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1.
Mikrochim Acta ; 191(3): 145, 2024 Feb 19.
Artigo em Inglês | MEDLINE | ID: mdl-38372818

RESUMO

A direct electrochemical sensor based on covalent organic frameworks (COFs)/platinum nanoparticles (PtNPs) composite was fabricated for the detection of ofloxacin (OFX) in water. Firstly, the COF material was synthesized via the condensation reaction of 1,3,5-tris(4-aminophenyl)benzene (TAPB) with terephthalaldehyde (TPA) and integrated with PtNPs by in situ reduction. Then, TAPB-TPA-COFs/PtNPs composite was loaded onto the surface of the glassy carbon electrode (GCE) by drip coating to construct the working electrode (TAPB-TPA-COFs/PtNPs/GCE). The electrochemical performance of TAPB-TPA-COFs/PtNPs/GCE showed a significant improvement compared with that of TAPB-TPA-COFs/GCE, leading to a 3.2-fold increase in the electrochemical signal for 0.01 mM OFX. Under optimal conditions, the TAPB-TPA-COFs/PtNPs/GCE exhibited a wide linear range of 9.901 × 10-3-1.406 µM and 2.024-15.19 µM with a detection limit of 2.184 × 10-3 µM. The TAPB-TPA-COFs/PtNPs/GCE-based electrochemical sensor with excellent performance provides great potential for the rapid and trace detection of residual OFX.

2.
Nanomaterials (Basel) ; 14(2)2024 Jan 17.
Artigo em Inglês | MEDLINE | ID: mdl-38251169

RESUMO

Dielectric materials with superb thermal and electrical properties are highly desired for high-voltage electrical equipment and advanced electronics. Here, we propose a novel strategy to improve the performance of epoxy composites by employing boron nitride nanosheets (BNNSs) and γ-glycidyl ether oxypropyl sesimoxane (G-POSS) as functional fillers. The resultant ternary epoxy composites exhibit high electrical resistivity (1.63 × 1013 Ω·cm) and low dielectric loss (<0.01) due to the ultra-low dielectric constants of cage-structure of G-POSS. In addition, a high thermal conductivity of 0.3969 W·m-1·K-1 is achieved for the epoxy composites, which is 114.66% higher than that of pure epoxy resin. This can be attributed to the high aspect ratio and excellent thermally conductive characteristics of BNNSs, promoting phonon propagation in the composites. Moreover, the epoxy composite simultaneously possesses remarkable dynamic mechanical properties and thermal stability. It is believed that this work provides a universal strategy for designing and fabricating multifunctional composites using a combination of different functional fillers.

3.
Chemosphere ; 331: 138842, 2023 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-37142102

RESUMO

In this work, a kind of multifunctional magnetic plasmonic photocatalyst was prepared by a green and efficient process. Magnetic mesoporous anatase titanium dioxide (Fe3O4@mTiO2) was synthesized by microwave-assisted hydrothermal, and Ag NPs were simultaneously in-situ grown on Fe3O4@mTiO2 (Fe3O4@mTiO2@Ag), graphene oxide (GO) was then wrapped on Fe3O4@mTiO2@Ag (Fe3O4@mTiO2@Ag@GO) to increase its adsorption capacity for fluoroquinolone antibiotics (FQs). Owing to the localized surface plasmon resonance (LSPR) effect of Ag, as well as the photocatalytic capacity of TiO2, a multifunctional platform based on Fe3O4@mTiO2@Ag@GO was constructed for adsorption, surface-enhanced Raman spectroscopy (SERS) monitoring and photodegradation of FQs in water. The quantitative SERS detection of norfloxacin (NOR), ciprofloxacin (CIP), and enrofloxacin (ENR) was demonstrated with LOD of 0.1 µg mL-1, and the qualitative analysis was confirmed by density functional theory (DFT) calculation. The photocatalytic degradation rate of NOR over Fe3O4@mTiO2@Ag@GO was about 4.6 and 1.4 times faster than that of Fe3O4@mTiO2 and Fe3O4@mTiO2@Ag, indicating the synergetic effects of Ag NPs and GO, the used Fe3O4@mTiO2@Ag@GO can be easily recovered and recycled for at least 5 times. Thus, the eco-friendly magnetic plasmonic photocatalyst provided a potential solution for the removal and monitoring of residual FQs in environmental water.


