A versatile, sensitive, and selective high-performance liquid chromatographic (HPLC) procedure for the determination of common benzodiazepines and some of their most frequently occurring metabolites in forensic samples was developed and optimized with respect to effective and rapid sample preparation and high selectivity of the analytical assay. The optimized method includes liquid-liquid extraction of the drugs with chloroform followed by isocratic reversed-phase chromatography on a LiChrospher-100 RP-8ec column (150 x 4.6-mm i.d.) with a mobile phase consisting of 0.03 mol/L acetate buffer (pH 4.6)/acetonitrile (55:45, v/v). The use of dual-mode detection made up of UV-detection (250 nm) in series with reductive electrochemical detection (-1.4 V vs. Ag/AgCl) at the hanging mercury drop electrode permits the detection and quantitation of benzodiazepines even in degraded samples with higher selectivities than usually reached with conventional HPLC techniques. Depending on the actual benzodiazepine species, detection limits are in the range of 2.0 to 14.1 ng/mL. Mean recovery values of the drugs from blood range from 82 to 92%; within-day and day-to-day repeatabilities typically lie between 3 and 9%. Several case work examples demonstrate the high selectivity and remarkably low matrix sensitivity of the described assay.
The toxicologic findings of a fatal poisoning with rifampicin (Rimactan) are presented. The concentration of rifampicin and its two major metabolites 25-desacetylrifampicin and 3-formylrifamycin in post-mortem blood, urine, bile and liver at about 10 h after ingestion of 14-15 g was determined using a high-performance liquid chromatographic method. The results of the toxicological analyses were compared with findings in fatal and non-fatal intoxications and after therapeutic administration of the drug. Possible explanation for the fatal outcome is given.
Barioliths consist of inspissated barium mixed with feces. They are a rare complication after barium contrast roentgenography and occur almost exclusively in the large bowel. Mostly asymptomatic or causing only slight symptoms and signs, they may persist for months or years. We report a severe case of cecal bariolith. Clinical symptoms and signs, radiological findings, intraoperative findings, and histology are presented and discussed with reference to the literature.
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