Institute of Legal Medicine and Traffic Medicine, University Hospital, Heidelberg, Germany.
Forensic Sci Int. 2010 Feb 25;195(1-3):73-7. doi: 10.1016/j.forsciint.2009.11.015. Epub 2009 Dec 16.
A liquid chromatographic/electrospray ionization tandem mass spectrometric method for the quantification of buprenorphine (BUP), norbuprenorphine (NBUP), buprenorphine-3-beta-D-glucuronide (BUPG) and norbuprenorphine-3-beta-D-glucuronide (NBUPG) in serum samples was developed and validated. Pre-treatment of BUP and NBUP was by liquid-liquid extraction, while glucuronides were favourably isolated by solid phase extraction. Separation in 2 separate runs (2 x 5 min) was achieved using isocratic elution. The method was applied to 20 authentic serum specimens collected for law enforcement purposes where BUP intake had been indicated. The parent drug was not detectable in half of the specimens at a lower limit of detection of 0.2 ng/mL, whereas NBUP could be determined from any sample but one. NBUPG is the major metabolite present, which could be identified along with BUPG in all samples under investigation. In authentic specimens it could be advisable to monitor BUP metabolites along with the parent drug.
建立并验证了一种用于血清样品中丁丙诺啡(BUP)、去甲丁丙诺啡(NBUP)、丁丙诺啡-3-β-D-葡糖苷酸(BUPG)和去甲丁丙诺啡-3-β-D-葡糖苷酸(NBUPG)定量的液相色谱/电喷雾串联质谱分析方法。BUP 和 NBUP 的预处理采用液-液萃取,而葡糖苷酸则通过固相萃取有利地分离。通过等度洗脱在 2 次单独运行(2 x 5 min)中实现分离。该方法应用于 20 份为执法目的收集的真实血清标本,其中表明摄入了 BUP。在检测下限为 0.2 ng/mL 时,一半的标本中无法检测到母体药物,而 NBUP 可以从任何样本中检测到,但有一个例外。NBUPG 是主要的存在代谢物,在所有研究样本中均可与 BUPG 一起识别。在真实标本中,监测 BUP 代谢物与母体药物一起可能是明智的。