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Packed cartridges have been widely used in solid-phase extraction. However, there are still some drawbacks, such as they are blocked easily and the method is time-consuming. In view of the advantages of monoliths, a monolithic extraction material has been directly synthesized in a glass syringe without any gap between the monolith and syringe inner wall. The monolithic syringe was modified with graphene oxide by loading graphene oxide dispersion onto it. The content of graphene oxide and the surface topography of the monolith have been evaluated by elemental analysis and scanning electron microscopy, respectively, which confirmed the successful modification. This prepared graphene oxide-modified monolithic syringe was directly used as a traditional solid-phase extraction cartridge. As expected, it shows good permeability and excellent capability for the extraction of quaternary ammonium alkaloids. The sample loading velocity (1-6 mL/min) does not affect the recovery. Under the optimal conditions, good linearities ( R = 0.9992-0.9998) were obtained for five quaternary ammonium alkaloids, and the limits of detection and quantification were 0.5-1 and 1-2 μg/L, respectively. The proposed method was successfully applied for the analysis of quaternary ammonium alkaloids in Chinese patent medicine. [ABSTRACT FROM AUTHOR]

A new β-cyclodextrin/graphene oxide hybrid material prepared via a chemical covalent interaction and layer-to-layer assembly was developed as a sorbent for the solid-phase microextraction of fragrance allergens. As a result of its ultra-large surface area, large delocalized π-electron system and abundant hydroxyls, the β-cyclodextrin/graphene oxide-coated fiber could be used to extract particular compounds via strong π–π interactions, van der Waals forces and hydrogen bonding interactions. β-Cyclodextrin with a hydrophobic interior cavity and hydrophilic peripheral face was conducive in extracting the fragrances with hydrophobic and hydrophilic groups. Under the optimized extraction and desorption conditions, the β-cyclodextrin/graphene oxide-coated fiber showed acceptable extraction efficiency for hydrophilic and hydrogen-bonding-donating alcohols. Compared with other methods based on different coating fibers, the proposed fiber obtained wide linear ranges for fragrances with correlation coefficients ranging from 0.9921 to 0.9970, and low limits of detection in the range of 0.050–0.150 μg L−1. The obtained results indicated that the newly developed fiber was a selective, feasible and cost-effective microextraction medium and could be successfully applied for the determination of several fragrances in personal products. [ABSTRACT FROM AUTHOR]

A novel graphene oxide decorated with silver nanoparticles coating on a stainless-steel fiber for solid-phase microextraction was prepared. Scanning electron microscopy and X-ray photoelectron spectroscopy were used to characterize the coating surface and showed that silver nanoparticles were dispersed on the wrinkled graphene oxide surface. Coupled to gas chromatography with flame ionization detection, the extraction abilities of the fiber for polycyclic aromatic hydrocarbons were examined in the headspace solid-phase microextraction mode. The extraction parameters including adsorption time, adsorption temperature, salt concentration, desorption time and desorption temperature were investigated. Under the optimized condition, wide linearity with low limits of detection from 2 to 10 ng/L was obtained. The relative standard deviations for single-fiber repeatability and fiber-to-fiber reproducibility were less than 10.6 and 17.5%, respectively. The enrichment factors were from 1712.5 to 4503.7, showing the fiber has good extraction abilities. Moreover, the fiber exhibited a good stability and could be reused for more than 120 times. The established method was also applied for determination of polycyclic aromatic hydrocarbons in two real water samples and the recoveries of analytes ranged from 84.4-116.3% with relative standard deviations less than 16.2%. [ABSTRACT FROM AUTHOR]

Highlights • A guanidyl functionalized graphene oxide-grafted silica was designed for the extraction of acidic compounds. • Experiment parameters were optimized using the response surface methodology. • The adsorption mechanism was investigated and evaluated. • The proposed method is suitable for the determination of acidic herbicides. Abstract A highly selective and efficient extraction material was synthesized through the functionalization of guanidyl onto the graphene oxide-grafted silica via a simple chemical modification, which was designed and proposed to improve the enrichment capacity for acidic herbicides. The extraction material was confirmed by scanning electron microscopy, Fourier transform infrared spectrometry, X-ray photoelectron spectrometry, thermal gravimetric analyzer and zeta potential analysis. Theoretical adsorption energies, static- and dynamic-state binding experiments, and comparative experiments with various adsorbents were investigated to elucidate the adsorption mechanism. The introduction of guanidyl endowed the sorbent with stronger Lewis base property and electron-donating ability, hence, excellent extraction recoveries for acidic herbicides could be obtained. Besides, electrostatic and π-π interactions were considered as two major driving impetuses in the adsorption process. Single-factor experiment and response surface methodology were utilized for the optimization of extraction and desorption conditions. Under the optimized conditions, the wide linearities were obtained with correlation coefficients ranging from 0.9904 to 0.9980, and the method detection limits were in the range of 0.5–2 μg L−1. The relative standard deviation values of the recoveries of five different extractions were 3.0–7.1%. Coupled with high performance liquid chromatography, the as-proposed method was successfully applied to detect five acidic herbicides in Lycium barbarum (Goji). It turned out that the proposed method provided a promising perspective for the selective extraction and determination of polar acidic compounds in complex samples. [ABSTRACT FROM AUTHOR]

