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Updated: Jan 31, 2026

Integration of Miniaturized Solid Phase Extraction and LC-MS/MS Detection of 3-Nitrotyrosine in Human Urine for Clinical Applications
Published on: July 14, 2017
Theoretical and experimental approach to hydrophilic interaction dispersive solid-phase extraction of
Joanna Giebułtowicz1, Monika Sobiech2, Monika Rużycka1
1Bioanalysis and Drugs Analysis Department, Faculty of Pharmacy, Medical University of Warsaw, Banacha 1, 02-097 Warsaw, Poland.
Abstract:
In this paper, we proposed an innovative hydrophilic interaction dispersive solid-phase extraction (HI-d-SPE) protocol suitable for the isolation of the potential cyanide intoxication marker, 2-aminothiazoline-4-carboxylic acid (ATCA), from such complicated matrix as post-mortem blood. To create an optimal HI-d-SPE protocol, two sorbents were used: a molecularly imprinted polymer (MIP) and commercially available Oasis-MCX®. The latter sorbent was identified as more recovery-efficient with higher clean-up abilities in a carefully optimized process. Computational analysis was employed to provide insight into the adsorption mechanism of the two selected sorbents. The theoretical results were in agreement with the experiment regarding the efficiency of the sorbent. HI-d-SPE was successfully applied to the analysis of ATCA in 20 post-mortem blood samples using LC-MS/MS. The analytical performance of the method was finally compared to prior existing methods, in turn revealing its superiority.
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