Verebey K, DePace A, Mulé S J
J Chromatogr. 1985 Oct 11;343(2):339-48. doi: 10.1016/s0378-4347(00)84602-2.
A procedure is described for the simultaneous measurement of l-alpha-acetylmethadol and its two pharmacologically active metabolites: noracetylmethadol and dinoracetylmethadol. In the method an intramolecular conversion reaction of the two metabolites to their amide configuration is utilized. The reaction is performed while the metabolites are still in the serum. Following solvent extraction the samples are analyzed by capillary gas-liquid chromatography coupled with nitrogen detection. Quantitation is achieved by internal standardization. The lower limit of sensitivity is 5 ng/ml in serum. Absolute sensitivity is 0.1 ng for all three compounds. The advantages over other procedures are: speed due to the single extraction step; increased recovery of noracetylmethadol and dinoracetylmethadol due to decreased polarity of the amides; greater stability of the metabolites in the amide configuration; better chromatographic quantitation and separation because detector response for the amides is greater than it is for the original configuration of the metabolites and the area of the chromatographic tracing is free of interfering substances.
本文描述了一种同时测定l-α-乙酰美沙醇及其两种药理活性代谢物：去甲乙酰美沙醇和双去甲乙酰美沙醇的方法。该方法利用了两种代谢物向其酰胺构型的分子内转化反应。该反应在代谢物仍存在于血清中时进行。溶剂萃取后，样品通过毛细管气液色谱结合氮检测进行分析。通过内标法进行定量。血清中的检测下限为5 ng/ml。所有三种化合物的绝对灵敏度为0.1 ng。与其他方法相比，其优点包括：由于只需一步萃取，速度更快；由于酰胺极性降低，去甲乙酰美沙醇和双去甲乙酰美沙醇的回收率提高；代谢物在酰胺构型下更稳定；由于酰胺的检测器响应大于代谢物原始构型的响应，且色谱图面积无干扰物质，因此色谱定量和分离效果更好。
