Solid-Phase Microextraction Mediated Solid-Phase Dielectric Barrier Discharge Vapor Generation-Atomic Fluorescence Spectrometry for Sensitive Determination of Mercury in Seawater.

A novel method coupling solid-phase microextraction (SPME) to solid-phase dielectric barrier discharge (SPDBD) vapor generation was proposed and used for the sensitive detection of trace mercury (Hg) in seawater with atomic fluorescence spectrometry (AFS) in this work. The method proposed herein offers the unique advantages of integrating desorption and chemical vapor generation into one step, eliminating the use of elution reagents, and reducing the analysis time. SPME with multiwalled carbon nanotubes (MWCNTs) coated on the glass tube was used to extract Hg2+ in seawater. The Hg2+ was then desorbed and reduced to Hg0 vapor by SPDBD, which was detected by cold vapor AFS. The parameters affecting Hg2+ extraction, desorption, and vapor generation were studied. The detection limit of Hg2+ was 0.0003 µg L-1, and the relative standard deviation at a Hg2+ concentration of 0.05 µg L-1 was 4.4%. This method also has excellent antimatrix interference ability for Hg2+ determination with recoveries between 91.8% and 101.1% in the presence of extremely high concentrations (two million times excess) of coexisting ions. The practicality of this method was also evaluated by analyzing two different certified reference materials of Hg2+ in water and several seawater samples with good spike recoveries (94.0%-107.4%). Compared with solid-phase photothermo-induced vapor generation, this method has higher extraction efficiency and higher desorption efficiency without the assistance of heating as well as a lower detection limit of Hg2+, which is capable of performing trace Hg analysis in seawater.

Monitoring Poly(methyl methacrylate) and Polyvinyl Dichloride Micro/Nanoplastics in Water by Direct Solid-Phase Microextraction Coupled to Gas Chromatography-Mass Spectrometry.

A simple, sustainable, and sensitive monitoring approach of micro/nanoplastics (MNPs) in aqueous samples is crucial since it helps in assessing the extent of contamination and understanding the potential risks associated with their presence without causing additional stress to the environment. In this study, a novel strategy for qualitative and quantitative determination of MNPs in water by direct solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was proposed for the first time. Spherical poly(methyl methacrylate) (PMMA) and irregularly shaped polyvinyl dichloride (PVDC) were used to evaluate the feasibility and performance of the proposed method. The results demonstrated that both PMMA and PVDC MNPs were efficiently extracted by the homemade SPME coating of nitrogen-doped porous carbons (N-SPCs) and exhibited sufficient thermal decomposition in the GC-MS injection port. Excellent extraction performances of N-SPCs coating for MNPs are attributed to hydrophobic cross-linking, electrostatic forcing, hydrogen bonding, and pore trapping. Methyl methacrylate was identified as the marker for PMMA, while 1,3-dichlorobenzene and 1,3,5-trichlorobenzene were the indicators for PVDC. Under the optimal extraction and decomposition conditions, the proposed method exhibited ultrahigh sensitivity, with a limit of detection of 0.0041 µg/L for PMMA and 0.0054 µg/L for PVDC. Notably, a programmed temperature strategy for the GC-MS injector was developed to discriminate and eliminate the potential interferences of intrinsic indicator compounds. Owing to the integration of sampling, extraction, injection, and decomposition into one step by SPME, the proposed method demonstrates exceptional sensitivity, eliminating the necessity for complex sample pretreatment procedures and the use of organic solvents. Finally, the proposed method was successfully applied in the determination of PMMA and PVDC MNPs in real aqueous samples.

Quantitative Determination of Poly(methyl Methacrylate) Micro/Nanoplastics by Cooling-Assisted Solid-Phase Microextraction Coupled to Gas Chromatography-Mass Spectrometry: Theoretical and Experimental Insights.