Assuntos
Fluoroquinolonas , Água , Fotólise , Adsorção , Norfloxacino , Antibacterianos , Fenômenos Magnéticos
4.
RSC Adv ; 13(15): 10135-10143, 2023 Mar 27.
Artigo em Inglês | MEDLINE | ID: mdl-37006373

RESUMO

Internal standard molecule 4-mercaptobenzoic acid (4-MBA) embedded Au core-Ag shell nanorods (Au-MBA@Ag NRs) were prepared by a seed-mediated growth method, then loaded on octahedral MIL-88B-NH2 to obtain a novel ratiometric SERS substrate of Au-MBA@Ag NRs/PSS/MIL-88B-NH2 (AMAPM) for detecting rhodamine 6G (R6G) in chili powder. The porous structure and excellent adsorption ability of MIL-88B-NH2, allowed for increased loading of Au-MBA@Ag NRs, thereby shortening the distance between adsorbed R6G and the "hot spot" resulting from local surface plasmon resonance (LSPR) of Au-MBA@Ag NRs. Based on the SERS characteristic peak ratio of R6G to 4-MBA, the ratiometric SERS substrate displayed improved accuracy and excellent performance for R6G detection, with a wide linear range of 5-320 nM and a low detection limit of 2.29 nM as well as fine stability, reproducibility and specificity. The proposed ratiometric SERS substrate offered a simple, fast and sensitive sensing strategy for R6G detection in chili powder, which demonstrated potential applications in food safety and the analysis of trace analytes in complex matrices.

5.
Mikrochim Acta ; 190(2): 50, 2023 01 11.
Artigo em Inglês | MEDLINE | ID: mdl-36629926

RESUMO

Poor selectivity and reusability of Au/Ag nanostructures are the main challenges for surface-enhanced Raman spectroscopy (SERS) in real sample detection. Herein, a novel specific and reusable three-dimensional (3D) SERS sensor with dual functions of selective trapping and photocatalytic degradation was designed. Firstly, Au-Ag bimetallic nanoparticles decorated silicon nanowires array (SiNWs-AuAg) were prepared as 3D SERS substrate. Then, silicon-based inorganic-framework molecularly imprinted TiO2 (TiO2@SiMIP) was synthesized and immobilized on SiNWs-AuAg by using rhodamine 6G (R6G) as template molecule. Owing to the excellent SERS performance of SiNWs-AuAg and the specific affinity of TiO2@SiMIP to template molecule, the prepared SERS sensor enables sensitive and selective detection of R6G in food samples with a limit of detection (LOD) of 0.27 nM. In addition, due to the photocatalysis of TiO2 and the stability of silicon-based inorganic framework, the residual templates in TiO2@SiMIP can be completely removed by UV irradiation, and the imprinted cavity of regenerated sensors still maintained good selectivity after regeneration by UV irradiation.


Assuntos
Nanopartículas Metálicas , Nanopartículas Metálicas/química , Silício/química , Análise Espectral Raman/métodos , Titânio/química
6.
IEEE Trans Pattern Anal Mach Intell ; 45(2): 2384-2399, 2023 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-35412976

RESUMO

Small and cluttered objects are common in real-world which are challenging for detection. The difficulty is further pronounced when the objects are rotated, as traditional detectors often routinely locate the objects in horizontal bounding box such that the region of interest is contaminated with background or nearby interleaved objects. In this paper, we first innovatively introduce the idea of denoising to object detection. Instance-level denoising on the feature map is performed to enhance the detection to small and cluttered objects. To handle the rotation variation, we also add a novel IoU constant factor to the smooth L1 loss to address the long standing boundary problem, which to our analysis, is mainly caused by the periodicity of angular (PoA) and exchangeability of edges (EoE). By combing these two features, our proposed detector is termed as SCRDet++. Extensive experiments are performed on large aerial images public datasets DOTA, DIOR, UCAS-AOD as well as natural image dataset COCO, scene text dataset ICDAR2015, small traffic light dataset BSTLD and our released S 2 TLD by this paper. The results show the effectiveness of our approach. The released dataset S 2 TLD is made public available, which contains 5,786 images with 14,130 traffic light instances across five categories.

