Department of Pharmacology and Molecular Sciences, Division of Clinical Pharmacology, Johns Hopkins University School of Medicine, 600 North Wolfe Street, Osler 527, Baltimore, MD 21287, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Dec 1;878(31):3217-24. doi: 10.1016/j.jchromb.2010.09.011. Epub 2010 Oct 8.
A combined UPLC-tandem mass spectrometric (UPLC-MS/MS) technique has been validated for quantitation of protein free efavirenz (EFV) as well as total concentrations of EFV in human blood and seminal plasma. The analytical method possesses capabilities for concentration measurements of EFV ranging from 0.5 to 10,000ng/ml with an accuracy (%dev) of -5.2-8.0% and precision (%CV) of <8%. Standard curves were linear with coefficients of variation (r(2)) >0.98. The method employs a racemic fluorinated analog of EFV (F-EFV) as the internal standard. EFV and F-EFV were eluted from a reverse-phase UPLC column via gradient elution with detection via negative ion multiple reaction monitoring (MRM). EFV and F-EFV, respectively, were detected via the following MRM transitions: m/z 314.0>244.1 and m/z 298.0>227.9. The time required for the analysis of each sample was 8.0min. The analytical technique is capable of a reliable detection limit of ∼15-20fmol of EFV injected on column.
一种联合超高效液相色谱-串联质谱（UPLC-MS/MS）技术已经被验证可用于定量检测人血液和精液中的游离依非韦伦（EFV）以及总浓度。该分析方法具有测量 EFV 浓度的能力，范围从 0.5 到 10,000ng/ml，准确度（%dev）为-5.2-8.0%，精密度（%CV）<8%。标准曲线具有大于 0.98 的变异系数（r(2)）。该方法采用 EFV 的对映体氟化类似物（F-EFV）作为内标。EFV 和 F-EFV 通过反相 UPLC 柱的梯度洗脱洗脱，并通过负离子多反应监测（MRM）进行检测。EFV 和 F-EFV 分别通过以下 MRM 转换进行检测：m/z 314.0>244.1 和 m/z 298.0>227.9。分析每个样品所需的时间为 8.0 分钟。该分析技术能够可靠地检测到柱上注入的约 15-20fmol 的 EFV。
