (MC-ICP-MS). The 44Ca/42Ca ratio in bones was significantly (0.44-0.84 per thousand) lower than the corresponding ratios in the diet, suggesting that Ca was isotopically fractionated during Ca metabolism for bone formation. The resulting 44Ca/42Ca ratios for blood plasma showed almost identical, or slightly higher, values (0.03-0.2 per thousand) than found in a corresponding diet. This indicates that a significant amount of Ca in the blood plasma was from dietary sources. Unlike that discovered for Fe, there were no significant differences in the measured 44Ca/42Ca ratios between female and male specimens (for either bone or blood plasma samples). Similarity, the 44Ca/42Ca ratios suggests that there were no significant differences in Ca dietary consumption or Ca metabolism between female and male specimens. In contrast, the 44Ca/42Ca ratios of blood plasma from mother mice during the lactation period were significantly higher than those for all other adult specimens. This suggests that Ca supplied to infants through lactation was isotopically lighter, and the preferential supply of isotopically lighter Ca resulted in isotopically heavier Ca in blood plasma of mother mice during the lactation period. The data obtained here clearly demonstrate that the Ca isotopic ratio has a potential to become a new tool for evaluating changes in dietary consumption, or Ca metabolism of animals.

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997383 [PubMed - indexed for MEDLINE]

Measurement of benzophenones in human urine samples by stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry.

Anal Sci. 2008;24(11):1509-12.
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Measurement of benzophenones in human urine samples by stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry.

Kawaguchi M, Ito R, Honda H, Endo N, Okanouchi N, Saito K, Seto Y, Nakazawa H.

Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences, Hoshi University, 2-4-41 Ebara, Shinagawa, Tokyo 142-8501, Japan.Determination of benzophenones (BPs) in human urine samples by stir bar sorptive extraction (SBSE) and thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS) is described. As analytes, BP, its metabolites benzhydrol (BP-OH) and 2-hydroxybenzophenone (2OH-BP), and its derivatives 2-hydroxy-4-methoxybenzophenone (BP-3) and 2-hydroxy-4-methoxy-4'-methylbenzophenone (BP-10) were selected. After enzymatic hydrolysis, a polydimethylsiloxane (PDMS) stir bar was placed in a urine sample diluted 1:1 with water and stirred for 60 min at room temperature. The limit of quantification (LOQ) of BPs is 0.2-0.5 ng ml(-1) (ppb). The method showed linearity over the calibration range (0.2-10 or 0.5-10 ng ml(-1)), and the correlation coefficients were equal to or higher than 0.993 for all of the analytes. The average recoveries of BPs were equal to or higher than 98.7% (RSD: 1.5-4.8%, n = 6).

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997384 [PubMed - indexed for MEDLINE]

Measurement of benzophenones in human urine samples by stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry.

Anal Sci. 2008;24(11):1509-12.
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Measurement of benzophenones in human urine samples by stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry.

Kawaguchi M, Ito R, Honda H, Endo N, Okanouchi N, Saito K, Seto Y, Nakazawa H.

Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences, Hoshi University, 2-4-41 Ebara, Shinagawa, Tokyo 142-8501, Japan.Determination of benzophenones (BPs) in human urine samples by stir bar sorptive extraction (SBSE) and thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS) is described. As analytes, BP, its metabolites benzhydrol (BP-OH) and 2-hydroxybenzophenone (2OH-BP), and its derivatives 2-hydroxy-4-methoxybenzophenone (BP-3) and 2-hydroxy-4-methoxy-4'-methylbenzophenone (BP-10) were selected. After enzymatic hydrolysis, a polydimethylsiloxane (PDMS) stir bar was placed in a urine sample diluted 1:1 with water and stirred for 60 min at room temperature. The limit of quantification (LOQ) of BPs is 0.2-0.5 ng ml(-1) (ppb). The method showed linearity over the calibration range (0.2-10 or 0.5-10 ng ml(-1)), and the correlation coefficients were equal to or higher than 0.993 for all of the analytes. The average recoveries of BPs were equal to or higher than 98.7% (RSD: 1.5-4.8%, n = 6).

Publication Types:
Research Support, Non-U.S. Gov't

PMID: 18997384 [PubMed - indexed for MEDLINE]

Determination of 56 elements in Lake Baikal water by high-resolution ICP-MS with the aid of a tandem preconcentration method.

Anal Sci. 2008;24(11):1513-7.
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Determination of 56 elements in Lake Baikal water by high-resolution ICP-MS with the aid of a tandem preconcentration method.