7.
Nanoscale ; 14(21): 7913-7918, 2022 Jun 01.
Artigo em Inglês | MEDLINE | ID: mdl-35593223

RESUMO

Interfacial heating is the most obvious feature that distinguishes the novel solar driven interfacial heating from the traditional solar heating technology, and it is also a key factor in promoting solar energy utilization and vapor generation performance. However, the inherent trade-off between water supply and the interfacial heating performance of photothermal materials has rarely been investigated. Herein, an all-in-one designed bilayer evaporator consisting of a top solar absorber (Fe3O4@PDA-SA) and a bottom water transport layer (SA) is reported. This bilayer structured aerogel can provide good thermal insulation, effective water transmission channels, and reliable light absorbance, and perform well as a high-quality solar steam evaporator with the evaporation rate of approximately 1.517 kg m-2 h-1 and the evaporation efficiency of approximately 98.27% under 1 kW m-2 solar illumination. Most importantly, we can control the pore size of the bottom layer by a simple free water evaporation method, so as to manipulate the water transport capacity of materials. There is flexibility to change the water content of the light-absorbing structure and further explore the influence of water supply on the interfacial heating performance of the evaporator, which provides more possibilities for the design and preparation of high-quality solar steam evaporators.

8.
Mikrochim Acta ; 188(10): 354, 2021 09 27.
Artigo em Inglês | MEDLINE | ID: mdl-34570272

RESUMO

A capillary-based SERS sensor was fabricated for ultrasensitive and selective detection of Hg2+ in water. Au@Ag core-shell NPs embedded with 4-mercaptobenzoic acid (4-MBA) (Au@4-MBA@Ag) were prepared by a seed growth method and fixed on the inner wall of the glass capillary to obtain the sensor. Owing to the amalgamation between Ag and Hg, the capillary-based SERS sensor can specifically recognize the reduced Hg2+ without any recognition element, and the resulted Ag/Hg amalgam can weaken the SERS activity of Ag shell; thus, the SERS intensity of the embedded 4-MBA at 1075 cm-1 gradually decreased with the increase of Hg2+ concentration. Under the optimum condition, the fabricated sensor can sensitively determine Hg2+ in water with a limit of detection (LOD) as low as 0.03 nM. The capillary-based SERS sensor offers the advantages of simple preparation, superior stability, and high selectivity, which is promising for rapid and on-site detection of Hg2+ in water combined with a portable Raman device.


Assuntos
Ouro
9.
J Food Sci ; 86(6): 2264-2275, 2021 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-33948957

RESUMO

The objective of this research was to identify and characterize the chemical compounds that exhibited monosodium glutamate (MSG)-like taste in the hydrolyzed bone meal produced by using flavourzyme. The free amino acids and peptides in the bone meal hydrolysate were analyzed. The results showed that the glutamic acid and the aspartic acid in the bone meal increased by 13.1 times and 14.2 times, respectively, after the flavourzyme hydrolysis. The peptides' isolation identified six MSG-like peptides in the hydrolysate, including APGPVGPAG, DAINWPTPGEIAH, FLGDEETVR, GVDEATIIEILTK, PAGPVGPVG, and VAPEEHPTL, which should contribute to the taste. The human sensory evaluation results indicated that the six peptides showed MSG-like taste, and the electronic tongue analysis indicated that the six peptides showed sourness, saltiness, bitterness, and astringency. The findings of this study demonstrated that the MSG-like taste of the bone meal hydrolysate should be attributed to the generation of MSG-like amino acids and peptides from the flavourzyme hydrolysis. PRACTICAL APPLICATION: The manuscript describes the umami compounds in the bone meal hydrolysate. The findings from this study should further confirm the feasibility of using bone meal to prepare meat-flavor essence and provide a better understanding of preparing bio-source flavoring peptides, which is very important to the artificial meat development and gene breeding.


