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An automated headspace gas chromatography method was developed for the determination of formate (formic acid) in postmortem specimens, based on the in situ sulfuric acid-methanol methylation of formic acid to methyl formate. Diisopropyl ether was used as an internal standard. The method was applied to over 150 postmortem cases where methanol was detected. Of the 153 cases presented, 107 deaths were attributed to acute methanol toxicity. In the vast majority of the remaining 46 deaths, the methanol was determined to be present as a postmortem or perimortem artifact, or was otherwise incidental to the cause of death. Of the 76 victims who were found dead and blood was collected by the medical examiner, all but one had a postmortem blood formate concentration greater than 0.50 g/L (mean 0.85 g/L; n = 74). The sole exception involved suicidal ingestion of methanol where the blood methanol concentration was 7.9 g/L (790 mg/100 mL) and blood formate 0.12 g/L. In 97% (72/74) of the cases where blood was available, the blood formate was between 0.60 and 1.40 g/L. In 31 of the 153 cases, the victim was hospitalized and blood obtained on admission or soon after was analyzed for methanol and formate during the subsequent death investigation; the vast majority (27/30) had antemortem blood formate concentrations greater than 0.50 g/L. Cases with samples taken prior to death with blood formate concentrations less than 0.5 g/L can readily be explained by active treatment such as dialysis. The blood formate method has also been useful in confirming probable perimortem or postmortem contamination of one of more fluids or tissues with methanol (e.g., windshield washer fluid or embalming fluid), where methanol ingestion was unlikely.

A 73-year-old man developed nausea, vomiting, and diarrhea 20-30 min after receiving a 1.0 mg intravenous dose of colchicine for the treatment of severe pain due to gouty arthritis in his physician's office. He was hospitalized 8 h later, and his condition deteriorated as he developed renal and respiratory failure. He subsequently died 10 h later, or a total of 18 h after he received the original 1 mg colchicine injection. The patient received a prescription for oral 0.6 mg colchicine tablets 8 days previously and consumed eight tablets during that period, an average of 0.6 mg/day (42 of 50 tablets remained at the time of death). Colchicine concentrations were measured by liquid chromatography-mass spectrometry in selected ion monitoring mode using positive ionization. Chromatography was performed using an Eclipse XDB C8 analytical column (30 mm x 2.1-mm i.d., 3-microm particle size) and a programmed mobile phase consisting of 50 mM pH 4 ammonium acetate buffer and acetonitrile. Colchicine concentrations were as follows: 50 microg/L in cardiac blood, 10 microg/L in vitreous humor, 575 microg/kg in liver, 12,000 microg/L in bile, and 4.4 microg in 60 g received gastric contents (estimated total gastric contents 100 g). The cause of death was ruled to be "acute colchicine toxicity" and the manner of death "accidental."

Chem. 53,1936 (1975).The natural abundance 13C magnetic resonance spectra of some Lycopodium alkaloids have been determined at both 25.15 and 22.63 MHz. By using standard techniques it has been possible to make self-consistent assignments of almost all of the resonances. The results suggest some interesting conclusions regarding the stereochemistry of some of the alkaloids and have been used to confirm the stereochemical assignment at C-12 in sauroxine and to assign the preferred conformation (axial) of the N-methyl group in the obscurines and N-methyllycodine. THOMAS T. NAKASHIMA, PETER P. SINGER, LOIS M. BROWNE et WILLIAM A. AYER. Can. J. Chem. 53,1936Chem. 53, (1975.On a determine, i 25.15 et 22.63 MHz, les spectres de resonance magnetique nucleaire du 13C en abondance naturelle de quelques alkaloides Lycopodium. Utilisant les techniques habituelles, on a pu faire des attributions cohkrentes de pratiquement toutes les resonances. Les resultats obtenus suggkrent quelques conclusions interessantes concernant la stereochimie de quelqu'uns des alkaloides et ces rCsultats ont etC utilisb pour confirmer I'attribution stereochimiqueen C-12 dans la sauroxine et pour attribuer la conformation priviligik (axiale) du groupe N-methyle des obscurines et de la N-methyllycodine.[Traduit par le journal]

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