Department of Forensic and Biological Sciences, Bournemouth University, Talbot Campus, Fern Barrow, Poole, Dorset, United Kingdom.
J Anal Toxicol. 2012 Jan-Feb;36(1):1-11. doi: 10.1093/jat/bkr006.
A gas chromatography-ion trap-tandem mass spectrometry method was developed and validated for the simultaneous solid-phase extraction and quantification of cocaine, benzoylecgonine, cocaethylene, morphine, codeine, and 6-monoacteylmorphine in blood, muscle tissue, and water. An assay for total morphine in blood and muscle was also validated. The limit of quantification was ≤ 0.01 mg/kg in muscle and ≤ 0.005 mg/L in blood and water. Good linearity was observed over the concentration ranges studied (r ≥ 0.99). The repeatability (% RSD) at the three concentration levels was typically ≤ 15% and never exceeded 17%. Intermediate precision of ≤ 16% was obtained for all matrices. Deviation < 20% of the nominal concentration was obtained in all repeatability and intermediate precision experiments. Extraction recoveries for cocaine and metabolites ranged from 91% to 110% in water, 81% to 110% in blood, and 61% to 75% in muscle. Recoveries for opiates ranged from 59% to 104% in water, 50% to 95% in blood, and 41% to 79% in muscle. The hydrolysis efficiency for the total morphine assay in blood and muscle ranged from 91% to 99% with within-day and intermediate precisions of ≤ 14% and ≤ 12%, respectively.
建立并验证了一种气相色谱-离子阱串联质谱法，用于同时固相萃取和定量检测血液、肌肉组织和水中的可卡因、苯甲酰可卡因而、可卡因-乙醇、吗啡、可待因和 6-单乙酰吗啡。还验证了血液和肌肉中总吗啡的测定方法。肌肉中的定量限≤0.01mg/kg，血液和水中≤0.005mg/L。在所研究的浓度范围内观察到良好的线性（r≥0.99）。三个浓度水平的重复性（%RSD）通常≤15%，从未超过 17%。所有基质均获得≤16%的中间精密度。在所有重复性和中间精密度实验中，实测浓度与名义浓度的偏差均<20%。可卡因及其代谢物在水中的提取回收率为 91%至 110%，在血液中为 81%至 110%，在肌肉中为 61%至 75%。阿片类药物在水中的回收率为 59%至 104%，在血液中为 50%至 95%，在肌肉中为 41%至 79%。血液和肌肉中总吗啡测定的水解效率为 91%至 99%，日内和中间精密度分别≤14%和≤12%。
