Determination of ethchlorvynol in body tissues and fluids after embalmment.

A 54 year-old female expired at her residence. Her husband, a physician, signed a certificate stating that her death was due to cerebrovascular accident (CVA) and released her body to a funeral home, where she was embalmed. Since the deceased had a long history of medical problems and drug abuse, an autopsy was performed and no evidence of CVA was found. Toxicological analyses of body fluids and tissues revealed the presence of ethchlorvynol in high concentration in the bile (112 mg/l). The bloody fluid collected from the heart contained a concentration of ethchlorvynol below the limit for quantitation. Other findings included phenobarbital (32.8 mg/l) in heart bloody fluid and methanol (an ingredient of embalming fluid). The significance of the findings is discussed in relation to embalmment prior to autopsy and toxicological analyses. Ethchlorvynol concentration in the bile is compared to other fatal cases due to ethchlorvynol overdose.

Titrimetric determination of acetylenic hyponotics using organic brominating agents.

A titrimetric method is described for the determination of three acetylenic hypnotics, namely ethchlorvynol, ethinamate, and methylpentynol carbamate, in bulk and in dosage forms. The method involves the use of either 1,3-dibromo-5,5-dimethylhydantoin (DBH), N-bromosuccinimide (NBS) or N-bromophthalimide (NBP) as titrants. A known excess volume of the reagent is added and, after the specified time, the residual reagent is determined iodometrically. This procedure permits semimicro determination (1-15 mg) of the drug. The procedure has been successfully applied to pharmaceutical dosage forms; the results agree well with those given by compendial methods. The stoichiometry of the reaction has been assessed and an explanation of the reaction pathway is presented.

Titrimetric and spectrophotometric determination of acetylenic hypnotics, using brominating agents.

Titrimetric and spectrophotometric titration methods are described for the quantitative determination of acetylenic hypnotics ethchlorvynol, ethinamate, and meparfynol carbamate as pure substances and in dosage forms. The methods involve the use of different brominating agents. A known excess of the reagent is added and, after the specified time, the residual reagent is determined iodometrically. These procedures permit semimicro determination (1-20 mg) of the drug. Recoveries ranged from 98.48 +/- 0.76 to 102.74 +/- 2.60%. The procedures have been successfully applied to pharmaceutical dosage forms; the results agree well with those for compendial methods.

Analysis of ethchlorvynol (Placidyl): evaluation of a comparison performed in a clinical laboratory.

Common techniques for analyzing ethchlorvynol (Placidyl) by colorimetry and gas liquid chromatography are evaluated. Matrix effects are thoroughly examined to determine their contribution to the validity of results.

Quantitative analysis of ethchlorvynol in a capsule dosage form by NMR spectroscopy.

A quantitative 1H-NMR procedure is described for measuring ethchlorvynol in capsules. Deuterochloroform is used as the solvent, and hexamethylenetetramine as the internal standard; the analysis is based on the comparison of the area of the AB peak system of ethchlorvynol with the area of the hexamethylenetetramine singlet. The 1H-NMR method yields results that are precise to within 1% and agree well with results of the more cumbersome and less specific USP titrimetric procedure.

The general toxicology unknown. I. The systematic approach.

The general toxicology unknown often presents challenges and interests to toxicologists. A systematic analytical approach to search for drugs or poisons is presented here. The preliminary screening analyses were as follows: alcohol by gas chromatography (GC), ethchlorvynol colorimetric analysis, enzyme multiplied immunoassay technique (EMIT), basic drug screening by GC, and neutral and weakly acidic drug screening by GC. Other additional analyses were performed depending on the special circumstance of each individual case and the results of these preliminary analyses. Positive findings were confirmed by computerized gas chromatography/mass spectrometry when practical. Quantitation was performed by GC whenever possible.

A comparative study of ethchlorvynol levels in blood versus bone marrow.

Bone marrow may be utilized as an alternative biological sample in cases where uncontaminated blood samples are not available for analyses. Bone marrow/blood ratios of ethchlorvynol as a function of time and dosage level were determined in 40 rabbits. A modified quantitative analysis that produced accurate and reproducible results was employed for the determination of ethchlorvynol levels. Further, ten blood and bone marrow samples containing ethchlorvynol were chosen to study the effects of storage for a period of 24 hours. Studies of blood and bone marrow ethchlorvynol levels with time showed no linear relationship. Bone marrow/blood ratios as a function of dose resulted in close mean averages with a wide range of values. Significant losses in both blood and bone marrow ethchlorvynol levels were evidenced in most of the samples subjected to the 24-hour storage study.

Rapid micro-method for the measurement of ethchlorvynol in blood plasma and in urine by gas-liquid chromatography.

A rapid gas-liquid chromatographic method has been developed for use in the measurement of the hypnotic drug ethchlorvynol in small (50 microliter) volumes of either blood plasma or urine. Neither solvent transfer nor evaporation steps are used in the procedure and sources of interference have proved to be minimal. The method has been applied primarily to the analysis of specimens obtained from patients who had ingested an overdose of this drug. However with slight modification, the technique may be used in the measurement of the plasma concentrations of ethchlorvynol attained during therapy.