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PubMed1992

Rapid determination of conditional partition constants in an FIA system.

This paper presents a simple and rapid method for the screening of substances for their conditional partition constants in the chloroform-water system. Samples are injected in either aqueous or organic solution into the corresponding phase. After equilibration in segmented flow the amount of sample remaining is measured photometrically. Performing the measurements at a series of phase volume ratios enables calculation of conditional partition constants knowing neither the amount injected nor the absorptivity of the substance under study. The time needed for a determination is about 15 min per substance, in many cases even shorter and the sample consumption is, in most cases, less than 1 mg. These characteristics make the method suitable for screening purposes. A series of compounds has been examined with this method, and acceptable results for the conditional partition constants were obtained in the range 0.2 less than D' less than 100 (-0.7 less than log D' less than 2.0).

Flow Injection Analysis↗
PubMed1993

On-line monitoring of urea in effluent liquid during haemodialysis.

An analytical system specially built for on-line urea monitoring is reported. Measurements are carried out in the effluent of a haemodialysis machine. The measuring system employs the dialyser inflow stream as a carrier solution channel in a continuous fashion. The analyser periodically samples the outflow stream of the dialyser by means of an automatic injection valve. The analyser features a bioreactor consisting of immobilized urease and a gas-diffusion module. It is through this module that the urea is converted to ammonia gas which is transferred to another carrier channel, this transports the ammonium ion to a tubular, all-solid-state, ion-sensitive electrode. A timer controls the transport, injection, the measuring and the recording subsystems. The analyser has been used during actual haemodialysis sessions. Urea clearances were also measured in batch, using conventional spectrophotometric clinical equipment. The correlation between both methodologies was sufficient to confirm the usefulness of the developed on-line analyser to monitor the optimal length of haemodialysis sessions.

Dialysis Solutions↗
PubMedDate not supplied

Copper carbonate as a solid-bed reactor for spectrophotometric determination of doxycycline and oxytetracycline in an unsegmented continuous flow assembly.

The FIA-spectrophotometric determination of doxycycline was carried out by reaction of the drug with cupric ions entrapped in a polymeric material in a packed-bed reactor: the complex formed was then injected into a manifold with an alkaline solution as carrier. The developed colour was monitored at 395.0 nm. The method was applied to the determination of doxycycline in different pharmaceutical formulations. The calibration graph for doxycycline hyclate was linear over the range 10.0-80.0 mg ml-1 (n = 8) with a relative standard deviation of 1.4% (at 25 mg ml-1) and a sample throughput of 128 h-1. The proposed procedure was also applied to the determination of oxytetracycline in pharmaceutical formulations.

Calibration↗
PubMed1993

Determination of drugs in biosamples at picomolar concentrations using competitive ELISA with electrochemical detection: application to steroids.

A competitive ELISA with electrochemical detection in a flow injection system (FIA) has been developed for determinations of the steroid drug budesonide in biological samples. Plasma samples were cleaned from interfering and cross-reacting compounds by two pretreatment steps consisting of a solid-phase extraction and a liquid chromatography fractionation. The enzyme label was alkaline phosphatase, which was used with p-aminophenyl phosphate (PAPP) as a substrate. The product, p-aminophenol, was detected electrochemically at a glassy carbon electrode at 250 mV (vs Ag/AgCl). The limited stability of both the substrate and the product influenced the performance of the method and had to be taken into account in the procedure by a normalization with time. Budesonide could be quantified in plasma samples down to 10 pM. The major sensitivity-limiting factor was the amperometric background response, probably due to spontaneous hydrolysis of PAPP to p-aminophenol.

Alkaline Phosphatase↗
PubMed1993

The study of the differential pulse voltammetric behaviour of ergot alkaloids and their determination by DC amperometric detection in a FIA system.

The ergot alkaloids possess strong pharmacological effects and are important drugs with widespread clinical uses. The ergot alkaloid preparations manufactured by Gedeon Richter Chemical Works Ltd have a very low active substance content (e.g. 1.0 mg in each Secadol (0.4 g) coated tablet); therefore a sensitive method of determination must be used. Because of this constraint the differential pulse voltammetric behaviour of ergot alkaloids was studied in respect of the effects of pH and composition of media and an automated FIA system with amperometric detection has been used to develop a selective and sensitive method for the routine quantitative assay of these alkaloids. A short summary is given of the experimental evidence to substantiate the stoichiometric equation proposed for the electrochemical oxidation of the lysergic acid type of ergot alkaloids, the mechanism may be generally applicable for compounds having the ergoloid skeleton. In the course of the work it was concluded that a simple DC amperometric method of detection in a FIA system could be applied to determine the content of ergot alkaloids of different pharmaceutical preparations. A suitable method designed to meet current analytical requirements has been developed and validated.