Determinations of micro/nanoplastics (MNPs) in environmental samples are essential to assess the extent of their presence in the environment and their potential impact on ecosystems and human health. With the aim to provide a sensitive method with simplified pretreatment steps, cooling-assisted solid-phase microextraction (CA-SPME) coupled to gas chromatography-mass spectrometry (GC-MS) is proposed as a new approach to quantify mass concentrations of MNPs in water and soil samples. The herein proposed CA-SPME method offers the unique advantage of integrating the thermal decomposition of MNPs and enrichment of signature compounds into one step. Poly(methyl methacrylate) (PMMA) was used as a model substance to verify the method performance in this work. Theoretical insights demonstrated that pyrolysis is the rate-determining step during the extraction process and that PMMA is effectively decomposed at 350 °C with an estimated incubation time of 13 min. Eight compounds were identified in the pyrolysis products by CA-SPME-GC-MS with the use of a DVB/CAR/PDMS coating, wherein methyl methacrylate was considered as the best indicator and dimethyl 2-methylenesuccinate was selected as the confirmation compound. Under the optimized conditions, the proposed method exhibited wide linearity (0.5-2000 µg for water and 5-1000 µg for soil) and high sensitivity, with limits of detection of 0.014 and 0.28 µg for water and soil, respectively. Finally, the proposed method was successfully applied for determinations of PMMA MNPs in real water and soil samples with satisfactory recoveries attained. The method only required the employment of a filter membrane for water analysis, while soil samples were analyzed directly without any pretreatment. The solvent-free approach, straightforward operation, and high sensitivity of the proposed method show great potential for the analysis of MNPs in different environmental samples.

Methyltrimethoxysilane modified tin dioxide microspheres with hydrophobic networks and abundant adsorbed oxygen for efficient solid-phase microextraction of polychlorinated biphenyls.

Methyltrimethoxysilane (MTMS) modified tin dioxide microspheres (MTMS/SnO2) were prepared by a facile hydrothermal method and heated reflux reaction strategy. The characterization results indicate that the modification of MTMS induced the formation of a hydrophobic network within the composites, while maintaining abundant adsorbed oxygen species. Subsequently, the MTMS/SnO2 microspheres were used as a solid-phase microextraction (SPME) coating for the efficient extraction and sensitive determination of trace polychlorinated biphenyls (PCBs) in aqueous solutions coupled to gas chromatography-mass spectrometry. MTMS/SnO2 coating exhibited superior extraction performances for PCBs compared with commercial SPME and pure SnO2 microspheres coatings, owing to the hydrophobic crosslinking and adsorbed oxygen-enhanced hydrogen bonding. The proposed analytical method presented respectable linearity in the concentration range 0.25-1000 ng L-1, with low limits of detection varying from 0.036 to 0.14 ng L-1 for seven PCBs and excellent precision, with relative standard deviations of 5.7-9.8% for a single fiber and 8.2-13.1% for five fibers. Finally, the proposed method was successfully used for determination of PCBs in real water with recoveries ranging from 75.8 to 115.6%. This study proposed a new type SPME coating of MTMS/SnO2 microspheres, which extended the potential of SnO2 in capturing and determining organic pollutants.

Improved crystal quality and enhanced optical performance of GaN enabled by ion implantation induced high-quality nucleation.

Hetero-epitaxial growth of GaN often leads to high density of threading dislocations, which poses a significant challenge to the promotion of the performance of GaN-based devices. In this study, we address this issue by utilizing an Al-ion implantation pretreatment on sapphire substrates, which induces high-quality regularly arranged nucleation and promotes the crystal quality of GaN. Specifically, we demonstrate that an Al-ion dose of 1013 cm-2 leads to a reduction of full width at half maximum values of (002)/(102) plane X-ray rocking curves from 204.7/340.9 arcsec to 187.0/259.5 arcsec. Furthermore, a systematic investigation of GaN film grown on the sapphire substrate with various Al-ion doses is also performed, and the nucleation layer growth evolution on different sapphire substrates is analyzed. As confirmed by the atomic force microscope results of the nucleation layer, the ion implantation induced high-quality nucleation is demonstrated, which results in the improved crystal quality of the as-grown GaN films. Transmission electron microscope measurement also proves the dislocation suppression through this method. In addition, the GaN-based light-emitting diodes (LEDs) were also fabricated based on the as-grown GaN template and the electrical properties are analyzed. The wall-plug efficiency at 20 mA has risen from 30.7% to 37.4% of LEDs with Al-ion implantation sapphire substrate at a dose of 1013 cm-2. This innovative technique is effective in the promotion of GaN quality, which can be a promising high-quality template for LEDs and electronic devices.

