4.4 Article

A simple extraction and LC-MS/MS approach for the screening and identification of over 100 analytes in eight different matrices

Journal

DRUG TESTING AND ANALYSIS
Volume 7, Issue 3, Pages 214-240

Publisher

WILEY
DOI: 10.1002/dta.1657

Keywords

LC-MS; MS; biosamples; multi-analyte; liquid-liquid extraction

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In the present study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) multi-analyte approach using one single work-up approach in whole blood, plasma, serum, post-mortem blood, liver tissue, gastric content, hair, and urine was developed for fast target screening and reliable identification of 130 analytes often requested in clinical and forensic toxicology. Samples (500 L each) of whole blood, plasma, serum, post-mortem blood, tissue (homogenized 1+4 with water), as well as 3 g of distilled gastric contents, 1 mL of urine, or 20 mg of pulverized hair were extracted at different pH values with an diethyl ether-ethyl acetate mixture (1:1). Separation and identification were performed using LC-QTRAP with electrospray ionization in positive mode. For identification 1 scheduled multi-reaction-mode (sMRM) method with 390 transitions was developed covering benzodiazepines, Z-drugs, antidepressants, neuroleptics, opioids, new synthetic drugs, and phosphodiesterase type 5 inhibitors. For positive sMRM transitions with intensities exceeding 5000 cps, dependent scans (EPI scan collision energy, 35 eV, collision energy spread, 15 eV) were performed for library search using our in-house library. The method was developed with respect to selectivity, matrix effects, recovery, process efficiency, limit of detection, and applicability. The simple work-up procedure was suitable for all biosamples with exception of urine in respect to low concentrated analytes, which showed median recovery values of 59%. The method was selective for 130 analytes in all 8 biosamples. For 106 analytes, the limit of detection in whole blood, plasma, and serum was lower than the lowest therapeutic concentration listed in blood level lists. Copyright (c) 2014 John Wiley & Sons, Ltd.

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