Simple and rapid determination of norethindrone in human plasma by supported liquid extraction and ultra performance liquid chromatography with tandem mass spectrometry

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• 作者：Zhilong Gong ; ^{zhilong.gong@covance.com} ; Kiresha Chandler ; Stephen Webster ; Remy Kerley ; Susan Buist ; Melanie McCort-Tipton
• 关键词：Norethindrone ; Ultra performance liquid chromatography ; Mass spectrometry ; Supported liquid extraction
• 刊名：Talanta
• 出版年：2012
• 期刊代码：106_00399140
• 类别：ch
• 出版时间：15 March, 2012
• 卷：91
• 期：Complete
• 页码：77-82
• 文件大小：442 K

摘要

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 50.0-25 000 pg mL^鈭? using a sample volume of 0.250 mL. Norethindrone and its internal standard (ISTD), norethindrone-¹³C₂, 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 脳 2.1 mm, 1.7 渭m) 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^鈭?. 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.