Core-shell structured Fe2O3/CeO2@MnO2 microspheres with abundant surface oxygen for sensitive solid-phase microextraction of polycyclic aromatic hydrocarbons from water.

Core-shell structured Fe2O3/CeO2@MnO2 microspheres were fabricated and used as solid-phase microextraction coating for determination of polycyclic aromatic hydrocarbons (PAHs) in water samples. XPS spectra demonstrated the generation of abundant surface oxygen on Fe2O3/CeO2@MnO2 microspheres, which provided binding sites for enhancement of analyte extraction. Under optimized conditions, the proposed method presented good linearity in the concentration range 0.04-100 ng mL-1, with low limits of detection varying from 0.38 to 3.57 ng L-1 for eight PAHs. Relative standard deviations for a single fiber and five batches of fibers were in the ranges of 4.1-8.2% and 7.1-11.4%, respectively. The proposed method was successfully used for determination of PAHs in real river water samples with recoveries ranging from 87.1 to 115.9%. The proposed method using as-prepared Fe2O3/CeO2@MnO2 microspheres as SPME coating exhibit significant potential for real sample analysis due to its excellent reproducibility, high sensitivity, and good linearity.

Determination of Ferulic Acid in Angelica sinensis by Temperature-Controlled Hydrophobic Ionic Liquids-Based Ultrasound/Heating-Assisted Extraction Coupled with High Performance Liquid Chromatography.

Hydrophilic ionic liquids are often used to extract the active ingredients of medicinal plants, while hydrophobic ionic liquids are rarely used to directly extract solid samples. In this paper, a simple, novel and efficient temperature-controlled hydrophobic ionic liquids-based ultrasound/heating-assisted extraction (TC-ILs-UHAE) procedure coupled with high-performance liquid chromatography (HPLC) was developed and applied to the determination of ferulic acid (FA) in Chinese herbal medicine Angelica sinensis. During the extraction procedure, hydrophobic ionic liquids (ILs) were dispersed into water to form cloudy solution (fine droplets) with the aid of ultrasound and heating simultaneous. After extraction, phase separation was easily achieved by centrifuging at 0 °C. Among all ILs used, 1-butyl-3-methylimidazolium bis(trifluoromethanesulphonyl)imide ([C4mim]NTf2) exhibited the highest extraction ability and the possible extraction mechanism was discussed. Additionally, the synergistic effect of heating and ultrasound on the extraction efficiency was investigated. Under the optimized conditions, a good linearity was observed with correlation coefficient (r) of 0.9995. The limit of detection of FA (LOD, S/N = 3) was 9.6 µg/L and the spiked recoveries of FA for real samples were in the range of 91.67 to 102.00% with relative standard deviation (RSD) lower than 3.87%. Compared with the traditional extraction methods, the proposed method gave the highest yield of FA and had the shortest extraction time. Therefore, this method is a potential simple, green and highly efficient technique and expected to be applied to the extraction of other bioactive ingredients in medicinal plants.

Conductometric acetone vapor sensor based on the use of gold-doped three-dimensional hierarchical porous zinc oxide microspheres.

