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Updated: Jan 21, 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
Porphyrin-functionalized graphene oxide sheets: An efficient nanomaterial for micro solid phase extraction of
Mahshid Manouchehri1, Shahram Seidi1, Ahmad Rouhollahi1
1Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran, Iran.
Abstract:
In this work, porphyrin-functionalized graphene oxide nanosheets (GO@meso-tetrakis(4-hydroxyphenyl)porphyrin) were synthesized and employed as the sorbent. Porphyrins owing to their unique structures and tunable terminal functional groups are expected to be promising media for extraction of the desired analytes. Also, GO with a high specific surface area has exhibited good potential for the extraction purposes. Inspired by these intriguing properties, the combination of GO and porphyrin can benefit both of these amazing features. The synthesized sorbent was utilized for micro solid phase extraction of non-steroidal anti-inflammatory drugs followed by HPLC-UV. Optimization of the experimental factors including sorbent amount, sample pH, sample and eluent flowrates, eluent volume, and the number of desorption cycles were performed with the aid of central composite design. Under the optimal conditions, the calibration curves were linear within the range of 2.0-600 ng mL-1 and limits of detection were found between 0.5-2.0 ng mL-1. The preconcentration factors and absolute recoveries were obtained in the range of 4.80-9.79 and 29%-59%, respectively. The matrix effect for the urine samples varied between 81.9%-91.6% at two concentrations of 50 and 300 ng mL-1, respectively. Intra- and inter-day RSD% (n = 3) of the spiked urine samples at three level concentrations of 25, 100, and 300 ng mL-1 were less than 10%. The relative recoveries of the urine samples were calculated in the range of 85.2-98.6%. Eventually, the method exhibits proper sensitivity, excellent repeatability, high reusability, and acceptable precision and accuracy.
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