Rahmi D, Zhu Y, Umemura T, Haraguchi H, Itoh A, Chiba K.

Department of Applied Chemistry, Graduate School of Engineering, Nagoya University, Chikusa, Nagoya 464-8603, Japan.A tandem preconcentration method integrating chelating resin adsorption and La coprecipitation was applied to an analysis of Lake Baikal water by high-resolution ICP-MS. As a result, 56 elements were determined in Lake Baikal water: Ca, Na, Mg, K, Si, Sr, B, Li, Ba, P, Fe, Al, Mo, Zn, Mn, Rb, U, As, V, Cu, Pb, W, Y, Cs, Se, Cr, Ni, Ti, Sb, Zr, Sn, Co, Cd, Rh, Te, Hf, Nb, Ru, Ga, Sc, Th, Bi, and all-rare earth elements (all-REEs), except for Pm. The concentrations of these elements covered a range of nine orders of magnitude, from approximately 17 microg mL(-1) of Ca to less than 50 fg mL(-1) of Tm. The elemental concentrations in Lake Baikal water were compared with reference data.

PMID: 18997385 [PubMed]

Outcome of transanal irrigation for bowel dysfunction in patients with spinal cord injury.

J Spinal Cord Med. 2008;31(5):560-7.
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Outcome of transanal irrigation for bowel dysfunction in patients with spinal cord injury.

Christensen P, Bazzocchi G, Coggrave M, Abel R, Hulting C, Krogh K, Media S, Laurberg S.

Department of Surgery P, Aarhus University Hospital, Aarhus, Denmark. piz@webspeed.dkBACKGROUND/OBJECTIVE: To compare symptoms of neurogenic bowel dysfunction in patients with spinal cord injury (SCI) at baseline and after 10 weeks of treatment with transanal irrigation and to identify possible factors that could predict outcome of the treatment. METHODS: Sixty-two patients with SCI (45 men and 17 women; mean age, 47.5 +/- 15.5 [SD] years) from 5 specialized European SCI centers were offered treatment with transanal irrigation for a 10-week period. Bowel function was assessed at baseline and at termination using the Cleveland Clinic Constipation Scoring System (CCCSS; 0-30, 30 = severe symptoms), St. Mark's Fecal Incontinence Grading System (FIGS; 0-24, 24 = severe symptoms), and the Neurogenic Bowel Dysfunction score (NBD; 0-47, 47 severe symptoms). Factors predicting improvement in bowel function scores were identified using a general linear model. RESULTS: Severity of symptoms at termination was significantly reduced compared with baseline values (CCCSS: -3.4; 95% confidence interval [CI], -4.6 to -2.2; FIGS: - 4.1; 95% CI, -5.2 to -2.9; NBD: -4.5; 95% CI, -6.6 to -2.4; all P < 0.0001). Although several factors were associated with positive outcome, no consistent and readily explainable pattern could be identified. Surprisingly, hand function, level of dependency, predominant symptom, and colonic transit time were not associated with outcome. CONCLUSIONS: Transanal irrigation in patients with SCI reduces constipation, improves anal continence, and improves symptom-related quality of life. No readily obtainable factors could predict outcome, which might be because of the relatively low number of patients. This supports the use of trial and error as a strategy in deciding on a bowel management method for neurogenic bowel dysfunction.Publication Types:
Research Support, Non-U.S. Gov't

PMID: 19086714 [PubMed - in process]
PMCID: PMC2607129 [Available on 2009/04/01]

Pulsed magnetic field faraday imaging of diamagnetic liquids.

Anal Sci. 2009 Jan;25(1):1-3.
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Pulsed magnetic field faraday imaging of diamagnetic liquids.
Isai K, Suwa M, Watarai H.
Department of Chemistry, Graduate School of Science, Osaka University, Japan.The Faraday rotation of diamagnetic liquids has been measured by applying a pulsed magnetic field. The observed results for water, alcohol, and aliphatic and aromatic organic liquids suggested a possible discrimination of such liquids by Faraday imaging. Actually, we have succeeded to observe Faraday images using a magneto-optical microscope system. The discrimination of several diamagnetic liquids including chiral liquids has been demonstrated.PMID: 19139566 [PubMed]

Direct observation of multiple and stochastic transition states by a feedback-controlled single-molecule force measurement.