A versatile nanoprobe for acetone vapor was designed and fabricated. It is based on the use of gold-doped three-dimensional (3D) hierarchical porous zinc oxide microspheres (Au/ZnO HPMSs). The nanoprobe was synthesized by annealing zinc hydroxide carbonate precursor (obtained by a hydrothermal method) doped with gold nanoparticles. The resulting products possess a 3D open framework structure built of 2D porous nanosheets with a nanoporous wormhole-like shape. The microspheres doped with 0.5 mol% gold display a good selectivity towards acetone. The conductometric nanoprobe, typically operated at a voltage of 5 V, can detect sub-ppm levels of acetone, and the detection limit is as low as 0.2 ppm. The response (at a level of up to 100 ppm of acetone at 325 °C) was high (74 ± 1.9), and the response and recovery time are 6 and 3 s, respectively. This superior performance is ascribed (a) to the hierarchical porous ZnO architecture that warrants a large surface area; and (b) to the presence of gold nanoparticles that facilitate the chemisorption and dissociation of gas molecules. Graphical abstract Gold-doped 3D hierarchical porous ZnO microspheres (Au/ZnO HPMSs) architectures assembled by interconnected 2D porous nanosheets structures. The resistive sensor using these Au/ZnO HPMSs demonstrates outstanding acetone vapor sensing behaviors and 0.2 ppm detection limits.

Quantitative Determination of Bulk Molecular Concentrations of ß-Agonists in Pork Tissue Samples by Direct Internal Extractive Electrospray Ionization-Mass Spectrometry.

Rapid quantitative determination of bulk molecular concentration in solid samples without sample pretreatment is demonstrated using the internal extractive electrospray ionization-mass spectrometry (iEESI-MS) analysis of six ß-agonists, including salbutamol (Sal), clenbuterol (Cle), ractopamine (Rac), terbutaline (Ter), tulobuterol (Tul), brombuterol (Bro), in pork tissue samples. Single sample analysis only required 1 min. The linear range of detection was about 0.01-1000 µg/kg (R2 > 0.9994). The limit-of-detection (LOD) varied from 0.002 µg/kg for Sal to 0.006 µg/kg for Tul. Relative standard deviation (RSD) of quantitation was in the range 6.5-11.3%. The analytical results were validated by gas chromatography-mass spectrometry (GC-MS) and high-performance liquid chromatography-mass spectrometry (LC-MS), showing the accuracy rates of 92-105%. The current study extends the power of ambient MS as a method for the quantification of molecules at the surface of solid samples (e.g., in µg/cm2 units) toward the quantification of molecules in bulk sample volume (i.e., in µg/kg units), which is commonly required in food safety control, biomedical analysis, public security, and many other disciplines.

Determination of Polycyclic Aromatic Hydrocarbons in Sediment by Pressure-Balanced Cold Fiber Solid Phase Microextraction.

An improved performance of the cold fiber solid phase microextraction (CF-SPME) technique was accomplished with the use of the pressure-balanced procedure. In order to obtain a pressure-balanced state during extraction at 200 °C, 7 mL of air volume was withdrawn from 10 mL commercial vials, while 15 mL was withdrawn from vials where 5 µL of diethylamine was added as a modifier/displacer. The benefits of the balanced system were demonstrated for determination of polycyclic aromatic hydrocarbons (PAHs) from solid matrixes, including sand and certified sediment samples. Results showed the pressure-balanced procedure enhanced the extraction efficiency of the method, especially for high volatility compounds, as the leakage of analytes was mitigated under sample temperature conditions of 200 °C. Analytical precision was also improved, with relative standard deviations (RSDs) ranging from 4% to 8% for all analytes under study. For the determination of PAHs in certified sediment samples, pressure-balanced CF-SPME yielded more accurate results in comparison to nonpressure-balanced CF-SPME. The proposed methodology provided the additional benefit of improved recoveries at lower pressures.

Determination of fatty acids in soil samples by gas chromatography with mass spectrometry coupled with headspace solid-phase microextraction using a homemade sol-gel fiber.

