A CuCr-layered double hydroxide nanosheet intercalated with terephthalic acid (TPA/LDH) was introduced as a coating for the in-tube solid phase microextraction (IT-SPME). The coating was placed on ...the inner surface of a stainless steel tube by using two-electrode electrodeposition. The sorbent was characterized by X-ray diffraction, scanning electronic microscopy, and Fourier transform infrared spectroscopy. The TPA/LDH coating, compared to a nitrate-LDH coating, exhibits enhanced extraction efficiency, long lifetime, good mechanical stability, and a large specific surface. The method was used for the extraction, preconcentration, and subsequent HPLC-based determination of dimethyl phthalate (DMP), dibutyl phthalate (DBP), diallyl phthalate (DAP), and diethylhexyl phthalate (DEHP). The effects of pH value of the solution, salt concentration, extraction and desorption conditions, and the effect of the alcohol content of the solution on the extraction efficiency were optimized. Under optimal conditions, the response is linear in the 0.05 to 1000 μg L
−1
ester concentration range, and the limits of detection (at S/
N
= 3) range between 0.01 to 0.1 μg L
−1
. The inter- and intra-assay precisions (RSD%, for
n
= 3) range from 3.8 to 6.8% and from 3.5 to 5.7%, respectively. The method was successfully applied to the determination of four phthalate esters in different beverage samples.
Graphical abstract
A CuCr-layered double hydroxide nanosheet intercalated with terephthalic acid was used as a coating for in-tube solid phase microextraction of some phthalate esters from beverage samples.
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•New biosorbent TPA/CuCr-LDH@bacterial cellulose prepared by in-situ coprecipitation.•The sorbent was applied in µQuEChERS for extraction of multi-class pesticides in vineyard ...soil.•The procedure's greenness was assessed by AGREE and ComplexGAPI protocols.•The analyses were performed by GC-µECD and GCMS techniques.
A novel nanostructure biosorbent comprised of bacterial cellulose (BC) and a Cu-Cr layered double hydroxide (LDH) intercalated with terephthalic acid (TPA) was prepared using the in-situ coprecipitation method. The synthesized TPA/CuCr-LDH@BC sorbent was used in quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction of multiclass pesticides (nine insecticides, five acaricides, one herbicide, and one fungicide) followed by gas chromatography-mass spectrometry. The extraction factors such as type and volume of eluent, sorbent dosage, adsorption and desorption times, sample pH, and salt were optimized. The sorbent was analyzed with field emission scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and adsorption/desorption isotherms to check its chemical structure, crystallinity, and porosity. Matrix effect (15.3–19.6 %), linearity (20–2000 µg/L, r2 > 0.9982), limits of quantification (6–12 µg/L), and enrichment factor (42–65) were calculated. The efficiency and accuracy of the developed method were assessed with the analysis of five vineyard soil samples and the resulting recoveries were in the range of 60–130 % (RSD%=3.5–12.9). The green aspects of the procedure were evaluated by the Complex-GAPI, the AGREE, and the Analytical Eco-Scale tools. This study describes the first-time synthesis of TPA/CuCr-LDH@BC composite and its application as sorbent material for the microextraction of multi-residue pesticides in agricultural soils.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
A novel adsorbent consisting of a composition of carbon dots and CuCr-layered double hydroxides intercalated with l-histidine (C-dots@His/LDHs) was introduced. This adsorbent was electrochemically ...deposited on the inner surface of a capillary copper tube. It was used as an adsorbent for in-tube solid-phase microextraction of chlorophenols (CPs). Separation and measurement of CPs were done by high-performance liquid chromatography-ultraviolet detector. The main parameters which had the most impact on the extraction efficiency and time such as extraction time and flow rate, desorption time and flow rate, ionic strength (salt concentration) and pH were optimized. Calibration curves (0.5–1000 μg L−1) were plotted in real sample (tap water) under optimal conditions which coefficients of determination better than 0.9893 and relative recoveries in the range of 88–120 % were obtained. The limits of detection (S/N = 3) and limits of quantification (S/N = 10) were obtained in the range of 0.1–1.0 μg L−1 and 0.3–3.0 μg L−1, respectively. The intra- and inter-assay precisions (RSD%, n = 3) were better than 5.9 and 8.8 %, respectively.
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•Carbon dot@l-histidine/LDH was synthesized in inner surface of a copper tube.•It was used for in-tube solid phase microextraction of five chlorophenols (CPs).•Separation and determination of the extracted CPs was performed by UV-HPLC.•Effective parameters on the extraction and determination of CPs were optimized.•The method was applied for determination of CPs in water, juice and honey samples.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
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