Abstract: A new three‐dimensional graphene oxide‐wrapped melamine foam was prepared and used as a solid‐phase extraction substrate. β‐Cyclodextrin was fabricated onto the surface of three‐dimensional graphene oxide‐wrapped melamine foam by a chemical covalent interaction. In view of a specific surface area and a large delocalized π electron system of graphene oxide, in combination with a hydrophobic interior cavity and a hydrophilic peripheral face of β‐cyclodextrin, the prepared extraction material was proposed for the determination of flavonoids. In order to demonstrate the extraction properties of the as‐prepared material, the adsorption energies were theoretically calculated based on periodic density functional theory. Static‐state and dynamic‐state binding experiments were also investigated, which revealed the monolayer coverage of flavonoids onto the β‐cyclodextrin/graphene oxide‐wrapped melamine foams through the chemical adsorption. 1H NMR spectroscopy indicated the formation of flavonoids–β‐cyclodextrin inclusion complexes. Under the optimum conditions, the proposed method exhibited acceptable linear ranges (2–200 μg/L for rutin and quercetin‐3‐O‐rhamnoside; 5–200 μg/L for quercetin) with correlation coefficients ranging from 0.9979 to 0.9994. The batch‐to‐batch reproducibility (n = 5) was 3.5–6.8%. Finally, the as‐established method was satisfactorily applied for the determination of flavonoids in Lycium barbarum (Goji) samples with relative recoveries in the range of 77.9–102.6%. [ABSTRACT FROM AUTHOR]

An environmental friendly sorbent of polymeric ionic liquids modified graphene oxide-grafted silica (PILs@GO@Sil) was synthesized for solid-phase extraction (SPE) of phenolic acids. The sorbent was prepared via a chemical layer-to-layer fabrication including amidation reaction, surface radical chain-transfer polymerization and in situ anion exchange. After modification with PILs, the silica surface had higher positive potential so that it would exhibit stronger electrostatic interaction for acidic compounds compared with GO@Sil. The adsorption performance of phenolic acids was investigated through the theoretical calculation and static, kinetic state adsorption experiments. Under the optimized conditions, wide linear ranges were obtained with correlation coefficients ranging from 0.9912 to 0.9998, and limits of detection were in the range of 0.20–0.50 μ g L −1 . Compared with other reported methods, the proposed PILs@GO@Sil-SPE-HPLC showed higher extraction efficiency. Finally, the black wolfberry yogurt and urine were analyzed as real samples and good recoveries spiked with standard solution were obtained. [ABSTRACT FROM AUTHOR]

A solid-phase extraction (SPE) method for the efficient analysis of trace phenolic acids (PAs, caffeic acid, ferulic acid, protocatechuic acid, cinnamic acid) in urine was established. In this work, a graphene oxide (GO) coating was grafted onto pure silica to be investigated as SPE material. The prepared GO surface had a layered and wrinkled structure that was rough and well organized, which could provide more open adsorption sites. Owing to its hydrophilicity and polarity, GO showed higher extraction efficiency toward PAs than reduced GO did, in agreement with the theoretical calculation results performed by Gaussian 09 software. The adsorption mechanism of PAs on GO@Sil was also investigated through static state and kinetic state adsorption experiments, which showed a monolayer surface adsorption. Extraction capacity of the as-prepared material was optimized using the response surface methodology. Under the optimized conditions, the as-established method provided wide linearity range (2-50 μg L for protocatechuic acid and 1-50 μg L for caffeic acid, ferulic acid, and cinnamic acid) and low limits of detection (0.25-1 μg L). Finally, the established method was applied for the analysis of urine from two healthy volunteers. The results indicate that the prepared material is a practical, cost-effective medium for the extraction and determination of phenolic acids in complex matrices. [ABSTRACT FROM AUTHOR]

