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PubMed1993

Automated sample preparation by on-line dialysis and trace enrichment. Analysis of morphine, 6-monoacetylmorphine, codeine, ethylmorphine and pholcodine in plasma and whole blood by capillary gas chromatography and capillary gas chromatography-mass spectrometry.

A fully automated sample preparation method for the determination of five opiates in human plasma and whole blood is described. The technique combines dialysis and trace enrichment prior to gas chromatography and gas chromatography-mass spectrometry. Dialysis and trace enrichment on a polymer column was shown to be a highly reliable method for sample preparation. The method can be used, after minor modification, to determine other basic drugs in plasma and whole blood. The method demonstrates the potential of the automated sequential trace enrichment of dialysate (ASTED) system for automated sample preparation.

Automation↗
PubMed2000

Synthesis of ring D modified morphinan systems via ring expansion of a key codeine intermediate

Ring expansion and ring fragmentation products were synthesized from pentacyclic ketones 3 and 4 via Baeyer-Villiger oxidation. Oxidation of 3 with m-chloroperbenzoic acid afforded delta-lactone 9 which was transformed to enone 12 en route to the C6 inverted ether 14. Analogous oxidation of 4 gave delta-lactone 18. Opening of the lactone ring of 14 and 18 led to seco structures which, in the case of 19, underwent reannulation with incorporation of nitrogen to yield the hydroxylactam 21.

Journal Article↗