Autoanalysis↗
PubMed1994

Mechanized determination of n-octanol/water partition constants using liquid-liquid segmented flow extraction.

A simple and rapid method for the determination of partition constants in the n-octanol/water system is presented. The substance under study is dissolved in n-octanol or water, and injected into a stream of the corresponding phase. Liquid-liquid segmented flow is utilized for equilibration of the two phases and after equilibration a fraction of the aqueous phase is separated with the aid of a hydrophilic membrane. The amount of substance in the aqueous phase is measured spectrophotometrically. The measurements are repeated at a small number of different phase flow ratios and the results obtained are plotted against these ratios. From slope and intercept for the regression line through these points the conditional partition constant, D', can be calculated. A simplified procedure using only two measurements, one of which is obtained with the flow rate of organic phase set to 0, can also be used. Partition constants in the range 0.48 < D < 873 (-0.32 < log D < 2.94) have been determined using this system. The precision, measured as relative standard deviation (RSD) is below 15%, corresponding to a standard deviation of +/- 0.1 log unit or less over the range of measurement. Measured values correspond to literature values within 0.07 log units. The time needed for a determination is about 15 min per substance, in many cases even shorter and the sample consumption is, in most cases, less than 1 mg.

Flow Injection Analysis↗
PubMed1994

Flow-injection determination of Novalgin using amperometric detection at a glassy carbon electrode.

An electroanalytical study of the oxidation of Novalgin (dipyrone) at a glassy carbon electrode in aqueous solution has been carried out. A flow-injection method with amperometric detection based on this oxidation process is also described. The influence of flow rate, coil length and injection volume on the sensitivity of the method was established. The calibration graph was linear within the range 3 x 10(-6)-3 x 10(-5) M in an ammonia buffer solution (pH 9) as a potential of 0.4 V versus an Ag/AgCl reference electrode. The sampling rate was 54 samples h-1. The applicability of the method to the determination of Novalgin in pharmaceutical preparations was demonstrated by investigating the effect of potential sources of interference and by analysing commercial preparations.

Biosensing Techniques↗
PubMed1995

Flow-injection extraction-spectrophotometric determination of bromhexine with orange IV.

An automatic flow-injection photometric method for the determination of bromhexine is proposed. The drug was determined by formation of an ion-pair with orange IV, extraction into 1,2-dichloroethane and measurement of the absorbance at 412 nm of the organic phase. A linear calibration graph was obtained at concentrations of 5 x 10(-6)-1.6 x 10(-4) M of bromhexine. Up to 40 samples h-1 can be processed with an RSD of 0.32-0.88%. The method was applied to the determination of bromhexine in blood serum and a pharmaceutical preparation.

Azo Compounds↗
PubMed1995

Flow-injection spectrofluorimetric determination of flufenamic and mefenamic acid in pharmaceuticals.

Two sensitive and rapid flow-injection (FI) spectrofluorimetric methods are proposed for the determination of flufenamic acid (FF) and mefenamic acid (MF), based on the formation of complexes of these compounds with A1(III) in an ethanolic medium. The calibration graphs resulting from the measurements of the fluorescence at lambda exc = 351 nm and lambda em = 440 nm, and lambdaexc = 355 nm and lambda em = 454 nm for the complexes with FF and MF, respectively, are linear over the range 0.030-1.20 micrograms ml-1 for FF and 0.30-16.1 micrograms ml-1 for MF. The methods have been applied to the determination of these drugs in pharmaceutical preparations.

Administration, Topical↗
PubMed1996

Flow-injection spectrophotometric determination of adrenaline and dopamine with sodium hydroxide.

