A core-shell amino-functionalized glycidyl methacrylate magnetic molecularly imprinted polymer (MIP) was synthesized by the suspension polymerization/surface imprinting method and characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), mercury porosimetry, nitrogen gas adsorption–desorption, and elemental analysis. This MIP was used as the sorbent in dispersive solid-phase microextraction (DSPME) of aniline from textile wastewater prior to high-performance liquid chromatography-mass spectrometry (HPLC-MS) measurements. Since aniline is toxic and a probable human carcinogen, its determination in water is of great significance. This is a challenging task because aniline is usually present at trace levels. The effects of different DSPME variables on the preconcentration efficiency have been studied by using the Plackett–Burman screening design of experiments (DoE) followed by response surface methodology optimization using the Box-Behnken design. Thus, DoE enabled the investigation of several variables simultaneously. Under optimized conditions, aniline was effectively and selectively separated by a small amount of the DSPME sorbent and detected in real textile wastewater samples. The method detection limit of 1 ng mL−1 was attained, with good method linearity and acceptable recovery and precision. The results showed that the studied MIP could be a reliable DSPME sorbent for efficiently analyzing trace aniline in real wastewater samples.
Solid-phase extraction (SPE) of eleven ultraviolet filters (UVFs): benzophenone-1 (BP-1); benzophenone-3 (BP-3); benzophenone-4 (BP-4); isoamyl p-methoxycinnamate (IAMC), homosalate (HMS); 4-hydroxybenzophenone (4-HB); 4-methylbenzylidene camphor (4-MBC); octocrylene (OC); octyl dimethyl-p-aminobenzoate (OD-PABA); 2-ethylhexyl-4-methoxycinnamate (EHMC); and avobenzone (AVO), has been optimized using Plackett-Burman design, Box-Behnken design, and Derrindzer desirability function. Of the six SPE variables studied, the most influencing is the type of eluent followed by pH and the methanol content in the rinsing solvent. A method with good analytical performance was obtained by applying optimal SPE conditions and liquid chromatography-tandem mass spectrometry (LC-MS/MS), with the method detection limit ranging from 0.1 to 5 ng/L, recovery from 44% to 99%, and relative standard deviation (RSD) within 19%. This method was used to analyze the content of UVFs in an urban lake (Sava Lake, Serbia). UVFs occurrence, geostatistical distribution, and associated environmental risk are highly dependent on recreational activities. The average concentrations of UVFs ranged from 0.3 to 113 ng/L, and the most present substance was EHMC, followed by 4-MBC and BP-3. The spatial distribution of the risk quotient (RQ = 0.04–1.7) inside the lake is highly correlated with the number of people bathing and swimming. Human exposure through the dermal pathway is higher than ingestion for most UVFs. Monte Carlo simulation of probabilistic risk assessment estimated the percentile P10, P50, P90 of 12.7; 17.3; 47.5 and 20.1; 27.6; 77.5 ng/kg∙day for total human exposure of adults and children, respectively. The sensitivity analysis revealed that the health risk estimate depends mostly on the content of EHMC, HMS, and 4-MBC, while the most influential exposure variables were human body weight and skin surface area. There is no serious concern to human health due to UVFs in the short term; however, a high ecological risk in some parts of the lake is estimated.
Sunscreen products contain ultraviolet (UV) filters. The daily use of benzophenone-type UV filters has led to indirect inputs of benzophenone-4 (BP-4) into the environment. Wastewater treatment plants (WWTP) have proven ineffective in removing benzophenone derivatives, therefore WWTP are classified as major source of BP-4 in surface water. The level of environmental risk due to presence of BP-4 in wastewater was estimated to be moderate to high, whereby dilution factor should be taken into account when considering the ecological risk due to the discharge of wastewater into the recipient.
Pesticides are extensively used in the cultivation and postharvest protection of citrus fruits, therefore continuous monitoring and health risk assessments of their residues are required. This study aimed to investigate the occurrence of pesticide residues on citrus fruits and to evaluate the acute and chronic risk for adults and children. The risk ranking of twenty-three detected pesticides was carried out according to a matrix ranking scheme. Multiple residues were detected in 83% of 76 analyzed samples. In addition, 28% contained pesticides at or above maximum residue levels (MRLs). The most frequently detected pesticides were imazalil, azoxystrobin, and dimethomorph. According to the risk ranking method, imazalil was classified in the high-risk group, followed by prochloraz, chlorpyrifos, azinphos-methyl, tebufenpyrad, and fenpiroximate, which were considered to pose a medium risk. The majority of detected pesticides (74%) posed a low risk. The health risk assessment indicated that imazalil and thiabendazole contribute to acute (HQa) and chronic (HQc) dietary risk, respectively. The HQc was negligible for the general population, while the HQa of imazalil and thiabendazole exceeded the acceptable level in the worst-case scenario. Cumulative chronic/acute risk (HIc/HIa) assessment showed that chronic risk was acceptable in all samples for children and adults, while the acute risk was unacceptable in 5.3% of citrus fruits for adults and 26% of citrus fruits for children. Sensitivity analyses indicated that the ingestion rate and individual body weight were the most influential risk factors.
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