Extraction of Phthalate Esters in Environmental Water Samples Using Layered-Carbon Magnetic Hybrid Material as Adsorbent Followed by Their Determination with HPLC
Abstract:In this paper, a layered-carbon-Fe 3 O 4 (LC-Fe 3 O 4 ) hybrid material was synthesized through a facile one-pot solvothermal method and used as the adsorbent for the preconcentration of some phthalate esters (dimethyl phthalate, diethyl phthalate, diallyl phthalate, diisobutyl phthalate and benzyl butyl phthalate) in water samples. The effects of the adsorbent dosage, extraction time, the solution pH and salinity on the adsorption of the phthalate esters (PAEs) were investigated. The magnetic nanocomposite ad… Show more
“…Meanwhile, the high viscosity of solution will decrease the formation of organic fine droplets, which also lead to the decrease of the extraction efficiency. These two factors accounted for the final decrease of the extraction efficiency . So, salt was not added in the subsequent experiments.…”
Benzoylurea (BU) insecticides have contributed greatly to the output of crops. Their residue in the environment put serious threats on human health and environmental safety. In this study, we have established a new, rapid, and reliable method for the monitoring of typical BU insecticides such as diflubenzuron, flufenoxuron, triflumuron, and chlorfluazuron with dispersive liquid-liquid microextraction prior to HPLC. Chlorobenzene and ethanol were employed as the extraction solvent and disperser solvent, respectively. The possible parameters which would influence the extraction efficiency such as the kinds and volumes of extraction and disperser solvents, extraction time, sample pH, centrifuging time, and salting-out effect were optimized in detail. Under the optimal conditions, the linear range of proposed method was in the range of 1.0-70 μg/L. The detection limits varied from 0.24 to 0.82 μg/L and the precision of the method was <6.5% (RSD, n = 6). The proposed method was validated with real water samples and satisfactory spiked recoveries were achieved. All these results indicate that the proposed method is a low cost, easy to operate, efficient, and sensitive method for the analysis of BU insecticides in water samples.
“…Meanwhile, the high viscosity of solution will decrease the formation of organic fine droplets, which also lead to the decrease of the extraction efficiency. These two factors accounted for the final decrease of the extraction efficiency . So, salt was not added in the subsequent experiments.…”
Benzoylurea (BU) insecticides have contributed greatly to the output of crops. Their residue in the environment put serious threats on human health and environmental safety. In this study, we have established a new, rapid, and reliable method for the monitoring of typical BU insecticides such as diflubenzuron, flufenoxuron, triflumuron, and chlorfluazuron with dispersive liquid-liquid microextraction prior to HPLC. Chlorobenzene and ethanol were employed as the extraction solvent and disperser solvent, respectively. The possible parameters which would influence the extraction efficiency such as the kinds and volumes of extraction and disperser solvents, extraction time, sample pH, centrifuging time, and salting-out effect were optimized in detail. Under the optimal conditions, the linear range of proposed method was in the range of 1.0-70 μg/L. The detection limits varied from 0.24 to 0.82 μg/L and the precision of the method was <6.5% (RSD, n = 6). The proposed method was validated with real water samples and satisfactory spiked recoveries were achieved. All these results indicate that the proposed method is a low cost, easy to operate, efficient, and sensitive method for the analysis of BU insecticides in water samples.
“…The current methods for detecting BBP include the following: high-performance liquid chromatography (HPLC) [ 12 , 13 ]; gas chromatography-mass spectrometry (GC-MS) [ 14 ]; high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS) [ 15 ]; and enzyme-linked immunosorbent assay (ELISA) [ 16 ]. Varieties of immunoassay have attracted the most attention for phthalic acid esters (PAEs) detection due to their cost-effectiveness and high-throughput screening capability [ 17 ], such as the ELISAs for dimethyl phthalate (DMP) [ 18 ]; for dibutyl phthalate (DEP) [ 19 ]; for di-(2-ethylhexyl) phthalate (DEHP) [ 20 ]; the fluorescence polarization immunoassay (FPIA) for dibutyl phthalate (DBP) [ 21 ];the polymerase chain reaction (PCR) immunoassay for DEP [ 22 ]; and electrochemical immunoassays for bis (2-methoxyethyl) phthalate (DMEP) [ 23 ] and DBP [ 24 ].…”
A magnetic-based immunoassay (MBI) combined with biotin-streptavidin amplification was proposed for butyl benzyl phthalate (BBP) investigation and risk assessment. The values of LOD (limit of detection, IC10) and IC50 were 0.57 ng/mL and 119.61 ng/mL, with a detection range of 0.57–24977.71 ng/mL for MBI. The specificity, accuracy and precision are well demonstrated. A total of 36 environmental water samples of urban sewage from Zhenjiang, China, were collected and assessed for BBP contamination. The results show that BBP-positive levels ranged from 2.47 to 89.21 ng/mL, with a positive rate of 77.8%. The health effects of BBP in the urban sewage were within a controllable range, and the ambient severity for health (ASI) was below 1.49. The highest value of AS for ecology (ASII) was 7.43, which indicates a potential harm to ecology. The entropy value of risk quotient was below 100, the highest being 59.47, which poses a low risk to the environment and ecology, indicating that there is a need to strengthen BBP controls. The non-carcinogenic risk of BBP exposure from drinking water was higher for females than that for males, and the non-carcinogenic risk from drinking-water and bathing pathways was negligible. This study could provide an alternative method for detecting BBP and essential information for controlling BBP contamination.
“…Hence, the determination of aromatic esters is essential for controlling their applications as well as their residual amount in environment. Since their concentrations are generally quite low, a preconcentration process is usually needed before the detection . Among various sample pretreatment methods SPME is quite convenient, because it integrates sample separation, concentration, and sample injection into a single step .…”
A polycarbazole film was electrodeposited on a stainless-steel wire from a solution of N,N-dimethylformamide/propylene carbonate (1:9 v/v) containing 0.10 M carbazole and 0.10 M tetrabutylammonium perchlorate. The obtained polycarbazole fiber was immersed into an ionic liquid (1-hydroxyethyl-3-methyl imidazolium bis[(trifluoromethyl)sulfonyl]imide) solution (in dimethylsulfoxide) for 30 min, followed by drying under an infrared lamp. The resulting polycarbazole/ionic liquid fiber was applied to the headspace solid-phase microextraction and determination of aromatic esters by coupling with gas chromatography and flame ionization detection. Under the optimized conditions, the limits of detection were below 61 ng/L (S/N = 3) and the linear ranges were 0.061-500 μg/L with correlation coefficients above 0.9876. The relative standard deviations were below 4.8% (n = 5) for a single fiber, and below 9.9% for multi-fiber (n = 4). This fiber also exhibited good stability. It could be used for more than 160 times of headspace solid-phase microextraction and could withstand a high temperature up to 350°C.
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