Assuntos
Minerais/química , Peptídeos/química , Paladar , Aminoácidos/análise , Produtos Biológicos/química , Nariz Eletrônico , Aromatizantes/análise , Manipulação de Alimentos , Humanos , Hidrólise , Carne/análise , Glutamato de Sódio/química
10.
Appl Microbiol Biotechnol ; 105(5): 2017-2032, 2021 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-33555361

RESUMO

In the present study, the complete mitogenome of Turbinellus floccosus was sequenced, assembled, and compared with other basidiomycete mitogenomes. The mitogenome of T. floccosus consists of a circular DNA molecule, with a size of 62,846 bp. Gene arrangement analysis indicated that large-scale gene rearrangements occurred in the levels of family and genus of basidiomycete species, and the mitogenome of T. floccosus contained a unique gene order. A significant correlation between the number of introns and the mitochondrial genome size of Basidiomycota were detected (P < 0.01). A total of 896 introns were detected in the core protein-coding genes (PCGs) of 74 basidiomycete species, and the cox1 gene was the largest host gene of basidiomycete introns. Intron position class (Pcls) P383 in the cox1 gene was the most common intron in Basidiomycota, which distributed in 40 of 74 basidiomycete species. In addition, frequent intron loss/gain events were detected in basidiomycete species. More than 50% of bases around insertion sites (- 15 bp to 15 bp) of Pcls from different species were conservative, indicating site preferences of intron insertions in Basidiomycota. Further analysis showed that 76.09% of introns tended to insert downstream to a T base in Basidiomycota. Phylogenetic analysis for 74 basidiomycetes indicated mitochondrial genes are effective molecular markers for phylogeny of basidiomycetes. The study served as the first report on the mitogenome from the family Gomphaceae, which will help to understand the intron origin and evolution in Basidiomycota. KEY POINTS: • The mitogenome of Turbinellus floccosus had a unique gene arrangement. • Intron loss/gain events were detected in the 74 basidiomycete species. • Introns tend to insert downstream of a T base in basidiomycete mitogenomes.


Assuntos
Basidiomycota , Genoma Mitocondrial , Basidiomycota/genética , Rearranjo Gênico , Íntrons , Filogenia
11.
Artigo em Inglês | MEDLINE | ID: mdl-32956057

RESUMO

The Deep learning of optical flow has been an active area for its empirical success. For the difficulty of obtaining accurate dense correspondence labels, unsupervised learning of optical flow has drawn more and more attention, while the accuracy is still far from satisfaction. By holding the philosophy that better estimation models can be trained with betterapproximated labels, which in turn can be obtained from better estimation models, we propose a self-taught learning framework to continually improve the accuracy using self-generated pseudo labels. The estimated optical flow is first filtered by bidirectional flow consistency validation and occlusion-aware dense labels are then generated by edge-aware interpolation from selected sparse matches. Moreover, by combining reconstruction loss with regression loss on the generated pseudo labels, the performance is further improved. The experimental results demonstrate that our models achieve state-of-the-art results among unsupervised methods on the public KITTI, MPI-Sintel and Flying Chairs datasets.

12.
Front Microbiol ; 11: 1970, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-32849488

RESUMO

In this study, the mitogenome of artillery fungus, Sphaerobolus stellatus, was assembled and compared with other Basidiomycota mitogenomes. The Sphaerobolus stellatus mitogenome was composed of circular DNA molecules, with a total size of 152,722 bp. Accumulation of intergenic and intronic sequences contributed to the Sphaerobolus stellatus mitogenome becoming the fourth largest mitogenome among Basidiomycota. We detected large-scale gene rearrangements in Basidiomycota mitogenomes, and the Sphaerobolus stellatus mitogenome contains a unique gene order. The quantity and position classes of intron varied between 75 Basidiomycota species we tested, indicating frequent intron loss/gain events occurred in the evolution of Basidiomycota. A novel intron position classes (P1281) was detected in the Sphaerobolus stellatus mitogenome, without any homologous introns from other Basidiomycota species. A pair of fragments with a total length of 9.12 kb in both the nuclear and mitochondrial genomes of Sphaerobolus stellatus was detected, indicating possible gene transferring events. Phylogenetic analysis based on the combined mitochondrial gene set obtained well-supported tree topologies (Bayesian posterior probabilities ≥ 0.99; bootstrap values ≥98). This study served as the first report on the mitogenome from the order Geastrales, which will promote the understanding of the phylogeny, population genetics, and evolution of the artillery fungus, Sphaerobolus stellatus.

