Derivative spectrophotometric determination of clotrimazole in single formulations and in combination with other drugs

First (D1) and second (D2) derivative spectrophotometric methods are presented for the determination of clotrimazole after its acid hydrolysis. Mixtures of clotrimazole with azidamfenicol and dexamethasone have been assayed using D2 measurement at 302 nm after acid hydrolysis for clotrimazole, D1 measurement at 288 nm for azidamfenicol, and D1 measurement at 436 nm after reaction with phenylhydrazinium sulfate for dexamethasone. Reproducible results with relative standard deviations of less than 2% are obtained. The proposed method has been successfully applied to the analysis of creams, topical solutions, and vaginal tablets.     

Atomic absorption spectrophotometric determination of mercury in mercury-containing drugs: collaborative study

An atomic absorption spectrophotometric (AAS) method applicable to a wide variety of mercury-containing drugs has been developed and subjected to a collaborative study. Samples were digested with a water-HCl-HNO3 (4 + 3 + 1) mixture, and the mercury was determined in solution by AAS. High levels of mercury were measured with a conventional air-acetylene flame, whereas low levels were measured by the flameless technique. Each of 7 collaborators received duplicate synthetic samples of a tincture, an ophthalmic solution, and an antiseptic solution, and duplicate commercial samples of an ointment and an injectable. The overall mean value found by collaborators for mercury in these samples was 100.13%. The corresponding overall repeatability SD (CV, %) and reproducibility SD (CV, %) values were 2.18 (2.18) and 3.38 (3.38), respectively. The proposed AAS method has been adopted official first action.     

Spectrophotometric determination of some catecholamine drugs using metaperiodate

A rapid spectrophotometric procedure for the determination of isoprenaline salts, levodopa, dopamine hydrochloride, and dobutamine hydrochloride, either in the drug substances or in pharmaceutical formulations, is described. The method is based on the development of orange, red, or violet products with sodium metaperiodate in an aqueous alcoholic medium. The reaction is suggested to proceed via oxidative cyclization of the catecholamine to form an aminochrome. The wavelengths of maximum absorption range from 465 to 520 nm. The structure of the cyclization product was confirmed by ultraviolet, infrared, and nuclear magnetic resonance spectroscopy and microanalysis data.     

Atomic absorption spectrophotometric determination of chromium in foods

A method is reported for determination of chromium in foodstuffs. Organic matter is digested with nitric acid, followed by oxidation to Cr(VI) and extraction with methyl isobutyl ketone (MIBK) after HCl addition. Chromium determinations are performed by flame absorption spectroscopy. Absence of interferences is verified and recovery tests are performed on food samples. Quantitation limit (3.8 ng/mL), accuracy (NBS Standard Reference Material 1,573 Tomato Leaves, 4,500 +/- 500 ng/g, found 3,860 +/- 409 ng/g), and precision (CV for vegetable matrix = 9.05%, CV for animal matrix = 14.95%) of the procedure are evaluated.     

First derivative spectrophotometric determination of anhydrotetracyclines in tetracyclines

A rapid method is presented for detection and determination of anhydrotetracycline-HCl (ATC-HCl) and 4-epianhydrotetracycline-HCl (4-EATC-HCl) in tetracycline-HCl (TC-HCl). The method determines the 2 compounds as a sum, not individually. The first derivative absorption curve has a trough (D1) at 460 nm which is linearly related to concentration (1-10 mg/mL). ATC-HCl + 4-EATC-HCl content was determined in TC-HCl powder and capsules by the D1 and the compensation D1 spectrophotometric methods. The results were compared with those obtained using U.S. Pharmacopeia and British Pharmacopoeia methods.     

Atomic absorption spectrophotometric determination of cobalt in foods

A method is described for the determination of cobalt in foods. After wet digestion, iron in the sample is removed by liquid-liquid extraction, and cobalt is isolated and extracted. Final determination is done by flame atomic absorption spectrophotometry. Analysis of NBS reference materials by this procedure gives results in close agreement with certified values. The limit of quantitation is 4.3 ng/mL. Recovery studies and analysis of standard materials show that this method is reliable.     

Ultraviolet spectrophotometric determination of hydralazine hydrochloride in tablets following derivatization with nitrite

Routine use of the USP XXI spectrophotometric method for the content uniformity determination of hydralazine hydrochloride tablets has shown that tablet excipients can significantly alter the spectral characteristics of the drug and thus cause inaccurate assay values to be obtained. Because of this problem, a simple and reliable alternative spectrophotometric assay method, based on the conversion of hydralazine to tetrazolo [5,1-alpha]phthalazine with nitrite ions under acidic conditions, was developed. The derivative showed an absorption maximum at about 274 nm and obeyed Beer's law over the concentration range 4-40 micrograms/mL. Mean recoveries of hydralazine hydrochloride added to commercial coated and uncoated tablets were 101.0% (n = 10) and 100.8% (n = 8), respectively. The proposed method was found suitable for the assay not only of individual tablets but also of tablet composites.     

Enzymatic determination of urea in milk by sequential injection with spectrophotometric and conductometric detection

In this work, an analytical system based on the coupling of gas diffusion separation and sequential injection analysis for urea determination in milk is presented. A versatile manifold that could simultaneously be used for either spectrophotometric or conductometric detection was constructed. The sample and urease solution are sequentially aspirated into the holding coil and sent to a thermoreactor, where urea is enzymatically hydrolyzed by urease and converted into ammonium. This stream merges an alkaline solution at a confluence point where ammonia is formed. Ammonia diffuses through a hydrophobic membrane and modifies the bromothymol blue indicator color, when spectrophotometric detection is used, or changes the conductance of a boric acid solution acceptor stream, when conductometric detection is used.This methodology was applied to the determination of urea in 18 milk samples and the results were statistically comparable with those furnished by the enzymatic recommended procedure. The detection limits were 2.6 x 10(-4) and 2.8 x 10(-5) mol L(-1) for conductometric and spectrophotometric detection, respectively. Repeatability (relative standard deviation, RSD) was better than 3.7% and 2.6% for conductometric and spectrophotometric detection, respectively.     

