Theis D L, Halstead G W, Capponi V J, Roach B L, Robins R H
J Chromatogr. 1986 Mar 7;375(2):299-311. doi: 10.1016/s0378-4347(00)83722-6.
This paper describes the development of a capillary gas chromatographic--mass spectrometric method for the determination of N-[trans-2-(dimethylamino)cyclopentyl]-N-(3',4'-dichlorophenyl)propan amide and its metabolites in serum. The method utilizes an automated sample preparation whereby drug, metabolites and internal standard are extracted from polar serum components by adsorption chromatography onto an XAD-type resin. The N-demethylated metabolites are derivatized by acetylation prior to chromatography. Detection is by mass spectrometry with chemical ionization. This method was utilized to determine levels of unlabeled and pentadeuterated drug and their respective metabolites in canine serum after oral co-administration. No significant kinetic isotope effects were observed for either absorption or metabolism.
本文描述了一种毛细管气相色谱-质谱法的开发,用于测定血清中N-[反式-2-(二甲基氨基)环戊基]-N-(3',4'-二氯苯基)丙酰胺及其代谢物。该方法采用自动样品制备,通过吸附色谱法将药物、代谢物和内标从极性血清成分中提取到XAD型树脂上。N-去甲基代谢物在色谱分析前通过乙酰化进行衍生化。检测采用化学电离质谱法。该方法用于在口服共同给药后测定犬血清中未标记和五氘代药物及其各自代谢物的水平。在吸收或代谢方面均未观察到明显的动力学同位素效应。