Paul B D, Mitchell J M, Mell L D, Irving J
Navy Drug Screening Laboratory, Norfolk, Virginia 23511-6295.
J Anal Toxicol. 1989 Jan-Feb;13(1):2-7. doi: 10.1093/jat/13.1.2.
A procedure for detection and quantification of urinary 6-acetylmorphine (6-AM), a metabolite of heroin, is described. After initial solvent extraction from urine, the 6-AM was purified either by acid-base liquid-liquid extraction or by solid-phase extraction techniques. The 6-AM was then derivatized to its propionyl ester, which was characterized by gas chromatography/mass spectrometry in the electron impact mode. Confirmation of 6-AM was accomplished by comparing retention times and relative abundances of selected ions with that of a standard. Quantification was based on 6-[2H3]acetyl-N-[2H3]methylnormophine (6-[2H6]AM) as internal standard. Excellent linearity was obtained in the concentration range 1-100 ng/mL. The overall yield after solvent extraction and acid-base purification ranged from 79 to 82%; for solvent extraction and solid-phase purification, it was 92 to 95%. The limit of detection was 810 pg/mL. Within-run and between-run CVs for 6-AM at concentrations in the range 1-100 ng/mL were generally less than 5% and less than 10%, respectively.
本文描述了一种检测和定量尿液中6-乙酰吗啡（6-AM，海洛因的一种代谢物）的方法。从尿液中进行初始溶剂萃取后，6-AM可通过酸碱液液萃取或固相萃取技术进行纯化。然后将6-AM衍生化为其丙酰酯，通过电子轰击模式下的气相色谱/质谱对其进行表征。通过将选定离子的保留时间和相对丰度与标准品进行比较来确认6-AM。定量基于6-[2H3]乙酰基-N-[2H3]甲基去甲吗啡（6-[2H6]AM）作为内标。在1-100 ng/mL的浓度范围内获得了良好的线性。溶剂萃取和酸碱纯化后的总产率为79%至82%；溶剂萃取和固相纯化后的总产率为92%至95%。检测限为810 pg/mL。6-AM在1-100 ng/mL浓度范围内的批内和批间变异系数通常分别小于5%和小于10%。