Through the use of a homemade sol-gel-derived fiber, a headspace solid-phase microextraction technique coupled to gas chromatography with mass spectrometry was developed for the determination of fatty acids with long, even-numbered carbon chains (C12 -C24 ) in soil samples. The experimental parameters such as reaction time, temperature, and ionic strength that might affect derivatization, extraction, and desorption were investigated. Under the optimized conditions, the linearity of the method ranged from 0.1 to 100 mg/L with a correlation coefficient >0.997. The limit of detection values based on a signal-to-noise ratio of 3:1 were determined with the concentration from 0.39 to 39.4 µg/L. The recoveries of the method for the soil samples were from 91.15 to 108.1%. This developed method using a homemade fiber showed a higher sensitivity than that using a commercial polydimethylsiloxane fiber and was also for the analysis of real soil samples from the Paomaling geological park of China.

Yellow luminescence of polar and nonpolar GaN nanowires on r-plane sapphire by metal organic chemical vapor deposition.

We have grown horizontal oriented, high growth rate, well-aligned polar (0001) single crystalline GaN nanowires and high-density and highly aligned GaN nonpolar (11-20) nanowires on r-plane substrates by metal organic chemical vapor deposition. It can be found that the polar nanowires showed a strong yellow luminescence (YL) intensity compared with the nonpolar nanowires. The different trends of the incorporation of carbon in the polar, nonpolar, and semipolar GaN associated with the atom bonding structure were discussed and proved by energy-dispersive X-ray spectroscopy, suggesting that C-involved defects are the origin responsible for the YL in GaN nanowires.

Development of an accurate hand-held sensing platform for nitrite detection based on nitrogen-doped carbon dots.

As is well known, excessive nitrite can seriously pollute the environment and can harm human health. Although existing methods can be used to determine nitrite content, they still have some drawbacks, such as relatively complicated operation and expensive equipment. Herein, a hand-held sensing platform (HSP) for NO2- determination was developed. First, ammonia-rich nitrogen-doped carbon dots with orange-yellow emission were designed and synthesised, which were suitable as fluorescent probes because of their good optical properties and stability. Then, the HSP based on fluorescence using photoelectric conversion technology was designed and manufactured using three-dimensional printing technology. Under optimum conditions, the voltage (V/V0) of the proposed HSP showed good linearity for NO2- detection in the range of 10-500 µM, with a detection limit of 1.95 µM. This portable sensor showed good stability, accuracy and reliability in detecting actual water and meat samples, which may ensure food safety in practical applications. Moreover, the HSP is compact, portable and easily assembled and is suitable for on-site real-time detection, which shows great application potential and prospects.

Cellulose Nanocrystals Induced Loose and Porous Graphite Phase Carbon Nitride/Porous Carbon Composites for Capturing and Determining of Organochlorine Pesticides from Water and Fruit Juice by Solid-Phase Microextraction.

Herein, novel, loose, and porous graphite phase carbon nitride/porous carbon (g-C3N4@PC) composites were prepared by decorating cellulose nanocrystals (CNCs). The characterization results demonstrate that the as-prepared composites presented high specific surface areas, porous structures, and abundant chemical groups, with the modification of CNCs. In view of the unique advantages, g-C3N4@PC was used as the coating material for the solid-phase microextraction (SPME) of organochlorine pesticides (OCPs) in water and juice samples. The g-C3N4@PC-coated fibers showed better extraction efficiencies than commercial fibers (100/7 µm PDMS and PA) toward the OCPs, with the enrichment factors of the g-C3N4@PC-coated fibers 5-30 times higher than the latter. Using a gas chromatography-mass spectrometry (GC-MS) instrument, the g-C3N4@PC-coated fibers exhibited a gratifying analytical performance for determining low concentrations of OCPs, with a wide linear range (0.1-1600 ng L-1 for water; 0.1-1000 ng L-1 for juice), low limits of detection (0.0141-0.0942 ng L-1 for water; 0.0245-0.0777 ng L-1 for juice), and good reproducibility and repeatability in optimal conditions. The established method showed good sensitivity and recovery in the determination of OCPs in the water and fruit juice samples, which displayed broad prospects for analyzing organic pollutants from environmental samples.

