ABSTRACT
A quantitative gas chromatographic (GC) method for the screening and confirmation of barbiturates in post mortem blood specimens is presented. Barbiturates were extracted from blood samples and the extracts cleaned-up, concentrated, and then analyzed as free drugs on a 10% UCW-982 GC column. Samples screened positive for free barbiturates were methylated to form 1,3-dimethylbarbiturates, which were then chromatographed on a 3% SE-30 column to confirm the barbiturate identity.
Subject(s)
Barbiturates/blood , Barbiturates/poisoning , Chromatography, Gas , HumansABSTRACT
A procedure has been developed for the TLC and GLC analysis of codeine and morphine derivatives in urine in cases where there is too much interference for TLC analysis as free drugs. Urine is hydrolyzed, then split into two fractions. One fraction is extracted with a polar solvent, concentrated, and acetylated. An aliquot is injected in a 3% OV-17 column and the rest is spotted on a plate developed in hexane:chloroform:diethylamine (50:30:6). The other fraction is ethylated (converting morphine to ethylmorphine), extracted with a nonpolar solvent, concentrated, acetylated, concentrated, and then spotted on a plate developed in hexane:n-butanol:acetonitrile:diethylamine (80:5:5:10). Codeine and morphine can be detected without interference at concentrations as low as 0.3 micrograms/mL.
Subject(s)
Codeine/urine , Morphine/urine , Chromatography, Gas/methods , Chromatography, Thin Layer/methods , Codeine/analogs & derivatives , Morphine Derivatives/urineABSTRACT
A thin-layer chromatography (TLC) procedure has been developed for the analysis of urine samples for benzoylecgonine and norpropoxyphene, the major metabolites of cocaine and propoxyphene, respectively. Urine is made slightly acidic and methylated with dimethyl sulfate to convert the difficult-to-extract benzoylecgonine back into the much more readily extractable cocaine. The urine is then chilled, made basic, and extracted with chloroform/isopropanol. The organic layer containing the cocaine and norpropoxyphene is separated and evaporated to dryness. The residue is reconstituted and spotted on a TLC plate which is developed in hexane:chloroform:diethylamine (80:10:10) which separates the two substances without interference from other drugs, metabolites, and urinary substances. The two substances are visualized with acidified iodoplatinate spray and can be detected down to levels of 2.0 microgram/mL for benzoylecgonine and 1.0 microgram/mL for norpropoxyphene.
Subject(s)
Cocaine/analogs & derivatives , Dextropropoxyphene/analogs & derivatives , Chromatography, Thin Layer , Cocaine/urine , Dextropropoxyphene/metabolism , Dextropropoxyphene/urine , Humans , MethodsABSTRACT
A thin-layer chromatography (TLC) procedure for the screening and confirmation of urinary codeine and morphine has been developed. Urine samples are hydrolyzed to liberate free codeine and morphine, extracted into an organic solvent, and concentrated. For screening, the extraction residues are spotted on TLC plates which are developed in chloroform:ethyl acetate:methanol:propylamine (35:45:5:5). For confirmation, the extraction residues are acetylated and then spotted on TLC plates which are developed in hexane:chloroform:diethylamine (50:30:7). The spots for the two drugs are visualized with acidified iodoplatinate. Codeine and morphine are well separated from one another and from normal urinary substances on both plates and can be detected at a concentration of 0.4 micrograms/mL.
