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Biomedical subjects

C T Kenner

Publications and source records attributed to C T Kenner.

At least 19 recordsLinked to original sources

Separation and determination of testosterone and testosterone esters in selected pharmaceutical formulations.

A rapid quantitative procedure is presented for the separation of testosterone esters from their hydrolysis products through the use of the acetonitrile-infusorial earth column. The method was applied to testosterone cypionate, testosterone enanthate, and testosterone propionate. Recovery and replication of reference standard testosterone and its three esters through the proposed method ranged from 99.1 to 100.3%, and the percent relative standard deviation ranged from 0.6 to 1.0%. Two samples can be separated into testosterone and testosterone ester fractions in about 1.5 hr. The analyses of 20 injectable and one buccal tablet formulations made by 12 different manufacturers are reported.

Drug Stability↗

High pressure liquid chromatographic determination of polynuclear aromatic hydrocarbons in oysters.

A high pressure liquid chromatographic (HPLC) procedure is described for determining 13 polynuclear aromatic hydrocarbon (PNA) compounds in oysters at the 2 ppb level. These compounds are extracted from shellfish with acetonitrile and partitioned into petroleum ether; the petroleum ether is removed and the residue is saponified. The aromatic compounds are isolated by passing the saponifeid residue through silica gel and further purified and fractionated by muStyragel gel permeation chromatography. The in-ividual PNAs are then quantitatively determined by using a reverse phase HPLC column coupled to fluorescence, spectrophotometric, and 254 nm absorbance detectors in series. Recoveries from spiked samples generally were greater than 80%.

Animals↗

Analysis of betamethasone and its organic esters in pharmaceutical products.

A rapid, quantitative analysis for betamethasone and its organic esters at room temperature is described. The method is similar to the official blue tetrazolium reaction for corticosteroids, except that methylene chloride is used as the solvent. The reaction is complete in 27-69 min, and the formazans produced are stable for at least 90 min after the addition of tetramethylammonium hydroxide. The results of the analysis of 13 different pharmaceutical formulations by the proposed method are reported. The degradation of betamethasone and its esters caused by strong bases is a pseudo-first-order reaction in methylene chloride. The average half-life of the corticosteroids studied is 56 min under the basic conditions described.

Aerosols↗

Rapid blue tetrazolium procedure for analysis of corticosteroids in pharmaceutical preparations.

A rapid quantitative analysis of nine selected corticosteroids and corticosteroid esters at room temperature is described. The procedure is similar to the official blue tetrazolium reaction for corticosteroids, except that methylene chloride instead of alcohol USP is used as a solvent and the reagents are dissolved in or diluted with nonaqueous solvents. These two modifications reduce the medium polarity, which increases the reaction rate. The reactions are complete in 7-18 min, and the formazans are stable for at least 90 min. The results from 15 different pharmaceutical formulations, 12 containing hydrocortisone and three containing prednisolone acetate, show that the proposed method gives results that compare favorably with those obtained by the official blue tetrazolium, isoniazid, and phenylhydrazine procedures.

Gels↗

Kinetic and mechanistic studies of blue tetrazolium reaction with phenylhydrazines.

The reaction kinetics of blue tetrazolium with selected arylhydrazines were investigated under pseudo-first-order conditions. The reaction rate constants were obtained at various temperatures, and the enthalpy (8.4-11.2 kcal/mole) and entropy (-38--45 eu) of activations were calculated. A Hammett plot yielded a straight line with a slope of 0.52. The reaction was inhibited by atmospheric oxygen and iodine. A free radical mechanism is presented.

Chemical Phenomena↗

Gas-liquid chromatographic determination of chlordene epoxide in catfish.

Chlordene epoxide was detected in the range of 0.04 to 0.27 ppm in the edible portion of 3 catfish samples during the analysis of 36 fish samples by electron capture gas-liquid chromatography (GLC) for pesticide and industrial chemical residues. Two of these catfish samples were from suppliers in Louisiana and the third was from a Texas supplier. Chlordene was also present; the amount of chlordene epoxide in the 3 samples averaged 46% of the amount of chlordene present. The epoxide was identified by comparison of the mass spectra and the GLC retention times of the samples with reference material prepared in the laboratory.

Animals↗

Kinetics and mechanism of blue tetrazolium reaction with corticosteroids.