High-throughput profiling volatiles in edible oils by cooling assisted solid-phase microextraction technique for sensitive discrimination of edible oils adulteration.

In this study, a cooling assisted solid-phase microextraction technique (CA-SPME) was proposed and used for identifying volatile and semi-volatile compounds in edible oil innovatively coupled to gas chromatography-mass spectrometry. Compared with regular SPME technique, CA-SPME presented significantly higher extraction efficiencies for analytes in edible oil due to its synergistic effect of heating and cooling. After optimization of the extraction conditions including heating temperature, cooling temperature, extraction time, and added amount of edible oil, thirty-eight, thirty-six, twenty-nine, and thirty-three kinds of compounds in peanut oil, olive oil, canola oil, and soybean oil were successfully identified, respectively, using DVB/CAR/PDMS coating with extraction time of 30 min and edible oil amounts of 20 µL. Principal component analysis, partial least squares discriminant analysis, and hierarchical clustering analysis (HCA) were performed to evaluate the potential of proposed method in discriminating edible oils adulteration (peanut oil adulterated with canola oil, peanut oil adulterated with soybean oil, olive oil adulterated with canola oil) subsequently. Results demonstrated that the method was useful in successful discrimination of pure and adulterated edible oils with adulteration percentages ranging from 0.5 to 10%. Furthermore, volatiles contributing to classifications between pure and adulterated edible oils were also illustrated based on variable importance for the projection analysis and distributions of volatiles in HCA heatmaps. The proposed method provided a novel strategy for sensitive detection of edible oil adulteration without any other sample pretreatment.

Polyacrylic Acid Functionalized Biomass-Derived Carbon Skeleton with Highly Porous Hierarchical Structures for Efficient Solid-Phase Microextraction of Volatile Halogenated Hydrocarbons.

In this study, polyacrylic acid functionalized N-doped porous carbon derived from shaddock peels (PAA/N-SPCs) was fabricated and used as a solid-phase microextraction (SPME) coating for capturing and determining volatile halogenated hydrocarbons (VHCs) from water. Characterizations results demonstrated that the PAA/N-SPCs presented a highly meso/macro-porous hierarchical structure consisting of a carbon skeleton. The introduction of PAA promoted the formation of polar chemical groups on the carbon skeleton. Consequently, large specific surface area, highly hierarchical structures, and abundant chemical groups endowed the PAA/N-SPCs, which exhibited superior SPME capacities for VHCs in comparison to pristine N-SPCs and commercial SPME coatings. Under the optimum extraction conditions, the proposed analytical method presented wide linearity in the concentration range of 0.5-50 ng mL-1, excellent reproducibility with relative standard deviations of 5.8%-7.2%, and low limits of detection varying from 0.0005 to 0.0086 ng mL-1. Finally, the proposed method was applied to analyze VHCs from real water samples and observed satisfactory recoveries ranging from 75% to 116%. This study proposed a novel functionalized porous carbon skeleton as SPME coating for analyzing pollutants from environmental samples.

Carbon Dot-Decorated Graphite Carbon Nitride Composites for Enhanced Solid-Phase Microextraction of Chlorobenzenes from Water.

In this work, carbon dot-decorated graphite carbon nitride composites (CDs/g-C3N4) were synthesized and innovatively used as a SPME coating for the sensitive determination of chlorobenzenes (CBs) from water samples, coupled with gas chromatography-mass spectrometry. The CDs/g-C3N4 coating presented superior extraction performance in comparison to pristine g-C3N4, owing to the enhancement of active groups by CDs. The extraction capacities of as-prepared SPME coatings are higher than those of commercial coatings due to the functions of nitrogen-containing and oxygen-containing group binding, π-π stacking, and hydrophobic interactions. Under optimized conditions, the proposed method exhibits a wide linearity range (0.25-2500 ng L-1), extremely low detection of limits (0.002-0.086 ng L-1), and excellent precision, with relative standard deviations of 5.3-9.7% for a single fiber and 7.5-12.6% for five fibers. Finally, the proposed method was successfully applied for the analysis of CBs from real river water samples, with spiked recoveries ranging from 73.4 to 109.1%. This study developed a novel and efficient SPME coating material for extracting organic pollutants from environmental samples.

