M�tyus M�ria - Kocsis Gy�rgy - Boldis Ott� - Gach�lyi Andr�s

DETERMINATION OF MORPHINE AND CODEINE IN SERUM
AFTER POPPY SEED CONSUMPTION
USING GAS CHROMATOGRAPHY - MASS SPECTROMETRY

Absztrakt/Abstract

Egy analitikai elj�r�s ker�lt kidolgoz�sra a v�rsz�rum morfin �s kodein tartalm�nak meghat�roz�s�ra g�zkromatogr�fi�s-t�megspektrometri�s technik�val szelekt�v ionmonitoroz�s technik�val. Az elj�r�ssal k�s�r� sztenderdk�nt a vizsg�lt vegy�letek deut�riummal jel�lt molekul�it alkalmaztuk. A mint�k tiszt�t�sa �s kivon�sa szil�rdf�zis� extrakci�val t�rt�nt. A vizsg�lt hat�anyagokat penta-fluoropropionsavanhidriddel sz�rmaz�koltuk. A m�rt inonok (n/z) morfin: 414, 577 �s 361; morfin-D3: 417, 580 �s 364; kodein: 282, 445; kodein-D3: 285 �s 485 voltak. Az analitikai elj�r�s visszanyer�si hat�sfoka 10 ng/mL koncentr�ci�kn�l morfinn�l 70-80 % illetve kodeinn�l 75-85 %. Az elj�r�s mennyis�gi kimutat�si hat�r�rt�kei morfinn�l 0,87 ng/mL  illetve kodeinn�l 0,9 ng/mL. A kalibr�ci�hoz hum�n sz�rumot haszn�ltunk �gy, hogy a vizsg�lt anyagnak a kalibr�ci�hoz sz�ks�ges koncentr�ci�j� elegy�vel jel�lt�k meg.

An analytical method is presented here for the assessment of morphine and codeine concentrations in human serum by employing mass spectrometry in the selective ion monitoring mode following its separation with gas chromatography. Deuterated (marked with heavy water) analogies of the analytes were used as surrogate internal standards. Samples were cleaned up using solid phase extraction. The target compounds were analyzed as pentafluoropropionic esters. The monitored ions were m/z=414, 577 and 361 [morphine], m/z=417, 580 and360 [D3-morphine], m/z=282, 445 [codeine], m/z=274, 448, [D3-codeine]. The recovery of the analytes from solid phase extraction was 70 to 80% (morphine) and 75 to 85% (codeine) at a concentration of 10 ng/mL. The limit of quantitation (confidence limit) was 0.87 ng/mL for morphine and 0.9 ng/mL for codeine. Calibration was accomplished employing blank human serum spiked with the analytes at various concentrations.

Kulcsszavak/Keywords: tiltott k�b�t�szerek, anyagcsere, m�k, GS-MS, morfin, ingyenes morfin, kodein ~ illicit drugs, metabolites, poppy seed, GS-MS, serum morphine, free morphine, codeine

 

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