A Simple Spectrophotometric Method for the Determination of Adrenaline by Reaction with Copper(II)-Neocuproine

Abstract

A new facile and sensitive spectrophotometric procedure for the quantitative determination of adrenaline has been established. The method is based principally on the interaction of the compound with Cu(II)-neocuproine and subsequent measurement of the cuprous neocuproine chelate produced in the reaction at 458 nm. Optimization of the reaction conditions was conducted. Beer's law was obeyed in the concentration range 0.4-2.4 ppm of adrenaline. The method finally developed has been successfully applied for the assay of the drug in some of its pharmaceutical formulations.     

Flow Injection Analysis of Glucose by Fiber Optic Chemiluminescence Measurement

Abstract

A flow injection system was developed for the determination of glucose based on fiber optic chemiluminescence measurements. The hydrogen peroxide produced from the glucose oxidase catalyzed reaction was quantified by measuring the intensity of luminol chemiluminescence in the presence of excess ferricyanide. Glucose oxidase was immobilized on aminopropyl glass using glutaraldehyde and packed in a reactor. The chemiluminescence was transported to the detector using an optical fiber. The system responds linearly to glucose in the concentration range 0.20 mM up to 2.5 mM, with a relative precision of 5%. Several fruit juices were analyzed for their glucose content and the results were compared with a standard AOAC procedure.     

Spectrophotometric Determination of Nitrite in Wastewater with 4,5-Dihydroxycoumarin

Abstract

A rapid and simple spectrophotometric method was developed for the determination of nitrite in wastewater. The procedure was based on the extraction of nitrite with ethyl acetate solution of 4,5-dihydroxycoumarin. Beer's law obeyed up to 0.75 ppm of nitrite-nitrogen. Results obtained by using the proposed method on waste-water samples agreed well with those obtained by the diazotising-coupling method.     

Detection of Oxidase Generated Hydrogenperoxide by a Solid State Peroxyoxalate Chemiluminescence Detector

Abstract

The compatability of a solid state peroxyoxalate chemiluminescence detector for hydrogen peroxide with an immobilized oxidase reactor is investigated. As a model system glucose oxidase immobilized by electrostatic forces on an ion-exchanger or chemically bonded to glass beads were chosen. The former support is less suitable for immobilization of oxydases due to strong retention of hydrogenperoxide on the ion exchanger.

The relatively little flow dependence of these systems renders them suitable for low-cost manual sample injection monitors as well as in a flow injection analyses (FIA) mode with low-cost pumping systems. The system was operated with 80% acetonitrile water solutions. A detection limit of 8 × 10^?7M of glucose was achieved in directly injected samples.

Enzymes more sensitive to organic solvents can be operated with pure water and adjustment for optimal chemiluminescence condition is achieved with a make-up flow prior to detection. A detection limit of 5 × 10^?8M glucose is achieved under these conditions. The feasability of this approach to other oxidase based monitors and to detection in liquid chromatography is discussed.     

Flow Injection Analysis of Glucose in Human Serum by Chemiluminescence

Abstract

Combining the rigidly controlable conditions of Flow Injection Analysis with detection by chemiluminescence, a method for determination of glucose in serum via enzymatic degradation by glucose in serum via enzymatic degradation by glucose oxidase is described. With a Standard deviation of less than 2% the sampling frequency is 75 samples per hour. Results obtained by the proposed procedure are compared with those acquired by a routine AutoAnalyzer method used at a local hospital. It is shown that any influence on the yield of chemiluminescence due to difference in viscosity of the injected samples effectively can be eliminated.     

Determination of Paracetamol by a Flow Injection-Spectrophotometric Method

Abstract

A flow injection-spectrophotometric determination of paracetamol is reported. The procedure is based on the oxidation of the analyte with potassium hexacyanoferrate (III) and reaction of the N-(hydroxyphenyl)-p-benzoquinonimine produced with phenol; both reactions are carried out at 80 × 1°C and in aqueous ammoniacal solution. Concentrations of paracetamol in 0.25-30 ppm range are determined; relative standard deviations are 0.4% (n=40).Injection rate 26 samples/h.The influence of foreign species and the determination of paracetamol in several pharmaceutical formulations are also reported.     

Colorimetric Determination of Terbutaline and Orciprenaline Through Nitration and Subsequent Treatment with Acetyl Acetone in Alkaline Medium

Abstract

A colorimetric method is proposed for the determination of terbutaline sulphate, orciprenaline sulphate and their dosage forms. The procedure is based on the formation of trinitroderivatives of the drug which are subsequently subjected to a charge transfer complexation reaction with a donor, acetyl acetone. Concentration ranges adhering to Beer's Law are 4–32 μg/ml for both. The proposed method has been applied to pharmaceutical preparations and has proven to be accurate and precise.     

