Sundström Ingela, Hedeland Mikael, Bondesson Ulf, Andrén Per E
Division of Analytical Pharmaceutical Chemistry, Uppsala University, Biomedical Center, P.O. Box 574, SE-751 23 Uppsala, Sweden.
J Mass Spectrom. 2002 Apr;37(4):414-20. doi: 10.1002/jms.298.
The glucuronide conjugates of ketobemidone, norketobemidone and hydroxymethoxyketobemidone were identified in human urine post-intravenous administration of Ketogan Novum. The human urine was extracted on a mixed-mode solid-phase micro-column before analysis with liquid chromatography/electrospray ionization time-of-flight mass spectrometry (LC/ESI-TOF-MS) and tandem MS (MS/MS). Accurate mass and collision-induced dissociation product ion spectra were used for identification of the glucuronide conjugates. Two different TOF mass spectrometers were used and the accurate mass measurements were performed on three separate days with each instrument. The accuracy of the mass measurements was better than 2.1 ppm for two out of three conjugates and the inter-day relative standard deviation was within +/-0.00049%. The MS/MS fragmentation patterns of the conjugates were in accordance with those of the synthetic aglycones and included peaks originating from the M + H ion of the respective aglycone.
在静脉注射Ketogan Novum后，在人尿液中鉴定出了凯托米酮、去甲凯托米酮和羟基甲氧基凯托米酮的葡萄糖醛酸缀合物。在采用液相色谱/电喷雾电离飞行时间质谱（LC/ESI-TOF-MS）和串联质谱（MS/MS）进行分析之前，先在混合模式固相微柱上对人尿液进行提取。利用精确质量和碰撞诱导解离产物离子谱对葡萄糖醛酸缀合物进行鉴定。使用了两台不同的飞行时间质谱仪，并且在三天内分别使用每台仪器进行精确质量测量。三种缀合物中的两种的质量测量准确度优于2.1 ppm，日间相对标准偏差在±0.00049%以内。缀合物的MS/MS碎裂模式与合成苷元的碎裂模式一致，并且包括源自各个苷元的M + H离子的峰。