Lotus-like Ni@NiO nanoparticles embedded porous carbon derived from MOF-74/cellulose nanocrystal hybrids as solid phase microextraction coating for ultrasensitive determination of chlorobenzenes from water.

Lotus-like Ni@NiO embedded porous carbons (Ni@NiO/PCs) were fabricated by pyrolysis of MOF-74/cellulose nanocrystal hybrids, and used as a solid phase microextraction (SPME) coating for ultrasensitive determination of chlorobenzenes (CBs) from water combined with gas chromatography-mass spectrometry. Owing to its abundant chemical groups, high porosity, and excellent thermal stability, the as-prepared Ni@NiO/PCs presented superior extraction performance compared to commercial SPME coatings. Notably, Ni@NiO/PCs derived from MOF-74/CNC hybrids presented higher extraction efficiencies towards CBs than that derived from pristine CNC and MOF-74 due to the formation of micro/mesopores and more abundant oxygen-containing groups. Under the optimum extraction conditions, the proposed analytical method presented wide linearity range (0.5-1500 ng L-1), ultra-low detection of limit (0.005-0.049 ng L-1), and excellent precision with relative standard deviations of 4.7-9.2% for a single fiber and 8.8-10.9% for 5 fibers, and long lifetime (≥160 times). The proposed analytical method was finally applied for determination of CBs from real water samples, and the recoveries were in the range of 93.2-116.8% towards eight CBs. This study delivered a novel and efficient sorbent as SPME coating to extraction and determination of CBs from water.

Facile fabrication of magnetic covalent organic frameworks for magnetic solid-phase extraction of diclofenac sodium in milk.

A robust magnetic solid-phase extraction (MSPE) method based on magnetic covalent organic framework (MCOF) coupled with high-performance liquid chromatography (HPLC)-ultraviolet (UV)/mass spectrometry (MS) was proposed for the determination of trace diclofenac sodium (DS) in milk. The prepared MCOF exhibited high extraction efficiency, which can be attributed to its high specific surface area as well as strong π-π and hydrophobic interactions between MCOF and DS. In addition, the potential influencing factors, including sample volume, adsorbent dosage, extraction time, and elution parameters, were fully estimated. The experimental results demonstrated that the established method was sensitive for the quantification of DS with high accuracy. Remarkably, the detection limit of DS was found to be 10 ng/kg under the optimal conditions. More impressively, the developed method was successfully applied to monitor trace DS in milk, demonstrating its outstanding durability and practical potential as an appealing method to regular monitor trace pharmaceutical contaminants in real food samples.

Comparative Research of GaN Growth Mechanisms on Patterned Sapphire Substrates with Sputtered AlON Nucleation Layers.

The utilization of sputtered AlN nucleation layers (NLs) and patterned sapphire substrates (PSSs) could greatly improve GaN crystal quality. However, the growth mechanism of GaN on PSSs with sputtered AlN NLs has not been thoroughly understood. In this paper, we deposited AlON by sputtering AlN with O2, and we found that the variation of thickness of sputtered AlON NLs greatly influenced GaN growth on PSSs. (1) For 10 nm thin AlON sputtering, no AlON was detected on the cone sidewalls. Still, GaN nucleated preferably in non-(0001) orientation on these sidewalls. (2) If the thickness of the sputtered AlON NL was 25 nm, AlON formed on the cone sidewalls and flat regions, and some small GaN crystals formed near the bottom of the cones. (3) If the sputtered AlON was 40 nm, the migration ability of Ga atoms would be enhanced, and GaN nucleated at the top of the cones, which have more chances to grow and generate more dislocations. Finally, the GaN growth mechanisms on PSSs with sputtered AlON NLs of different thicknesses were proposed.