作者: Caroline Bylda , Vanya Velichkova , Jens Bolle , Roland Thiele , Uwe Kobold
DOI: 10.1002/DTA.1708
关键词: Analyte 、 Extraction (chemistry) 、 Phenacetin 、 Sample preparation 、 Imipramine 、 Electrospray 、 Selected reaction monitoring 、 Mass spectrometry 、 Chromatography 、 Chemistry
摘要: This paper describes a sample preparation method that complements previously published liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay for acetaminophen and eight structurally-related compounds in human serum (C. Bylda, R. Thiele, U. Kobold, D.A. Volmer. Drug Test. Anal. 2014, 6, 451). The analytes (acetaminophen [APAP] + metabolites acetaminophen-glucuronide [APG], -cysteine [APC], -mercapturate [APM] structurally similar analogues phenacetin p-phenetidine, as well tricyclic antidepressants imipramine amitryptiline) were extracted from using magnetized hyper-crosslinked polystyrene particles. protocol was developed by means of design experiments (DoE) statistical approach. Using three representative the analyte panel with different polarities (high, medium, low), two screening designs used to identify factors exhibited significant impact on recovery analytes. These parameters then optimized permit extraction complete target exhibiting broad range chemical polarities. Liquid chromatographic separations achieved gradient elution pentafluorphenyl column subsequent detection electrospray ionization-triple quadrupole multiple reaction monitoring (MRM) mode. linear over 0.1–100 µg/mL APAP, APG, p-phenetidine phenacetin, 0.03–50 µg/mL APS, 0.01–10 µg/mL APM, APC, amitriptyline, R2 > 0.99. good precision CVs ranging 2 9% all analytes; accuracy assessed comparing LC-MS/MS methods set 68 patient samples. Copyright © 2014 John Wiley & Sons, Ltd.