Anal Sci. 2009 Jan;25(1):5-7.
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Direct observation of multiple and stochastic transition states by a feedback-controlled single-molecule force measurement.
Fukagawa A, Hiroshima M, Sakane I, Tokunaga M.
Structural Biology Center, National Institute of Genetics, Mishima, Shizuoka 411-8540, Japan.To overcome the ensemble-averaging barrier, single-molecule experiments have been performed, but energy landscapes comprising multiple intermediates have not yet been defined. We performed mechanical unfolding of staphylococcal nuclease using intermolecular force microscopy, modified AFM with high resolution and feedback control of the positioning. The force dropped vertically just after its peak, and multiple transition states were detected as force peaks. The multiple and stochastic intermediates found in the present study provide new important information on protein folding.PMID: 19139567 [PubMed - indexed for MEDLINE]

Direct observation of multiple and stochastic transition states by a feedback-controlled single-molecule force measurement.

Anal Sci. 2009 Jan;25(1):5-7.
Related Articles,
Links
Direct observation of multiple and stochastic transition states by a feedback-controlled single-molecule force measurement.

Fukagawa A, Hiroshima M, Sakane I, Tokunaga M.

Structural Biology Center, National Institute of Genetics, Mishima, Shizuoka 411-8540, Japan.To overcome the ensemble-averaging barrier, single-molecule experiments have been performed, but energy landscapes comprising multiple intermediates have not yet been defined. We performed mechanical unfolding of staphylococcal nuclease using intermolecular force microscopy, modified AFM with high resolution and feedback control of the positioning. The force dropped vertically just after its peak, and multiple transition states were detected as force peaks. The multiple and stochastic intermediates found in the present study provide new important information on protein folding.PMID: 19139567 [PubMed - indexed for MEDLINE]

Analytical and separation chemistry by taking advantage of organic photochromism combined with macrocyclic chemistry.

Anal Sci. 2009 Jan;25(1):9-20.
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Analytical and separation chemistry by taking advantage of organic photochromism combined with macrocyclic chemistry.

Kimura K, Nakahara Y.

Department of Applied Chemistry, Faculty of Systems Engineering, Wakayama University, Japan. kkimura@sys.wakayama-u.ac.jpPhotochromic crown compounds, such as monomeric and polymeric crown compounds incorporating spirobenzopyran, spironaphthooxazine, spirobenzothiapyran, Malachite Green, and Crystal Violet moieties, were synthesized for applications in the fields of analytical and separation chemistry. The photochromic crown compounds, especially crowned spirobenzopyran derivatives, were applied to metal ion extraction, extraction spectrophotometry, membrane transport, and ion chromatography, the sensitivity and selectivity of which were controlled and enhanced photochemically. Also, micelles and vesicles containing lipophilic crowned spirobenzopyrans and Malachite Greens were tested for their usefulness in spectrophotometric and fluorometric metal-ion determination and photocontrol of organic substance in aqueous systems. The polymeric crowned spirobenzopyrans were tried to use as a photochemical valve based on photochemical rheology changes. Moreover, attempts were made to directly observe photoinduced aggregation of the spirobenzopyran moiety and photoresponsive rheology changes of the polymeric crowned spirobenzopyran, by using chemical force microscopy.Publication Types:
ReviewPMID: 19139568 [PubMed - indexed for MEDLINE]

Analytical studies on the development of high-performance liquid chromatographic methods with fluorescence or chemiluminescence detections and their p

Anal Sci. 2009 Jan;25(1):21-31.
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Analytical studies on the development of high-performance liquid chromatographic methods with fluorescence or chemiluminescence detections and their practical applications.

Nakashima K, Ikeda R, Wada M.

Department of Clinical Pharmacy, Graduate School of Biomedical Sciences, Nagasaki University, Japan. naka-ken@nagasaki-u.ac.jpThis review describes a comprehensive investigation focusing on syntheses of analytical reagents, followed by their utilization in development of analytical methods, and leading to practical applications for rational use of medicaments centering on abused drugs. Many kinds of analytical reagents for fluorescence and chemiluminescence detections have been synthesized with the intention of improving sensitivity. By properly combining the developed analytical reagents with an HPLC separation technique, one could determine ultra-small amounts of abused drugs such as stimulants, narcotics and obesity drugs in various matrices. Furthermore, chiral analyses of some abused drugs and evaluation of their potential for drug-drug interaction were also performed. The developed methods might be useful for forensic and toxicological studies on drug abuse. Also, the results obtained in our study might contribute to the prediction of and the protection of human health from risks of abused drugs.Publication Types:
Research Support, Non-U.S. Gov't
ReviewPMID: 19139569 [PubMed - indexed for MEDLINE]