A new, rapid and economical flow-injection method for determining adrenaline and dopamine is proposed on the basis of the hydrolysis of these compounds in alkaline medium. The method was optimized by using a spectrophotometer operating at lambda = 390 nm as detector. Calibration graphs were linear up to 2 x 10(-4) M with quantification limits of 2.5 x 10(-6) M and 3.3 x 10(-6) M for dopamine and adrenaline respectively. Flow-injection allows the measurement of 130 samples per hour. The method was successfully applied for the determination of catecholamines in pharmaceuticals.

Chemistry, Pharmaceutical↗
PubMed1996

Chemiluminescent immunoenzyme biosensor with a thin-layer flow-through cell. Application for study of a real-time bimolecular antigen-antibody interaction.

A simple flow enzyme system for real-time continuous monitoring of interaction of biological molecules has been developed. It relies upon a thin-layer flow-through cell placed directly into the measuring compartment of the luminometer. One ligand (antibody) is immobilized on the inner surfaces of the flow cuvette, and a second ligand (antigen) labeled with a peroxidase molecule moves through the flow cell. The quantity of the complex on the surface of the cell may be monitored by measurement intensity of chemiluminescence in the reaction of peroxidase label with substrates (p-iodophenol, luminol and hydrogen peroxide). In such a way one can detect in a real-time regime the kinetics of association (or dissociation) of the complex labeled ligand-receptor on the surface of the cuvette. Due to the small thickness of the flow cell the diffusion limitations of interaction for two kinds of biomolecules (soluble and immobilized) are negligible, so the resulting intensity of chemiluminescent signal reflects the kinetics of interaction between soluble and immobilized components. The system may be successfully used for molecular recognition studies, analyzing the kinetics of bimolecular interaction and for concentration determination.

Antigen-Antibody Reactions↗
PubMed2005

Glucose sensing based on the intrinsic fluorescence of sol-gel immobilized yeast hexokinase.

In this study, we investigated measurements of the intrinsic fluorescence of yeast hexokinase as an assay for glucose and immobilization of the enzyme in a silica sol-gel matrix as a potential in vivo glucose sensor for use in patients with diabetes. The intrinsic fluorescence of hexokinase in solution (excitation=295 nm, emission=330 nm) decreased by 23% at a saturating glucose concentration of 1 mM (Kd=0.3 mM), but serum abolished the glucose-related fluorescence response. When entrapped in tetramethylorthosilicate-derived sol gel, hexokinase retained activity, with a 25% maximal glucose-related decrease in intrinsic fluorescence, and the saturation point was increased to 50 mM glucose (Kd=12.5 mM). The glucose response range was increased further (to 120 mM, Kd=57 mM) by a covering membrane of poly(2-hydroxyethyl) methacrylate. Unlike free enzyme, the fluorescence responses to glucose with sol-gel immobilized hexokinase, with or without covering membrane, were similar for buffer and serum. We conclude that fluorescence monitoring of sol-gel entrapped yeast hexokinase is a suitable system for development as an in vivo glucose biosensor.

Biosensing Techniques↗
PubMed2006

Multicommutated flow-through optosensors implemented with photochemically induced fluorescence: determination of flufenamic acid.

This article describes a multicommutated flow injection-solid phase spectroscopy system implemented with photochemically induced fluorescence for the determination of flufenamic acid (FFA). A strongly fluorescent photoproduct is generated when FFA is irradiated online under UV light in a strong sulfuric medium. The photoproduct generated is retained on C(18) silica gel (which fills the detection area of the flow cell) and directly monitored on the active solid support at 258/442 nm (lambda(ex)/lambda(em)). After maximum signal recording, the sensing zone is regenerated by eluting the retained photoproduct with an appropriate H(2)SO(4)/MeOH solution. The sensor, completely automated, is based on the use of three-way solenoid valves conveniently operated by a homemade multicommutation software written in Java language. The system is calibrated at 10 and 60s for sampling time, showing detection limits of 1.28 x 10(-9) and 5.33 x 10(-10) molL(-1) and sampling rates of 38 and 28 h(-1), respectively, with relative standard deviations of 0.9 and 1.2%. The applicability of the method is demonstrated for the determination of FFA in human serum, human urine, and a pharmaceutical preparation without any pre-treatment. Good recovery levels were achieved between 90.5 and 103.7%.

Anti-Inflammatory Agents↗
PubMed2004

The reaction of indole with the aminoacrylate intermediate of Salmonella typhimurium tryptophan synthase: observation of a primary kinetic isotope effect with 3-[(2)H]indole.

