Stomach, small intestine contents, blood, liver, kidney and urine of a 28-years old man, were analyzed for residues of Endosulfan (6, 7, 8, 9, 10, 10-hexachloro-1, 5, 5a, 6, 9, 9a-hexahydro-6, 9-methano-2, 4, 3-benzo(e)dioxathiepin 3-oxide). The analysis results showed the presence of high concentrations of the two endosulfan isomers in all samples. Since also alcohol was present in all the tissues analyzed, it was concluded that the victim died of a combined endosulfan-alcohol poisoning. No other drugs were found.
High-resolution gas chromatography (HRGC) and gas chromatography/mass spectrometry (GC/MS) are the techniques of choice to determine the retention indices of more than 200 organic acids as their trimethylsilyl (TMS) or oxime-trimethylsilyl derivatives. Several types of apolar and semipolar fused-silica capillary columns (OV-1, SE-52, and OV-1701), used to analyze and separate organic acids isolated from urine samples, are evaluated.
A new, sensitive and selective detection method for vitamin K1 in human serum is reported. After the chromatographic separation, vitamin K is converted to its hydroquinone form in a wet-chemical post-column reduction reaction with tetramethylammonium octahydridotriborate. The reaction proceeds in an open tubular knitted reaction coil at elevated temperature. This system, when combined with a two-step multidimensional liquid chromatographic separation, has proven useful for the quantitative determination of serum concentrations of vitamin K1 in normal, healthy individuals.
A multi-stage screening and identification scheme for the diagnosis of inborn errors in amino acid, fatty acid, carbohydrate and intermediary metabolism is described. The method is based on a computerized analysis of data obtained with dual-column gas chromatography/FID (GC/FID) and gas chromatography/mass spectrometry (GC/MS) profiling of urinary organic acids. It involves: (1) isolation of the compounds by solvent or solid-phase extraction; (2) conversion into trimethylsilyl (TMS) or TMS-oxime derivatives; (3) GC/FID analysis on SE-52 and OV-1701 capillary columns; (4) tentative identification by comparing the methylene unit (MU) values on both columns with a user-built library of reference compounds; (5) quantitative evaluation of the excretion profile; and (6) analysis by GC/MS of samples with an abnormal profile using an automated peak identification programme.
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