Souza Seba Karine, Berg Cattani Vitória, Saraiva Gonçalves José Carlos, Vianna-Jorge Rosane, Elias Estrela Rita de Cássia
Fundação Oswaldo Cruz, Escola Nacional de Saúde Pública, Programa de Pós-Graduação em Saúde Pública e Meio Ambiente, Rio de Janeiro, RJ, Brasil.
Universidade Federal do Rio de Janeiro, Faculdade de Farmácia, Rio de Janeiro, RJ, Brasil.
Bioanalysis. 2019 May;11(10):913-922. doi: 10.4155/bio-2018-0323.
To develop and validate a simple method using LC-MS/MS for determination of dextromethorphan (DXM) and dextrorphan (DT) in human oral fluid. Following protein precipitation, chromatographic separation used a phenyl column with isocratic elution (1 ml/min) of 10 mM ammonium-formate buffer and acetonitrile (65:35; v/v) with 0.1% formic acid. Retention times were 2.6 min for DT and 5 min for DXM. Total run time was 7 min. The intra- and inter-assay deviations (accuracy) for DT (1-100 ng/ml) and DXM (5-1000 ng/ml) ranged from -13.6 to 8.8% and -9.6 to 5.7%, respectively. Precision variations were ≤7.5%. Matrix effect was ≤11.8%. This method may prove helpful for quantification of DT and DXM in oral fluid for either clinical or toxicological purposes.
开发并验证一种使用液相色谱-串联质谱法(LC-MS/MS)测定人唾液中右美沙芬(DXM)和右啡烷(DT)的简单方法。蛋白质沉淀后,色谱分离采用苯基柱,以10 mM甲酸铵缓冲液和乙腈(65:35;v/v)加0.1%甲酸进行等度洗脱(1 ml/min)。DT的保留时间为2.6分钟,DXM的保留时间为5分钟。总运行时间为7分钟。DT(1-100 ng/ml)和DXM(5-1000 ng/ml)的批内和批间偏差(准确度)分别为-13.6%至8.8%和-9.6%至5.7%。精密度变化≤7.5%。基质效应≤11.8%。该方法可能有助于临床或毒理学目的下人唾液中DT和DXM的定量分析。