13.
Materials (Basel) ; 13(16)2020 Aug 17.
Artigo em Inglês | MEDLINE | ID: mdl-32824409

RESUMO

Understanding the properties of defects is crucial to design higher performance semiconductor materials because they influence the electronic and optical properties significantly. Using ab initio calculations, the dynamics properties of nitrogen interstitial in GaN material, including the configuration, migration, and interaction with vacancy were systematically investigated in the present work. By introducing different sites of foreign nitrogen atom, the most stable configuration of nitrogen interstitial was calculated to show a threefold symmetry in each layer and different charge states were characterized, respectively. In the researches of migration, two migration paths, in-plane and out-of-plane, were considered. With regards to the in-plane migration, an intermediated rotation process was observed first time. Due to this rotation behavior, two different barriers were demonstrated to reveal that the migration is an anisotropic behavior. Additionally, charged nitrogen Frenkel pair was found to be a relatively stable defect complex and its well separation distance was about 3.9 Å. Part of our results are in good agreement with the experimental results, and our work provides underlying insights of the identification and dynamics of nitrogen interstitial in GaN material. This study of defects in GaN material is useful to establish a more complete theory and improve the performance of GaN-based devices.

14.
Anal Chem ; 92(12): 8090-8096, 2020 06 16.
Artigo em Inglês | MEDLINE | ID: mdl-32431153

RESUMO

Current rapid bacterial detection methods are dedicated to the classification and identification of bacteria. However, there is still a lack of a method for specific quantitative analysis of certain bacteria. In this work, a method based on elemental-tags laser-induced breakdown spectroscopy (ETLIBS) was developed for the rapid and specific quantitative analysis of Salmonella typhimurium (S. ty). Elemental tags were first synthesized by assembling copper nanoparticles (CuNPs) with poly(thymine) (poly-T) template that linked with the aptamer sequence. Under the specific recognition of the aptamer, S. ty can be fully combined with the elemental tags within 30 min to achieve labeling. Afterward, the silicon nanowires (SiNWs) array modified with Au@Ag nanoparticles (SiNWs-Au@Ag) was employed to capture S. ty in 30 min. Attributed to the rapid analysis superiority of ETLIBS mapping, 100 spectra of SiNWs-Au@Ag/S. ty/CuNPs can be obtained in 5 min. It was found that the peak area of the Cu(I) atomic emission line at 324.75 nm fitted by the Voigt profile was linearly related to the bacterial concentration in the range of 102-106 CFU/mL(R2 = 0.978). Furthermore, ETLIBS mapping achieved a low limit of detection (LOD) of 61 CFU/mL and showed good selectivity to S. ty compared with other bacteria. Besides, the method exhibited preeminent detection performance in spiked samples with the recoveries of 87-113%. With the advantages of rapidity, high efficiency, and specificity, the proposed method is expected to be a powerful tool for bacterial detection.


Assuntos
Lasers , Salmonella typhimurium/isolamento & purificação , Aptâmeros de Nucleotídeos/química , Cobre/química , Ouro/química , Nanopartículas/química , Tamanho da Partícula , Silício/química , Prata/química , Análise Espectral , Propriedades de Superfície
15.
Nanoscale ; 11(12): 5346-5354, 2019 Mar 21.
Artigo em Inglês | MEDLINE | ID: mdl-30848272

RESUMO

Three-dimensional nano-biointerfaces, emerging as significant cell-guiding platforms, have attracted great attention. Nevertheless, complicated chemical modifications and instability of bio-ligands limit their widespread application. In this study, a novel biointerface, based on silicon nanowires (SiNWs) array, was prepared for bacterial capture and sensing. Vertically aligned SiNWs were fabricated via metal assisted chemical etching and decorated with uniform Au@Ag core-shell nanoparticles (Au@Ag NPs). These deposited Au@Ag NPs formed multi-scale topographic structures with nanowires, which provided effective attachment sites for bacterial adhesins. In addition, the Au cores of Au@Ag NPs enhanced the activity of the surface silver atoms and promoted the binding of Au@Ag NPs to bacteria. Thus, the Au@Ag NPs decorated SiNWs (SiNWs-Au@Ag) substrate exhibited high capture capacity for bacteria in drinking water (8.6 and 5.5 × 106 cells per cm2 for E. coli and S. aureus in 40 min, respectively) via physical and chemical effects. Bacteria in drinking water can be sensitively detected by using a combination of laser induced breakdown spectroscopy (LIBS) and label based surface-enhanced Raman spectroscopy (SERS) techniques. Due to the antibacterial activity of Au@Ag NPs and the physical stress exerted on SiNWs, the prepared biointerface also showed high antibacterial rates towards both Gram-positive and Gram-negative bacteria strains. With these excellent properties, the flexible sensing platform might open a new avenue for the prevention and control of microbial hazards in water.


