Stereochemical effect in mass spectrometry .19. Determination of the optical purity of alpha-phenylethylamine by mass spectrometry

It is found that in the fast atom bombardment (FAB) mass spectra R-alpha-phenylethylamine and S-alpha-phenylethylamine can be clearly distinguished by S-1,1'-binaphthyl-2, 2'-diylhydrogenphosphate (S-BNP), Mixture of R-alpha-phenylethylamine and S-alpha-phenylethylamine also be tested and the relative abundance of the characteristic ion of mixture is related to the composition of the mixtute. We have therefore proposed a possible method to determine the optical purity of alpha-phenylethylamine.

The determination of ethylene-propylene copolymer-grafted-glycidyl methacrylate by the contact angle method

The contact angles theta of some liquids on ethylene-propylene copolymer-grafted-glycidyl methacrylate (EPM-g-GMA) were measured. The critical surface tensions r(c) of EPM-g-GMA were evaluated by the Zisman Plot (cos theta versus r(L)), Young-Dupre-Good-Girifalco plot (1 + cos theta versus 1/r(L)(0.5)) and log (1 + cos theta) versus log(r(L)) plot. The following results were obtained: the r(c) values varied significantly with the estimation methods. The critical surface tension r(c) decreased with the increase of the degree of grafting of EPM-g-GMA.

Determination of isoniazid and hydrazine by capillary electrophoresis with amperometric detection at a Pt-particle modified carbon fiber microelectrode

Capillary electrophoresis (CE)/electrochemical detection (EC) for the simultaneous determination of hydrazine and isoniazid has been developed. The electrochemical method uses a novel modified electrode dispersed with ultrafine platinum particles on the surface of a 30 mu m carbon fiber microelectrode. The unique characteristic of the Pt-particles modified carbon fiber microelectrode is its excellent stability. The current measurement for hydrazine is more sensitive than that of isoniazid. Selective determination of trace amount of free hydrazine in isoniazid and its formulation can be achieved at applied potential of 0.5 V.

The solution properties of phenolphthalein poly(arylether sulfone) .1. The solubility behavior and determination of M-II equations

A series of narrow molecular weight distribution fractions of phenolphthalein polyarylether sulfone(PES-C) had been prepared, The <(M) over bar (w)> of these fractions were determined by conventional light scattering method. The [eta] and the Huggins slope constant k' in DMF, CHCl3 and 1,2-dichloroethane were also determined. The Huggins constants are greater than 0.5 in all of these solvents showing a special solubility behavior. The Mark-Houwink equations of PES-C in these solvents at 25 degrees C are [eta] = 2.79 x 10(-2) <(M) over bar (0.615)(w)> (DMF); [eta] = 3.96 x 10(-2) <(M) over bar (0.58)(w)> (CHCl3); [eta] = 7.40 x 10(-2) <(M) over bar (0.52)(w)> (CH2ClCH2Cl).

DETERMINATION OF AMINOPYRINE AND ITS METABOLITE BY CAPILLARY ELECTROPHORESIS ELECTROCHEMICAL DETECTION

An electrochemical pretreatment regime for a cylindrical carbon fibre microelectrode was optimized for the determination of aminopyrine (AM) and its metabolite 4-aminoantipyrine (AAN) by capillary electrophoresis (CE)-electrochemical detection (ED). Under optimized conditions, a response of high sensitivity and stability was obtained for AM and AAN at a detection voltage as low as 0.9 V following CE-ED, by which AM and AAN were separated satisfactorily. The calibration graph was linear over three orders of magnitude and the limits of detection for AM and AAN were in the femtomole range.

STUDY ON ELECTROCATALYTIC OXIDATION OF NADH BY FERROCENE DERIVATIVES AND DETERMINATION OF CATALYTIC RATE-CONSTANT AT MICRODISK ELECTRODE

The electrocatalytic oxidation of NADH by ferrocene derivatives and the influence of complexation with beta-cyclodextrin (beta-CD) were investigated at a microdisk electrode in a buffer solution. The cyclic voltammetric behavior of the ferrocene derivatives on the microdisk electrode was used to determine the electron-transfer rate constant from NADH to the ferricinium species. The heterogeneous rate constants and the diffusion coefficient of ferrocene derivatives were determined with the microdisk electrode. The effect of temperature and pH on the electrocatalytic oxidation of NADH were assessed.

SIMULTANEOUS DETERMINATION OF GUANINE, URIC-ACID, HYPOXANTHINE AND XANTHINE IN HUMAN PLASMA BY REVERSED-PHASE HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY WITH AMPEROMETRIC DETECTION

A reversed-phase high-performance liquid chromatographic method with amperometric detection is described for the separation and quantification of uric acid, guanine, hypoxanthine and xanthine. The isocratic separation of a standard mixture of the compounds was achieved in 5 min on a Spherisorb 5 C-18 reversed-phase column, with a mobile phase of NaH2PO4 (300 mmol dm(-3) pH 3.0)-methanol-acetonitrile-tetrahydrofuran (97.8 + 0.5 + 1.5 + 0.2). Uric acid, guanine, hypoxanthine and xanthine were completely separated, with detection limits in the range 2-20 pmol per injection. The effect of pH and the composition of the mobile phase on the separation are described. The hydrodynamic voltammograms of these compounds were recorded at a glassy carbon electrode. The linear range of the calibration graph for each compound was: uric acid; 1-5000 mu mol dm(-3); guanine, 0.5-2000 mu mol dm(-3); hypoxanthine, 0.1-500 mu mol dm(-3) and xanthine, 0.5-5000 mu mol dm(-3). The within- and between-day precision was good. The uric acid and hypoxanthine content in human plasma was measured using the proposed method. Good recoveries of uric acid (97.9-103%), hypoxanthine (98.0-99.2%), guanine (96.0-98.3%) and xanthine (96.0-102%) were obtained from human plasma. The results of electrochemical detection were in good agreement with those of UV detection.

