PMID- 38039622 OWN - NLM STAT- MEDLINE DCOM- 20240108 LR - 20240108 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1713 DP - 2024 Jan 4 TI - Dummy molecularly imprinted polymer-based solid-phase extraction method for the determination of some phthalate monoesters in urine by gas chromatography-mass spectrometry analysis. PG - 464532 LID - S0021-9673(23)00757-4 [pii] LID - 10.1016/j.chroma.2023.464532 [doi] AB - A dummy molecularly imprinted polymer-based solid-phase extraction (SPE) sorbent was used for the selective extraction of some phthalate monoesters, monoethyl phthalate (MEP), monobutyl phthalate (MnBP) and mono-(2-ethylhexyl) phthalate (MEHP) in urine prior to gas-chromatography-mass spectrometry (GC-MS) analysis. Diethyl phthalate (DEP), a phthalate ester, was successfully used as a dummy template to prepare selective sorbent for MEP, MnBP, and MEHP extraction. DEP-imprinted poly(ethylene glycol dimethacrylate N-methacryloyl-l-tryptophan methyl ester) (DPEMT) microbeads were synthesized by suspension polymerization and characterized by Fourier Transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and Brunauer Emmet Teller (BET) analysis. The critical parameters (i.e., pH, sorbent amount, ionic strength, sample volume, elution solvent) affecting the extraction performance of the DPEMT-SPE sorbent were optimized. Under optimum conditions, good linearities were obtained in the concentration range of 4 to 60 ng/mL with determination coefficients (R(2)) of greater than 0.9959. The developed SPE method provided low limits of detection (LOD) of 0.05-1.20 ng/mL and limits of quantification (LOQ) of 0.18-4.01 ng/mL with relative standard deviations (RSDs) of less than 8.95 % for intra- and inter-day analyses. The proposed SPE method was used to analyze phthalate monoesters in spiked urine samples, and recoveries of 97.45-109.26 % were obtained. DPEMT-SPE sorbent was reused for 15 times without any losses of performance. Consequently, a highly selective and sensitive SPE method based on a dummy molecularly imprinted polymer combined with GC-MS was successfully developed to monitor human phthalate exposure via urine samples. CI - Copyright (c) 2023. Published by Elsevier B.V. FAU - Kucuk, Melike AU - Kucuk M AD - Department of Chemistry, Faculty of Arts and Science, Bursa Uludag University, Gorukle, Bursa 16059, Turkey. FAU - Osman, Bilgen AU - Osman B AD - Department of Chemistry, Faculty of Arts and Science, Bursa Uludag University, Gorukle, Bursa 16059, Turkey. FAU - Tumay Ozer, Elif AU - Tumay Ozer E AD - Department of Chemistry, Faculty of Arts and Science, Bursa Uludag University, Gorukle, Bursa 16059, Turkey. Electronic address: etumay@uludag.edu.tr. LA - eng PT - Journal Article DEP - 20231125 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Molecularly Imprinted Polymers) RN - 6O7F7IX66E (phthalic acid) RN - FU2EWB60RT (mono-(2-ethylhexyl)phthalate) RN - ZI46LWZ45G (monobutyl phthalate) RN - 0 (monoethyl phthalate) SB - IM MH - Humans MH - Gas Chromatography-Mass Spectrometry/methods MH - *Molecularly Imprinted Polymers MH - Solid Phase Extraction/methods MH - *Molecular Imprinting/methods OTO - NOTNLM OT - Dummy molecular imprinting OT - GC-MS OT - Phthalate monoester OT - SPE OT - Urine COIS- Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. EDAT- 2023/12/02 00:41 MHDA- 2024/01/08 06:43 CRDT- 2023/12/01 18:03 PHST- 2023/09/06 00:00 [received] PHST- 2023/11/13 00:00 [revised] PHST- 2023/11/24 00:00 [accepted] PHST- 2024/01/08 06:43 [medline] PHST- 2023/12/02 00:41 [pubmed] PHST- 2023/12/01 18:03 [entrez] AID - S0021-9673(23)00757-4 [pii] AID - 10.1016/j.chroma.2023.464532 [doi] PST - ppublish SO - J Chromatogr A. 2024 Jan 4;1713:464532. doi: 10.1016/j.chroma.2023.464532. Epub 2023 Nov 25.