A solid-phase extraction method for the efficient analysis of the excretion-dynamics of flavonoids in urine was established and described. In this work, in situ surface radical chain-transfer polymerization and in situ anion exchange were utilized to tune the extraction performance of poly(1-vinyl-3-hexylimidazolium bromide)-graphene oxide-grafted silica (poly(VHIm + Br − )@GO@Sil). Graphene oxide (GO) was first coated onto the silica using a layer-by-layer fabrication method, and then the anion of poly(VHIm + Br − )@GO@Sil was changed into hexafluorophosphate (PF 6 − ) by in situ anion exchange. The interaction energies between two PILs and four flavonoids were calculated with the Gaussian09 suite of programs. A Box-Behnken design was used for the optimization of four greatly influential parameters after single-factor experiments to obtain more accurate and precise results. Coupled to high performance liquid chromatography, the poly(VHIm + PF 6 − )@GO@Sil method showed acceptable extraction recoveries for the four flavonoids, with limits of detection in the range of 0.1–0.5 μ g L −1 , and wide linear ranges with correlation coefficients (R) ranging from 0.9935 to 0.9987. Under the optimum conditions, the proposed method was applied to analyze the urines collected from a healthy volunteer. The excretion amount-time profiles revealed that 4–15 h was the main excretion time for the detected flavonoids. The results indicated that the newly developed method offered the advantages of being feasible, green and cost-effective, and could be successfully applied to the extraction and enrichment of flavonoids in human body systems allowing the study of the metabolic kinetics. [ABSTRACT FROM AUTHOR]

A class of novel, environmental friendly ionic liquids (ILs) were synthesized by on-fiber preparation strategy and modified on graphene oxide (GO)-coated stainless steel wire, which was used as a solid-phase microextraction (SPME) fiber for efficient enrichment of polycyclic aromatic hydrocarbons (PAHs) and phthalate esters (PAEs). Surface characteristic of the ILs and polymeric-ILs (PILs) fibers with the wave-structure were inspected by scanning electron microscope. The successfully synthesis of bis(trifluoromethanesulfonyl)imide (NTf 2 − )-based ILs were also characterized by energy dispersive spectrometer analysis. Through the chromatograms of the proposed two ILs (1-aminoethyl-3-methylimidazolium bromide (C 2 NH 2 MIm + Br − ), C 2 NH 2 MIm + NTf 2 − ) and two PILs (polymeric 1-vinyl-3-hexylimidazolium bromide (poly(VHIm + Br − )), poly(VHIm + NTf 2 − ))-GO-coated fibers for the extraction of analytes, NTf 2 − -based PIL demonstrated higher extraction capacity for hydrophobic compounds than other as-prepared ILs. Analytical performances of the proposed fibers were investigated under the optimized extraction and desorption conditions coupled with gas chromatography (GC). Compared with the poly(VHIm + Br − )-GO fiber, the poly(VHIm + NTf 2 − )-GO SPME fiber brought wider linear ranges for analytes with correlation coefficient in the range of 0.9852–0.9989 and lower limits of detection ranging from 0.015–0.025 μg L −1 . The obtained results indicated that the newly prepared PILs-GO coating was a feasible, selective and green microextraction medium, which could be suitable for extraction and determination of PAHs and PAEs in potatoes and food-wrap sample, respectively. [ABSTRACT FROM AUTHOR]

A new polyethylene glycol/graphene oxide composite material bonded on the surface of a stainless-steel wire was used for solid-phase microextraction. The layer-by-layer structure increased the adsorption sites of the novel fiber, which could facilitate the extraction of trace compounds. The polyethylene glycol/graphene oxide was characterized by Fourier transform infrared spectroscopy and elemental analysis, which verified that polyethylene glycol was successfully grafted onto the surface of graphene oxide. The performance of the polyethylene glycol/graphene oxide coated fiber was investigated for phenols and phthalate esters coupled with gas chromatography with flame ionization detection under the optimal extraction and desorption conditions, and the proposed method exhibited an excellent extraction capacity and high thermal stability. Wide linear ranges were obtained for the analytes with good correlation coefficients in the range of 0.9966-0.9994, and the detection limits of model compounds ranged from 0.003 to 0.025 μg/L. Furthermore, the as-prepared fiber was used to determine the model compounds in the water and soil samples and satisfactory results were obtained. [ABSTRACT FROM AUTHOR]

In the initial phase of this study, graphene oxide (GO)/silica was fabricated by assembling GO onto the silica particles, and then gold nanoparticles (GNPs) were used to modify the GO/silica to prepare a novel stationary phase for high-performance liquid chromatography. The new stationary phase could be used in both reversed-phase chromatography and hydrophilic interaction liquid chromatography modes. Good separations of alkylbenzenes, isomerides, amino acids, nucleosides, and nucleobases were achieved in both modes. Compared with the GO/silica phase and GNPs/silica phase, it is found that except for hydrophilicity, large π-electron systems, hydrophobicity, and coordination functions, this new stationary phase also exhibited special separation performance due to the combination of 2D GO with zero-dimensional GNPs. [ABSTRACT FROM AUTHOR]