Flow-Injection Determination of Glucose by a Photoinduced Chemiluminescent Reaction

Abstract

A flow-injection procedure for the photochemical determination of glucose has been developed. The method is based on the photo-oxidation of glucose sensitized by 9,10-anthraquinone-2.6-disulfonate (disodium salt). The hydrogen peroxide formed in the photochemical reaction was measured by means of the chemiluminescent reaction with luminol and hematin. A linear calibration graph was obtained over the range 2.0x10^?6-8.5 x 10^?5 mol L^?1. The method was applied to determining glucose in blood serum, urine and fruit juices.     

Spectrophotometric Determination of Quintomycin Sulphate with Phloroglucinol

Abstract

A new absorptiometric procedure for the determination of quintomycin sulphate in complex galenical mixtures is proposed, based on the reaction of the sample compound with a mineral acid-containing phloroglucinol solution. Absorbance readings at 448 nm obey Lambert-Beer's law within the concentration range from 4. 0 to 32. 0 μg ml^?1. The method is operationally simple and has a good precision and an adequate selectivity.     

Utility of p-chloranilic Acid and 2,3 Dichloro-5,6-dicyano p-Benzoquinone (DDQ) for the Spectrophotometric Determination of Triamterene

Abstract

Two simple and sensitive spectrophotometric procedures are suggested for analysis of triamterene. The first procedure is based on the reaction of triamterene with p-chloranilic acid (p-CA) in methylene chloride to form a highly stable coloured product, exhibiting maximum absorbance at λ 530 nm. Beer's law is obeyed in the range of 40–220 μg.ml^?1 with a mean percentage accuracy of 99.98 ± 0.446. Limit of determination is 20 μg.ml^?1. In the second procedure, the drug is determined via charge transfer complex formation with 2,3 dichloro-5,6-dicyano p-benzoquinone (DDQ) using methylene chloride as a solvent. Here the reaction product has two well defined maxima at 460 nm and 530 nm where each has been utilized for quantitative determination. Beer's law is obeyed in concentration ranges of 25–125 μg.ml^?1 and 25–150 μg.ml^?1 with mean percentage accuracies of 99.92 ± 0.449 and 100.00 ± 0.511 for both maxima. 460 and 530 nm. respectively. Limit of determination is 12.5 μg.ml^?1 at both maxima. Optimum conditions for each procedure have been studied and the stoichiometry of both reactions was ascertained using Job's method of continuous variation. The validity of the suggested procedures was assessed by applying the standard addition technique using the drug capsules. Both procedures are statistically analyzed as compared with BP method for analysis of triamterene (non aqueous titration) revealing good accuracy and precision as indicated by t and F tests.     

Kinetic Spectrophotometric Determination of Trace Amounts of Pyridine With 4,4′-Diaminostilbene-2,2 ′-Disulphonic Acid

Abstract

A kinetic method for the determination of traces of pyridine (40-400 ng.ml″1) is described, based on the Konig reaction with cyanogen bromide for ring-opening and using 4,4 ′-diarninostilbene-2,2′-disulphonic acid (amsonic acid) as the coupling agent. Some disadvantages of earlier Konig-based equilibrium methods are removed in the new procedure. Figures of merit of the method are given, interfering effects by several con-pounds are studied and a view on the mechanism of the process is derived.     

An Efficient and Simple Method for Diazotization-Thiocyanation of Aryl Amine using Cross-Linked Poly (4-Vinylpyridine) Supported Thiocyanate Ion

Abstract

An efficient and simple method for the facile synthesis of arylthiocyanates via diazotization-thiocyanation of aryl amines using cross-linked poly (4-vinylpyridine) supported thiocyanate ion is described. Various primary aromatic amines, with electron-withdrawing and electron-donating groups, were transformed into aryl thiocyanates in high to excellent yields in a short reaction time. The present procedure offers advantages such as short reaction time, simple reaction work-up, and the polymeric reagents can also be regenerated and reused for several times without significant loss of their activity.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

A Microdialysis Probe Coupled with A Miniaturized Thermal Glucose Sensor for In Vivo Monitoring

Abstract

A miniaturized thermal flow injection analysis biosensor has been coupled with a microdialysis probe for continuous subcutaneous glucose monitoring. Thermal biosensors are based on the principle of measuring the heat evolved during enzyme catalysed reactions. The system presented here consists of a miniaturized thermal biosensor with a small column containing coimmibolized glucose oxidase and catalase. The analysis buffer passes through the column at a flow rate of 60μL/min via an 1μL sample loop which is connected to a microdialysis probe.

Invitro results showed constant permeability of the probe and stability of the biosensor response during 24 hours. The response time was 85 sec giving a sample rate of 42 samples/hour.

During a load experiment, the glucose profile in a healthy volunteer was followed both in the subcutaneous tissue and blood using the microdialysis set-up proposed and comparing to blood glucose analyser.     