The kinetics of the reaction of blue tetrazolium with corticosteroids were investigated under pseudo-first-order conditions. The reaction rates for various corticosteroids were determined at various temperatures, and the enthalpy and entropy of activation for these compounds were determined. A mechanism is proposed in which an electron pair and a proton are transferred to blue tetrazolium from the anion formed by the action of tetramethylammonium hydroxide on the alpha-carbonyl moiety of the corticosteroid. The proposed mechanism is consistent with previous experimental results.

Adrenal Cortex Hormones↗

Effect of solvent on tetrazolium reaction.

The rate of color development of a tetrazolium formazan is shown to be inversely proportional to the dielectric constant of the solvent medium and directly proportional to the hydrogen-bonding capability of solvent mixtures having the same dielectric constant. The geometric isomers of the formazans have different absorbance maxima, and the wavelength of maximum absorbance of a mixture of formazans in different solvents depends upon which isomer predominates in that solvent. The trans-syn-isomer (blue form) of blue tetrazolium has a maximum absorbance at 625 nm in dimethylformamide while the trans-anti-isomer (red form) absorbs at 517 nm in methanol. The absorbance maxima of the corresponding isomers of the formazans of triphenyltetrazolium occur at 535 and 485 nm, respectively. Water and/or methanol (to a lesser extent) are important in the stabilization of the trans-anti-isomer, since the small size of these two substances allows them to form strong intermolecular hydrogen bonds with one or both nitrogen atoms of the azo linkage, thereby preventing the formation of the intramolecular hydrogen bonding exhibited by the trans-syn-isomer. The formazan produced by the reaction of corticosteroids with tetrazolium in strongly basic media can lose a reduction unit and be reoxidized to the tetrazolium. This reaction is solvent dependent and occurs at a much faster rate in chloroform than in alcohol USP.

Adrenal Cortex Hormones↗

High-pressure liquid chromatography of benzo(a) pyrene and benzo (ghi) perylene in oil-contaminated shellfish.

A high-pressure liquid chromatographic procedure is described for the determination of benzo(a) pyrene and benzo(ghi) perylene. These polynuclear aromatics are extracted with acetonitrile and partitioned into petroleum ether, the petroleum ether is removed, and the residue is saponified. The compounds are purified and isolated by passing the residue through a silica gel column and a high-pressure liquid chromatographic column, and detected by their ultraviolet absorption. Recoveries of standards through the procedure averaged 104%.

Benzopyrenes↗

Reduction of blue tetrazolium by corticosteroids.

Pseudo-first-order rate constants were observed for the reaction of corticosteroid or corticosteroid esters with blue tetrazolium. The data indicate that the reactivity of corticosteroids is, in part, a function of their geometry in that corticosteroid reactivity toward blue tetrazolium increases with increasing planarity of the steroid molecule and that corticosteroid esters must be hydrolyzed as a necessary prerequisite to reaction with blue tetrazolium. Evidence is presented indicating that free radicals are not involved in the blue tetrazoliun reaction with corticosteroids. Certain pharmaceutically important compounds such as pyrocatechol derivatives and hydroquinone appear to reduce blue tetrazolium by the anion free radical mechanism proposed previously. A spectrophotometric method for determining the number of reduction units transferred to blue tetrazolium per molecule is described.

Adrenal Cortex Hormones↗

Determination of iodochlorhydroxyquin and corticosteroids in pharmaceutical formulations.

Iodochlorhydroxyquin was separated from various corticosteroids using an acetonitrile-diatomaceous earth column. Iodochlorhydroxyquin was eluted with cyclohexane, and the corticosteroid was eluted with chloroform. Iodochlorhydroxyquin was determined by both a UV absorbance method and a new compleximetric method using the nickel chelate of iodochlorhydroxyquin. The corticosteroid was determined by the blue tetrazolium and isoniazid procedures. The average percent recovery for these four methods was 100.8, 99.4,100.7, and 99.9, respectively, for 10 known mixtures. The standard deviation for the absorbance for 10 determinations of the nickel complex was 0.002 absorbance unit (0.31%). Various characteristics of the nickel and other complexes were evaluated, including the sensitivity, solubility, and wavelength of maximum absorbance in 14 different solvents. The analyses of 23 typical products are reported, for which the standard deviation, expressed as a percentage of the amount declared, was 1.31% for the UV, 1.34% for the compleximetric, 1.49% for the blue tetrazolium, and 1.22% for the isoniazid procedures. Methods of determination in the presence of interferences are discussed.

Administration, Topical↗