Application of Fe3O4@TbBd nanobeads in microextraction by packed sorbent (MEPS) for determination of BTEXs biomarkers by HPLC–UV in urine samples

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2022-05, Vol.1197, p.123197-123197, Article 123197
• Main Authors: Kurd, Nematullah, Bahrami, Abdulrahman, Afkhami, Abbas, Shahna, Farshid Ghorbani, Assari, Mohammad Javad, Farhadian, Maryam
• Format: Article
• Language: English
• Subjects: BTEX biomarkers; Fe3O4@TbBd nanobeads; HPLC-UV; Microextraction by packed sorbent; Urine samples
• ISSN: 1570-0232; 1873-376X
• DOI: 10.1016/j.jchromb.2022.123197

[Display omitted] •Fe3O4@TbBd sorbent with MEPS technique used to extract and determine of BTEXs chief biomarkers for the first time.•Fe3O4@TbBd sorbent represented good adsorption efficiency for the extraction of tt-MA, MA, HA and m-MHA in urine.•MEPS with Fe3O4@TbBd sorbent is a practical evaluation method for BTEXs chief biomarkers in urine. A relatively new adsorbent based on covalent organic frameworks (COFs) was employed for the first time to extract and determine Trans, trans-muconic acid (tt-MA), Mandelic acid (MA), Hippuric acid (HA), and 3-Methylhippuric acid (m-MHA) in urine. For this purpose, microextraction was performed using the packed sorbent (MEPS) method. Following the extraction process, the prepared samples were specified via the high-performance liquid chromatography-ultraviolet detector system. The precipitation polymerization was applied to synthesize the Fe3O4@TbBd nanobeads, and the morphological and dimensional structures of the products were specified with FE-SEM images. Some key variables affecting the extraction efficiency (i.e., sample volume, elution volume, condition and washing solvents, type and volume of elution solvent, extraction cycles, temperature, and pH of the sample solution) were investigated. In ideal conditions, the limit of detection (LOD) was obtained from 0.02 µg/ml for tt-MA to 0.5 µg/ml for MA. Calibration curves (at five-point) were plotted in the range 0.05–5 µg/ml for tt-MA to 1–300 µg/ml for MA (R2 > 0.98). Moreover, intra- and inter-day precision values were 3.1–5.5 and 4.6–9.8%, respectively. The developed method was successfully employed to determine four analytes in three concentrations (low, medium, and high QCs). The results showed a satisfactory recovery (70–87%). COF-MEPS technique is a rapid, easy, user-friendly, and environment-friendly method for separating the minimum values of all BTEXs chief biomarkers from urine samples without using complicated processes and only with one adsorbent. Also, it can be a good alternative for biomonitoring the workers exposed to BTEX compounds in occupational and environmental access.