Simple spectrophotometric method for determination of phosphine residues in wheat

A method has been developed for determination of phosphine residues in wheat, based on the reaction of phosphine with silver nitrate in aqueous solution to form an egg-yellow chromophore with an absorption maximum at 400 nm. At this wavelength, there is a linear relationship between absorbance and concentration of phosphine in the range 10-100 ng/mL. Phosphine-fumigated wheat is soaked in a known volume of AgNO3 solution, and the absorbance of the filtrate is read against a blank at 400 nm. The method is sensitive, with lower detection and estimation limits of 0.008 and 0.01 micrograms PH3, respectively. Recovery of added phosphine from a closed system was 85-100%. Accuracy for this method has been compared with that for the gas chromatographic method.     

Ultraviolet spectrophotometric determination of benzoic acid in soy sauce.

Proteins and other interfering substances are precipitated from soy sauce, using sodium tungstate under acidic conditions. After centrifugation, the supernate is successively extracted with ethyl ether to isolate the benzoic acid in the organic solvent. The ethyl ether extract is washed with dilute HCl. Benzoic acid is then quantitatively determined by ultraviolet spectrophotometry. Recovery of sodium benzoate added to soy sauce ranged from 94 to 104%.     

UV spectrophotometric determination of piperine in pepper preparations: collaborative study

Eight collaborating laboratories performed replicate analyses for piperine on 5 samples representing pepper raw spice, oleoresins, and soluble seasonings. Piperine is extracted into ethylene dichloride and measured at maximal absorbance 342-345 nm with a UV light source. Piperine content is calculated using an absorbance factor derived from piperine. Intralaboratory coefficients of variation (CVo) ranged from 0.5 to 3.1%; interlaboratory coefficients of variation (CVx) ranged from 3.0 to 5.8%. The method has been adopted as an official method of the American Spice Trade Association and as an official first action method by AOAC.     

UV spectrophotometric determination of hydralazine hydrochloride in tablets: collaborative study

A UV spectrophotometric method for the determination of hydralazine hydrochloride in tablets was collaboratively studied by 5 laboratories. The method is based on conversion of hydralazine to a tetrazolo [5,1-alpha]phthalazine derivative which shows an absorption maximum at about 274 nm. Each collaborator received blind duplicate samples of 2 commercial powdered composites from 10 and 100 mg tablets, and 1 synthetic tablet formulation. Each collaborator also received a set of 10 tablets for determination of content uniformity. The pooled mean recovery of hydralazine hydrochloride from the synthetic formulation was 101.2 +/- 0.94%. The mean assay values for 10 and 100 mg tablets were 95.6 +/- 0.98 and 101.0 +/- 0.73% of the declared amounts, respectively, with corresponding CV values of 1.02 and 0.73%. The pooled mean for individual tablet assay was 99.8 +/- 3.26% of the declared value, with a CV of 3.29%. The method has been adopted official first action.     

Improved spectrophotometric determination of cyclopiazonic acid in poultry feed and corn

An improved visible spectrophotometric method has been developed for cyclopiazonic acid in poultry feed and corn. The method is based on the reaction of cyclopiazonic acid with Ehrlich reagent and detection at 580 nm. Reaction conditions were optimized with respect to reaction and measurement times and acid and Ehrlich reagent concentrations. Calibration curves were linear from 1 to 20 micrograms cyclopiazonic acid in 3 mL Ehrlich reagent, with a lower detection limit of 0.08 mg/kg for 50 g samples of poultry feed and corn. Recoveries from 50 g samples of poultry feed spiked with cyclopiazonic ranging from 0.16 to 1.20 mg/kg averaged 93.8%. Moldy corn and poultry feed samples analyzed by this method contained between 1 and 4 mg/kg cyclopiazonic acid.     

Atomic absorption spectrophotometric determination of liver copper: collaborative study

Eleven collaborating laboratories conducted replicate analyses on 4 blind duplicate pairs of bovine liver samples that either had naturally acquired copper levels or were spiked with one of 3 copper levels. A National Bureau of Standards Bovine Liver sample (SRM 1577, 193 +/- 10 mg copper/kg) and a 1000 mg copper/L standard were also submitted to the collaborators. The method requires the tissue to be digested with concentrated HNO3 at 60 degrees C, diluted to volume with water, and analyzed by atomic absorption spectrophotometry. The intralaboratory coefficients of variation (CVo) ranged from 5.6 to 19%; the interlaboratory CVx values ranged from 7.1 to 21%. The lower limit of detection was estimated to be 1 mg copper/kg tissue. The method has been adopted official first action.     

Spectrophotometric determination of some benzene sulfonamides with 7,7,8,8-tetracyanoquinodimethane

A new spectrophotometric method for the determination of some unsubstituted benzene sulfonamides is presented. The method is based on the interaction of these derivatives with 7,7,8,8-tetracyanoquinodimethane at pH 9.0-9.5 to produce intense blue products. The quantitation of the products was carried out at 578 nm. Beer's law was obeyed over a wide range of concentrations for all sulfonamide compounds studied. Optimum analytical conditions were determined, and the color produced was stable for at least 90 min at 25 degrees C. Analytical data for determination of sulfonamide compounds in pure form are presented together with application of the proposed method for analysis of some commercially available pharmaceutical preparations. The results are in good agreement with those obtained by official procedures.