Simultaneous identification and quantification of several opiates and derivatives by capillary gas chromatography and nitrogen selective detection

Summary

A capillary column gas chromatographic method is described for the simultaneous determination of morphine, codeine, heroin, 3- and 6-monoacetylmorphine, nalorphine, naloxone, ethylmorphine, and naltrexone. The drugs were extracted from 2 ml plasma, urine, or other biological samples, including tissue under alkaline conditions in chloroform-isopropanol-n-heptane (50:17:33, v/v), with levallorphan as an internal standard. The drugs were extracted into acid and then reextracted into chloroform after the acid had been alkalinized. After derivatization with trifluoroacetic anhydride, an aliquot was injected into a 25m capillary column equipped with a nitrogen phosphorus detector. The lower limits of detectability, extraction recovery, and the within-run and day-to-day precision of results were determined for each drug. Our results indicate that the procedure is suitable for use in overdose screening and therapeutic drug monitoring.

Zusammenfassung

Es wird eine Capillargaschromatographische Methode zur simultanen Bestimmung von Morphin, Codein, Heroin, 3- und 6-Mono-acetylmorphin, Nalorphin, Naloxone, Naltrexon und Ethylmorphin beschrieben. Von 2 ml Plasma, Urin oder anderen biologischen Proben (z. B. Gewebepräparate) wurden die Substanzen in alkalischen Milieu durch Chloroform: isopropylalkohol: n-heptan extrahiert, anschließend in Chloroform rückextrahiert. Nach Derivatiesierung mittels Trifluoressigsäureanhydrid wurden die aliquoten Teile an einer 25 m Capillarsäule eingesetzt. Die Detektion erfolgte durch einen Nitrogen-Phosphorous Detektor, und die Nachweisgrenzen und Wiederfindungsraten wurden ebenfalls ermittelt.