Bassem Jamoussi

Styrene, a chemical widely used in various industries, undergoes metabolic breakdown in the human body, resulting in the production of phenylglyoxylic acid (PGA). A novel molecularly imprinted polymer (MIP) was synthesised for selective extraction and enrichment of PGA in urine samples prior to high-performance liquid chromatography. The MIP employed in this research was a 4-vinylpyridine molecularly imprinted polymer (4-VPMIP) prepared via mass polymerisation using a noncovalent method. The structural and morphological characteristics of the molecularly imprinted polymers (MIPs) and non-imprinted polymers (NIPs) were evaluated using Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). The efficiency of the molecularly imprinted solid-phase extraction (MISPE) process was optimised by investigating critical variables such as sample pH, sorbent mass, sample flow rate, and volume of the elution solvent. A central composite design (CCD) within the response surface methodology was utilised to develop separate models for the adsorption and desorption steps. Analysis of variance (ANOVA) confirmed the excellent fit of the experimental data to the proposed response models. Under the optimised conditions, the molecularly imprinted polymers exhibited a higher degree of selectivity and affinity for PGA, with a relative selectivity coefficient (α) of 2.79 against hippuric acid. The limits of detection (LOD) and quantification (LOQ) for PGA were determined to be 0.5 mg/L and 1.6 mg/L, respectively. The recoveries of PGA ranged from 97.32% to 99.06%, with a relative standard deviation (RSD) lower than 4.6%. Furthermore, MIP(4VP)SPE demonstrated the potential for recycling up to three times without significant loss in analyte recovery.

4-Vinylpyridine molecularly imprinted polymer (4-VPMIP) microparticles for mandelic acid (MA) metabolite as a major biomarker of exposure to styrene (S) were synthesized by bulk polymerization with a noncovalent approach. A common mole ratio of 1:4:20 (i.e., metabolite template: functional monomer: cross-linking agent, respectively) was applied to allow the selective solid-phase extraction of MA in a urine sample followed by high-performance liquid chromatography–diode array detection (HPLC-DAD). In this research, the 4-VPMIP components were carefully selected: MA was used as a template (T), 4-Vinylpyridine (4-VP) as a functional monomer (FM), ethylene glycol dimethacrylate (EGDMA) as a cross-linker (XL), and azobisisobutyronitrile (AIBN) as an initiator (I) and acetonitrile (ACN) as a porogenic solvent. Non-imprinted polymer (NIP) which serves as a “control” was also synthesized simultaneously under the same condition without the addition of MA molecules. Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM) were used to characterize the imprinted and nonimprinted polymer to explain the structural and morphological characteristics of the 4-VPMIP and surface NIP. The results obtained from SEM depicted that the polymers were irregularly shaped microparticles. Moreover, MIPs surfaces had cavities and were rougher than NIP. In addition, all particle sizes were less than 40 µm in diameter. The IR spectra of 4-VPMIPs before washing MA were a little different from NIP, while 4-VPMIP after elution had a spectrum that was almost identical to the NIP spectrum. The adsorption kinetics, isotherms, competitive adsorption, and reusability of 4-VPMIP were investigated. 4-VPMIP showed good recognition selectivity as well as enrichment and separation abilities for MA in the extract of human urine with satisfactory recoveries. The results obtained in this research imply that 4-VPMIP might be used as a sorbent for MA solid-phase extraction (MISPE), for the exclusive extraction of MA in human urine.

Deodorization of vegetable oils may introduce potentially carcinogenic, as well as genotoxic contaminants, generating health risks for consumers. However, the deodorization step of the refining process leads to the formation of 3-monochloro-1,2-propanediol (3-MCPD). 3-MCPD has been classified as potentially carcinogenic to humans by the World Health Organization (WHO). The purpose of this study was to optimize recently updated oil treatment techniques using Instant Controlled Pressure Drop (DIC) to improve 3-MCPD elimination in edible palm oil. Based on the central composite (CCD-DoE), response surface methodology (RSM) was developed to find the best combination of two variables at five levels to remove 3-MCPD from the palm oil. Samples of palm oil were split into two groups. The first group was treated only by the traditional method, including refining, degumming, deacidification, decolorization, deodorization, dehydration, filtration, and dewaxing processes. The second group was first treated by the traditional method, followed by the DIC technique during different periods at various temperatures and pressures. In the experiment, the effect of 3-MCPD removal in palm oil was examined by varying the oil inlet pressure and reaction time from 200 to 325 kPa and from 8.66 to 26.34 s/cycle, respectively. The 3D surface graphs showed that the optimum reduction of 3-MCPD occurs with a reaction time of 26.34s and a pressure value of 413 kPa. Samples of palm oil were analyzed using a GC-MS/MS method to determine 3-MCPD concentrations. It was found that the DIC technology reduces oil contamination with 3-MCPD when used after the traditional oil treatment process.

The aqueous extract of red algae was used for bio-inspired manufacturing of cobalt oxide nanoparticles (Co3O4NPs) and for antioxidant, antibacterial, hemolytic potency, and anticancer activity. Typical, characterization techniques include UV-Vis, SEM, EDAX, TEM, FTIR, XRD, and TGA. Using an X-ray diffraction assay, the size of the Co3O4NPs crystal was determined to range from 23.2 to 11.8 nm. Based on TEM and SEM pictures, biosynthesized Co3O4NPs’ had a homogeneous spherical morphology with a 28.8 to 7.6 nm average diameter. Furthermore, Co3O4NPs biological properties were investigated, including determining the antibacterial potency using the zone of inhibition (ZOI) method and determining the minimal inhibitory concentration (MIC). The antibacterial activity of Co3O4NPs was higher than that of the ciprofloxacin standard. Alternatively, scavenging of DPPH free radical investigation was carried out to test the antioxidant capacitance of Co3O4NPs, revealing significant antioxidant ability. The biosynthesized Co3O4NPs have a dose-dependent effect on erythrocyte viability, indicating that this technique is harmless. Furthermore, bioinspired Co3O4NPs effectively against HepG2 cancer cells (IC50: 201.3 μg/ml). Co3O4NPs would be a therapeutic aid due to their antioxidant, antibacterial, and anticancer properties.