Quantitative analysis of maytansinoid (DM1) in human serum by on-line solid phase extraction coupled with liquid chromatography tandem mass spectrometry - Method validation and its application to clinical samples

Journal of Pharmaceutical and Biomedical Analysis
Olivier HeudiOlivier Kretz

Abstract

A sensitive and specific method was developed and validated for the quantitation of maytansinoid (DM1) in human serum using on-line solid phase extraction (SPE)-liquid chromatography-tandem mass spectrometry (LC-MS/MS). Because DM1 contains a free thiol moiety, likely to readily dimerize or react with other thiol-containing molecules in serum, samples were pre-treated with a reducing agent [tris (2-carboxyethyl) phosphine] (TCEP) and further blocked with N-ethylmaleimide (NEM). The resulting samples were diluted with acetonitrile prior to the on-line solid phase extraction (SPE) on a C18 cartridge. A C18 (150×4.6mm ID 3μm particle size) column was used for chromatographic separation with a 10.0min HPLC gradient and DM1-NEM was detected in the selected reaction monitoring mode of a triple quadrupole mass spectrometer. DM1 concentrations were back-calculated from DM1-NEM amount found in the human serum samples. The quantitation range of the method was 0.200-200ng/mL when using 0.25mL serum. Within-run day precisions (n=6) were 0.9-4.4% and between-run day (3 days runs; n=18) precisions 2.5-5.6%. Method biases were between 3.5-14.5% across the whole calibration range. DM1-NEM exhibited sufficiently stability under all relevant ana...Continue Reading

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Citations

Jun 9, 2016·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·Dwight StollAlain Beck
Jul 28, 2016·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·Tao ChenKelly Zhang
Jul 6, 2016·Molecular Pharmaceutics·Boning LiuHao Wang
Sep 21, 2016·Philosophical Transactions. Series A, Mathematical, Physical, and Engineering Sciences·Glenn LoosDeirdre Cabooter
Dec 18, 2020·Pharmaceuticals·Héloïse Cahuzac, Laurent Devel
Jul 10, 2017·Journal of Pharmaceutical and Biomedical Analysis·Balázs BobálySzabolcs Fekete

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