采用固相萃取和超高效液相色谱-串联质谱法快速测定人血浆中的去氧孕烯。
Simple and rapid determination of norethindrone in human plasma by supported liquid extraction and ultra performance liquid chromatography with tandem mass spectrometry.
机构信息
Department of Bioanalytical Chemistry, Covance Inc., 8211 SciCor Dr., Indianapolis, IN 46214, USA.
出版信息
Talanta. 2012 Mar 15;91:77-82. doi: 10.1016/j.talanta.2012.01.019. Epub 2012 Jan 14.
We report for the first time an ultra performance liquid chromatographic method with tandem mass spectrometric detection (UPLC/MS/MS) for the determination of norethindrone alone in human plasma over the concentration range of 50.0-25000 pg mL(-1) using a sample volume of 0.250 mL. Norethindrone and its internal standard (ISTD), norethindrone-(13)C(2), were extracted from human plasma by supported liquid extraction (SLE). After evaporation of the organic solvent, samples were reconstituted and analyzed on an UPLC/MS/MS system. The UPLC system used a Waters BEH C18 (100 mm × 2.1mm, 1.7 μm) column with mobile phase A of 0.05% formic acid in water:acetonitrile (65:35, v/v) and mobile phase B of 0.05% formic acid in methanol:acetonitrile (50:50, v/v). The flow rate was 0.500 mL min(-1). The method was fully validated. The inter-run accuracy and precision at the lower limit of quantitation (LLOQ), low, mid and high quality control (QC) concentration levels were 99.2-108.4% with a <8.1% CV (coefficient of variation), respectively. The validated method has been successfully applied to analysis of thousands of pharmacokinetic samples.
我们首次报道了一种超高效液相色谱-串联质谱法（UPLC/MS/MS），用于测定人血浆中单独的去氧孕烯浓度范围为 50.0-25000 pg/mL（使用 0.250 mL 样品体积）。去氧孕烯及其内标（ISTD），去氧孕烯-（13）C（2），通过支持液体萃取（SLE）从人血浆中提取。在蒸发有机溶剂后，用 UPLC/MS/MS 系统重新制备和分析样品。UPLC 系统使用 Waters BEH C18（100mm×2.1mm，1.7μm）柱，流动相 A 为 0.05%甲酸水溶液：乙腈（65:35，v/v），流动相 B 为 0.05%甲酸甲醇：乙腈（50:50，v/v）。流速为 0.500mL/min。该方法经过全面验证。在定量下限（LLOQ）、低、中、高质控（QC）浓度水平的批间准确度和精密度分别为 99.2-108.4%，<8.1%CV（变异系数）。验证后的方法已成功应用于数千个药代动力学样品的分析。
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