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Detection of florfenicol (FF) residues in animal-derived foods, as one of the most widely used antibiotics, is critically important to food safety. The fluorescent molecularly imprinted polymer (MIP) was synthesized by surface-initiated atom transfer radical polymerization technique with poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate) microspheres, 4-vinylpyridine, ethylene glycol dimethacrylate, and FF as the matrix, functional monomer, crosslinker, and template molecule, respectively. Meanwhile, N-S co-doped carbon dot (CD) was synthesized with triammonium citrate and thiourea as precursors under microwave irradiation at 400 W for 2.5 min and then integrated into FF-MIP to obtain CD@FF-MIP. For comparison, non-imprinted polymer (NIP) without FF was also prepared. The adsorption capacity of CD@FF-MIP to FF reached 53.1 mg g-1, which was higher than that of FF-MIP (34.7 mg g-1), whereas the adsorption capacity of NIP was only 17.3 mg g-1. The adsorption equilibrium of three materials was reached within 50 min. Particularly, CD@FF-MIP exhibited an excellent fluorescence quenching response to FF in the concentration range of 3-50 µmol L-1. As a result, CD@FF-MIP was successfully utilized to extract FF in milk samples, which were analyzed by high-performance liquid chromatography. The standard recoveries were 95.8%-98.2%, and the relative standard deviation was 1.6%-4.2%. The method showed the advantages of simple operation, high sensitivity, excellent selectivity, and low cost, and also demonstrated a great application prospect in food detection.
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A carbon dot (CD) was prepared by o-phenylenediamine and water, which showed bright yellow fluorescence under ultraviolet light irradiation (λ = 580 nm), and verified good fluorescence quenching effect on penicillin G sodium (Png-Na). Using methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a crosslinker, and Png-Na as a template, a kind of composite microsphere combining CD and molecularly imprinted polymer (MIP) was synthesized by surface-initiated atomic transfer radical polymerization (SI-ATRP). For reasons of comparison, we also prepared MIP without CD and non-imprinted polymers (NIPs). Through static and dynamic adsorption experiments, the maximum adsorption capacity was 47.05 mg g-1 and the equilibrium time was 30 min. High-performance liquid chromatography (HPLC) was utilized to determine the content of Png-Na in the spiked milk samples. A sensitive, rapid, and simple method for determination of Png-Na in food samples was developed. The utilized approach enabled the quantification of Png-Na within the concentration range 20-1000 µg L-1 (with a limit of detection of 5 µg L-1). The recoveries achieved were in the range 93.3-98.2%, with a relative standard deviation of 1.2-4.2%. The results demonstrated that CD@MIP possessed the capability of specific adsorption and fluorescence detection of Png-Na, enabling simultaneous detection and enrichment of Png-Na in real samples.
Assuntos
Leite , Polímeros Molecularmente Impressos , Animais , Adsorção , Penicilina G , CarbonoRESUMO
The unique structure and ultralow interlayer shear strength give molybdenum disulfide (MoS2) materials a broad prospect for energy savings, economic benefits, and extended operating life of lubrication systems. Herein, we prepared an effective integration strategy to prepare novel small-sized and chemically grafted MoS2 to solve the problems of poor dispersibility and easy agglomeration of MoS2. The MoS2 powder was stripped and oxidized to generate active centers using acid oxidation and high-speed ultrasonic crushing to obtain two different types of alkylamine chemically, covalently grafted, oxidized MoS2 nanosheets as lubricant additives to achieve friction reduction and antiwear. The chemical changes and structural characteristics of different types of alkylamine molecules upon covalent interaction with oxidized MoS2 were investigated in detail by FTIR, XPS, TGA, XRD, and TEM analyses. The results showed that the alkylamine-grafted MoS2 oxide nanosheets had good dispersion in 15# industrial white oil, and friction experiments confirmed that the alkylamine-grafted MoS2 oxide (MoS2-O-OLA) nanosheets exhibited better friction and wear resistance such that, compared with pure 15# industrial white oil, the 0.02 wt % MoS2-O-OLA nanosheets could significantly reduce friction (36.2%) and wear (22.4%). The field-emission scanning electron microscopy (FESEM) and EDS analyses of the wear surface showed that MoS2-O-OLA nanosheets play an important role in improving tribological properties by generating interlayer slippage at the steel ball contact interface, thereby forming surface protection and a uniform oil film.