Spectrophotometric Determination of Ampicillin with Some Nitro Compounds

Abstract

A spectrophotometric procedure for the determination of ampicillin (Amp.) in pure solutions and in its pharmaceutical preparations has been developed. This new method offers advantages of simplicity, rapidity and stability in comparison with the official BP (1980) method. The proposed method is based on the formation of a colour condensation product through the reaction of ampicillin and nitrobenzene derivatives in an alkaline aqueous-acetone medium 40% (v/v). Beer's law is obeyed in the range 0.5–28 μg ml^?1. The colours were produced within 20 min. after heating at 60±5°C and stable for at least 6 h. The method is relatively accurate (recovery 100±2%) and precise (RSD 1.9%) and can be used successfully for the preparation of capsules, syrup and ampoules.     

A Simple Analytical Method for Monitoring the Total Concentration of Heavy Metal Ions in Environmental Waters

Abstract

A non-sophisticated analytical procedure has been developed for monitoring the sum of heavy metal elements which form stronger EDTA complexes than manganese(II). It is based on complexation of the heavy metals with EDTA and a catalytic indication of its stoichiometry. The equivalence point is determined visually using the substitution reaction between Mn(II)-EDTA and heavy metal ions, followed by the Mn(II)-catalyzed oxidation of Acid Blue 45 dye with hydrogen peroxide. The method has a reasonable accuracy, uses simple test equipment and stable reagents, there are few interferences and it can be carried out by non-technical personnel. Neither preconcentration nor dilution of the sample is required and it is applicable to aqueous samples containing heavy metals down to ppm levels. Some applications to river and groundwaters are shown.     

Detection of Nanomole Quantities of Reducing Sugar by Liquid Chromatography

Abstract

The alkaline ferricyanide and the Park-Johnson's methods were studied in order to determine glucose oligomers separated by liquid chromatography in nanomole quantities. In the alkaline ferricyanide method, high sensitivity was obtained by measuring ultraviolet absorbance of the reduced reagents. The presence of some kinds of salts or alcohols did not affect the colour development of the reagents. The applicability of the present measuring system to an automatic sugar analyzer has been demonstrated by examining several glucose oligomers.     

Rapid Determination of Lactulose in Milk Using Seliwanoff's Reaction

ABSTRACT

A rapid method based on Seliwanoff's reaction to distinguish between UHT and sterilised milk was proposed. Lactulose was determined directly in milk with no treatment. Analysis of raw milk and its carbohydrates showed that the only interference was the relatively high concentration of lactose, which imposes the lower limit of detection. Small variations of lactulose (9mg dL^?) during heat treatment could be observed when the absorbance was measured against pretreated milk (blank). This method showed a linear range between 17–170mg dL^? and a detection limit lower than that of the official HPLC method. This novel procedure was compared with a commercially available enzymatic method and the results obtained correlated well.     

Use of an Aqueous Micellar Medium to Improve the Spectrophotometry Determination of Cyanide Ion with 5,5′-Dithiobis(2-Nitrobenzoic Acid)

Abstract

The spectrophotometric method for the determination of cyanide, which is based on the reaction of cyanide ion with 5,5′-dithiobis(2-nitrobenzoic acid) to displace the corresponding absorbing thiol anion, has been reinvestigated using an aqueous cetyltrimethylammonium bromide micellar reaction medium. The rate of the analytical reaction is increased considerably in the presence of the cationic surfactant. Thus, the time required for the spectrophotometric determination of cyanide ion in the 0.18 – 2.80 μg/ml range using this procedure is decreased from 25 minutes to 1 – 3 minutes.     

A Split-Flow Enzyme Thermistor

Abstract

The split-flow system is comprised of two identical micro-columns, one of which contains an immobilized enzyme preparation, the other an inert support material.

The heat produced in each column on introduction of a sample is measured with thermistors placed in these columns. The use of a reference column virtually eliminates the influence on the measurements of artifactual signals as unspecific heat, i.e., heat not produced by the enzymic reaction. The performance of the split-flow enzyme thermistor at a variety of pH's, ionic strengths or viscosities associated with the sample has been investigated and compared with previously described alternative enzyme thermistor arrangements. In this comparative study glucose at a concentration of 5 · 10^?4 M was used throughout. On passage through the imnobilized glucose oxidase preparation this solution gave rise to a heat change At of about 0.01°C. The insensitivity of the system described herein towards such variations makes it particularly suitable for the analysis of metabolities present in crude solutions such as urine and skim-milk.     

Amperometric Enzyme Biosensor Based on the Controlled Pore Glass

Abstract

A new amperometric biosensor based of glucose oxidase immobilized in aminopropyl-controlled pore glass (CPG) is reported. The glucose oxidase was linked to the CPG by covalent bonds with glutaraldehyde. The effect of analytical variables on the biosensor response was studied using experimental design methodology. Analytical properties such as linearity, detection limit, quantitation limit, range, and precision are reported. Interferences caused by compounds usually present in biological samples were eliminated.