DETERMINATION OF CYSTEINE AND REDUCED GLUTATHIONE IN HUMAN PLASMA BY LIQUID-CHROMATOGRAPHY WITH PULSED AMPEROMETRIC ELECTROCHEMICAL DETECTION USING A PLATINUM-PARTICLES MODIFIED GLASSY-CARBON ELECTRODE

An assay procedure utilizing pulsed amperometric detection at a platinum-particles modified electrode has been developed for the determination of cysteine and glutathione in blood samples following preliminary separation by reversed-phase liquid chromatography. A chemically modified electrode (CME) constructed by unique electroreduction from a platinum-salt solution to produce dispersed Pt particles on a glassy carbon surface was demonstrated to catalyze the electo-oxidation of sulfhydryl-containing compounds: DL-cysteine (CYS), reduced glutathione (GSH). When used as the sensing electrode in flow-system pulsed-amperometric detection (PAD), electrode fouling could be avoided using a waveform in which the cathodic reactivation process occurred at a potential of - 1.0 V vs. Ag/AgCl to achieve a cathodic desorption of atomic sulfur. A superior detection limit for these free thiols was obtained at a Pt particle-based GC electrode compared with other methods; this novel dispersed Pt particles CME exhibited high electrocatalytic stability and activity when it was employed as an electrochemical detector in FIA and HPLC for the determination of those organo-sulfur compounds.

DETERMINATION OF AMINOPYRINE AND ITS METABOLITE IN BIOLOGICAL FLUID BY LIQUID-CHROMATOGRAPHY ELECTROCHEMISTRY WITH A GLASSY-CARBON ELECTRODE DISPERSED WITH ALPHA-ALUMINA PARTICLES

A sensitive high-performance liquid chromatographic method has been developed for the quantitative determination of aminopyrine (AM) and its metabolite 4-aminoantipyrine (AAN). The method utilizes reverse-phase chromatography/amperometric detection with a glassy carbon electrode dispersed with alpha-arumina particles as the working electrode, on which the oxidation of AM and AAN was greatly improved compared with that on a bare glassy carbon electrode. As a result, the detection limit was as low as 1.4 ng for AM and 0.8 ng for AAN, and the calibration plots for the above compounds have wide linear ranges from 100 ng/mL to 100 mu g/mL and 60 ng/mL to 80 mu g/mL (for AM and AAN, respectively). The above method was applied for the detection of these materials in human urine with satisfactory results.

COMPARISON OF THE CRACK-GROWTH METHOD AND THE CRACK STRESS WHITENING ZONE METHOD FOR THE FRACTURE-TOUGHNESS DETERMINATION OF PHENOLPHTHALEIN POLY(ETHER KETONE)

Fracture toughness values of phenolphthalein poly(ether ketone) (PEK-C) at 190 degrees C were determined by two different methods, i. e. the conventional crack growth method and the crack stress whitening zone method, which show consistent results. This indicates that the crack stress whitening zone method can be used to determine the crack initiation of some polymers for which the blunting line concept is unsuitable.

DETERMINATION OF HYDRAZINES BY CAPILLARY ZONE ELECTROPHORESIS WITH AMPEROMETRIC DETECTION AT A PLATINUM PARTICLE-MODIFIED CARBON-FIBER MICROELECTRODE

A novel modified electrode dispersed with ultrafine platinum particles on the surface of a 30-mu m carbon fibre microelectrode was investigated as an amperometric detector in capillary zone electrophoresis (CEEC) for determining hydrazines. The unique cha

DIRECT-INJECTION OF URINE AND DETERMINATION OF ACETAMINOPHEN BY MICELLAR LIQUID-CHROMATOGRAPHY WITH A WALL-JET CELL CARBON-FIBER MICROELECTRODE

A wall-jet cell/carbon fibre microelectrode detector was designed and used for the micellar liquid chromatographic assay of acetaminophen. The separations were carried out in an analytical column packed with C-18 stationary phase and the mobile phase was

HIGHLY SENSITIVE AND SELECTIVE DETERMINATION OF RIBOFLAVIN BY FLOW-INJECTION ANALYSIS USING PARALLEL DUAL-CYLINDER MICROELECTRODES

A novel wall-jet cell with parallel dual cylinder (PDC) microelectrodes was constructed and used for flow injection analysis (FLA). The detector takes the advantages of ''redox recycling'' between bipotentiostated microcylinder electrodes (- 0.4 V/SCE an

DETERMINATION OF THE VINYL-ACETATE CONTENT IN ETHYLENE-VINYL ACETATE COPOLYMERS BY THERMOGRAVIMETRIC ANALYSIS

The dependence of thermal degradation behaviour on vinyl acetate (VA) content of ethylene-vinyl acetate (EVA) copolymers was studied by thermogravimetric analysis (t.g.a.). Among the parameters investigated, the maximum rate of weight loss at the stage of

ELECTROCATALYTIC OXIDATION AND FLOW-INJECTION DETERMINATION OF REDUCED NICOTINAMIDE COENZYME AT A GLASSY-CARBON ELECTRODE MODIFIED BY A POLYMER THIN-FILM

G chemically modified electrode (CME) was prepared by electrochemical copolymerization of pyrrole and Methylene Blue. The resulting CME exhibits effective electrocatalytic activity towards the oxidation of reduced nicotinamide coenzymes (NADH and NADPH),