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The addition of bisphenol A has been frequently used in industrial manufacturing because it imparts plastic products with characteristics such as transparency, durability, and excellent impact resistance. However, its widespread use raises concerns about potential leakage into the surrounding environment, which poses a significant risk to human health. In this study, molecularly imprinted polymers with specific recognition of bisphenol A were synthesized through surface-initiated atom transfer radical polymerization using poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate) as the substrate, bisphenol A as the template molecule, 4-vinylpyridine as the monomer, and ethylene glycol dimethacrylate as the cross-linker. The bisphenol A adsorption capacity was experimentally investigated, and the kinetic analysis of the molecularly imprinted polymers produced an adsorption equilibrium time of 25 min, which is consistent with the pseudo-second-order kinetic model. The results of the static adsorption experiments exhibited consistency with the Langmuir adsorption model, revealing a maximum adsorption capacity of 387.2 µmol/g. The analysis of molecularly imprinted polymers-enriched actual samples using high-performance liquid chromatography demonstrated excellent selectivity for bisphenol A, with a linear range showing 93.4%-99.7% recovery and 1.1%-6.4% relative standard deviation, demonstrating its high potential for practical bisphenol A detection and enrichment applications.
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A carbon dot (CD) was prepared by using tryptophan as a single carbon source and demonstrated its good selective fluorescence quenching effect on tetracycline (TC). The modified metal-organic frameworks (MOF) NH2-MIL-101 was chosen as matrix, doped with CD, molecularly imprinted polymer (MIP) prepared with TC as the template, and finally CD-MOF-MIP complexes (CD@MIP) was synthesized. For comparison, MIP were also prepared without CD as well as non-imprinted polymers and their ability was tested, respectively. CD@MIP is a nanomaterial with bright fluorescence under the irradiation of ordinary UV equipment (λ = 360 nm), which has a fast and stable fluorescence quenching for TC and a good linear relationship for TC in the concentration range 0-400 µmol L-1. The quantum yield of CD@MIP was 12.75% and the 3σ limit of detection (LOD) for CD@MIP was 0.59 µmol L-1. The maximum adsorption capacity of CD@MIP reached 304.6 mg g-1 and the adsorption equilibrium was reached after about 75 min. The adsorption of CD@MIP to tetracycline spiked in milk samples reached 90.0 mg g-1 within 2 h, which was much higher than that of NIP (48.4 mg g-1) under the same conditions, as demonstrated by high performance liquid chromatography (HPLC). The results obtained showed that CD@MIP combined the high adsorption capacity of MOF, the specific adsorption of molecular imprinting and the fluorescence properties of CD, can determine and rapidly removeTC in the environment.
Assuntos
Estruturas Metalorgânicas , Impressão Molecular , Adsorção , Carbono/química , Tetraciclina/análise , Antibacterianos , Impressão Molecular/métodos , Polímeros Molecularmente ImpressosRESUMO
2-Methyl-4-chlorophenoxyacetic acid (MCPA) is one of the most widely used herbicides, so adsorption and detection of MCPA in the environment is critical. Blue fluorescent carbon dot (CD) was synthesized from citric acid and urea, which could be quenched by MCPA. Herein, bifunctional molecularly imprinted polymer (CD@MIP) was prepared on monodisperse poly (glycidyl methacrylate-co-ethylene glycol dimethacrylate) microspheres, with 4-vinylpyridine as the functional monomer, ethylene glycol dimethacrylate as the cross-linking agent, and doped with CD. The enrichment ability of CD@MIP for MCPA and fluorescence detection performance were determined. The maximum adsorption amount of MCPA was 93.9 mg g-1 as determined by isothermal adsorption experiments and was in accordance with the Langmuir adsorption model. The results of the kinetic experiments showed that the adsorption equilibrium reached within 30 min, which possessed a relatively fast adsorption rate and was in accordance with the pseudo-second-order adsorption model. Both MIP without CD and non-imprinted polymers were also fabricated and tested as references. Fluorescence experiments showed good linearity of CD@MIP in the range of 0-80 µmol. The cabbage samples were analyzed by high performance liquid chromatography with a linear range of 0.02-15 µg mL-1, recoveries of 90.5%-98% and low relative standard deviations (RSD, n = 3) of 1.5%-5.9%. CD@MIP with excellent performance provides a feasible practical application in the detection and enrichment of MCPA.