The bacterial tryptophan synthase alpha(2)beta(2) complex catalyzes the final reactions in the biosynthesis of L-tryptophan. Indole is produced at the active site of the alpha-subunit and is transferred through a 25-30 A tunnel to the beta-active site, where it reacts with an aminoacrylate intermediate. Lane and Kirschner proposed a two-step nucleophilic addition-tautomerization mechanism for the reaction of indole with the aminoacrylate intermediate, based on the absence of an observed kinetic isotope effect (KIE) when 3-[(2)H]indole reacts with the aminoacrylate intermediate. We have now observed a KIE of 1.4-2.0 in the reaction of 3-[(2)H]indole with the aminoacrylate intermediate in the presence of monovalent cations, but not when an alpha-subunit ligand, disodium alpha-glycerophosphate (Na(2)GP), is present. Rapid-scanning stopped flow kinetic studies were performed of the reaction of indole and 3-[(2)H]indole with tryptophan synthase preincubated with L-serine, following the decay of the aminoacrylate intermediate at 350 nm, the formation of the quinonoid intermediate at 476 nm, and the formation of the L-Trp external aldimine at 423 nm. The addition of Na(2)GP dramatically slows the rate of reaction of indole with the alpha-aminoacrylate intermediate. A primary KIE is not observed in the reaction of 3-[(2)H]indole with the aminoacrylate complex of tryptophan synthase in the presence of Na(2)GP, suggesting binding of indole with tryptophan synthase is rate limiting under these conditions. The reaction of 2-methylindole does not show a KIE, either in the presence of Na(+) or Na(2)GP. These results support the previously proposed mechanism for the beta-reaction of tryptophan synthase, but suggest that the rate limiting step in quinonoid intermediate formation from indole and the aminoacrylate intermediate is deprotonation.

Acrylates↗
PubMed2006

Effect of alcohols on binding of camphor to cytochrome P450cam: spectroscopic and stopped flow transient kinetic studies.

Addition of alcohols to cytochrome P450cam (CYP101) was shown to release the substrate camphor from the heme pocket of the enzyme. The release of the substrate was found to be caused both due to increased solubility of the substrate in solution in presence of alcohol and due to change in the tertiary structure of the active site of the enzyme. The far-UV CD and near-UV CD spectra reveal that addition of alcohols to cytochrome P450cam cause a small change in the secondary structural elements but a significant change in the tertiary structural organization of this enzyme. The CD spectra at the heme region at various concentrations of alcohols indicate a substantial change in the tertiary structural organization around the heme moiety too. The equilibrium constant associated with the binding of camphor to Cyt P450cam is strongly dependent on the concentration of alcohols and the corresponding free energy associated with the binding is found to scale linearly with the concentration of alcohols. Kinetic experiments on binding of camphor to Cyt P450cam show that both k(on) and k(off) rate constants are strongly affected by addition of alcohols suggesting that alcohol expel camphor out of the heme cavity of Cyt P450cam by affecting tertiary structure of Cyt P450cam as well as by modifying the solubility properties of camphor in aqueous medium.

Alcohols↗
PubMed2003

Direct conversion of ferrous myeloperoxidase to compound II by hydrogen peroxide: an anaerobic stopped-flow study.

Myeloperoxidase (MPO) is one of the essential components of the antimicrobial systems of polymorphonuclear neutrophils. It is unique in having a globin-like standard reduction potential of the ferric/ferrous couple. Here, it is shown that ferrous MPO heterolytically cleaves hydrogen peroxide forming water and oxyferryl MPO (compound II). The two-electron oxidation reaction follows second-order kinetics with the apparent bimolecular rate constant being (6.8+/-0.6)x10(4)M(-1)s(-1) at pH 7.0. After depletion of (micromolar) H(2)O(2) compound II slowly decays to ferric MPO, whereas upon addition of millimolar H(2)O(2) to ferrous MPO, compound III (oxyperoxidase) is formed in a sequence of two reactions involving compound II formation and its direct reaction with H(2)O(2), which also follows second-order kinetics [(78+/-2)M(-1)s(-1) at pH 7.0]. It is discussed how these reactions contribute to the interconversion of compound II and compound III and could explain the catalase activity of MPO.

Anaerobiosis↗