Assuntos
Lasers , Nanopartículas Metálicas/química , Nanofios/química , Silício/química , Análise Espectral Raman , Antibacterianos/química , Antibacterianos/farmacologia , Ouro/química , Bactérias Gram-Negativas/efeitos dos fármacos , Bactérias Gram-Negativas/isolamento & purificação , Bactérias Gram-Positivas/efeitos dos fármacos , Bactérias Gram-Positivas/isolamento & purificação , Microscopia Eletrônica de Transmissão , Nanofios/toxicidade , Tamanho da Partícula , Espectroscopia Fotoeletrônica , Prata/química
16.
Anal Chim Acta ; 1043: 64-71, 2018 Dec 28.
Artigo em Inglês | MEDLINE | ID: mdl-30392670

RESUMO

In this study, a novel strategy based on the combination of 3D SERS and LIBS was developed for qualitative and quantitative detection of bacteria. SERS-active Ag nanoparticles (AgNPs) were prepared by an improved in situ synthesis method, and reproducible SERS spectra of bacteria were obtained by natural evaporation of a droplet of the in situ synthesized sample. Four types of bacteria were classified via principal component analysis (PCA) and hierarchy cluster analysis (HCA). LIBS acted as a quantitative technique for bacterial detection based on the intracellular mineral cations, and bacteria could be detected in a linear range of 5 × 103-5 × 107 CFU mL-1, with recovery values ranging from 81.0% to 101.7%. The whole detection process including sample preparation and detection could be completed in approximately 30 min. With short assay time and simple operation, the proposed strategy has showed great potential for bacterial analysis.


Assuntos
Bactérias/isolamento & purificação , Lasers de Estado Sólido , Análise Espectral Raman/métodos , Microbiologia da Água , Bactérias/química , Bactérias/metabolismo , Análise por Conglomerados , Água Potável/microbiologia , Água Doce/microbiologia , Nanopartículas Metálicas/química , Análise de Componente Principal , Prata/química
17.
J Chromatogr Sci ; 54(9): 1694-1700, 2016 Oct 17.
Artigo em Inglês | MEDLINE | ID: mdl-27473418

RESUMO

In this work, a simple and effective method based on magnetic solid-phase extraction combined with high-performance liquid chromatography was developed for the determination of benzo[α]pyrene (BaP) in cigarette smoke. Oleic acid coated Fe3O4 (Fe3O4-OA) was synthesized and directly used as an efficient sorbent for the first time in magnetic solid-phase extraction (MSPE) procedure for the clean-up of BaP in cigarette smoke extracts. The synthesized Fe3O4-OA was characterized by transmission electron microscopy, X-ray diffraction and Fourier transformed infrared spectroscopy. The extraction via Fe3O4-OA was dispersed in the extracts of cigarette smoke followed by the magnetic isolation, acetonitrile-tetrahydrofuran (ACN-THF; v/v = 9:1) was used for desorption of the analyte. The effects of important parameters such as the amount of adsorbent, solution pH, the content of acetonitrile, temperature and sorption time were investigated. The method showed good linearity for the determination of BaP in the concentration range of 0.5-50 ng mL-1 with a regression coefficient (R2) of 0.9987. The limit of detection and limit of quantification for BaP were obtained to be 0.12 and 0.41 ng mL-1, respectively. The mean recoveries were in the range from 81.0% to 97.6% at low, medium, high spiked levels, and the relative standard deviations were in the range of 2.7-6.8%. Combined with high-performance liquid chromatography and fluorescence detection, a simple and effective method was developed for the analysis of BaP in cigarette smoke.

18.
Biomed Chromatogr ; 29(12): 1871-7, 2015 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-26019021

RESUMO

A novel and efficient sample preconcentration technique based on the Fe3O4 magnetic nanoparticles (Fe3O4 MNPs) coated with silica (SiO2) has been developed for extraction and determination of sulpiride. The functionalized MNPs showed excellent dispersibility in aqueous solution and were applied to magnetic solid-phase extraction of sulpiride from human urine and blood prior to high-performance liquid chromatography analysis. The separation, preconcentration and desorption procedure was completed in 10 min. Optimal experimental conditions, including sample pH, the amount of the MNPs, eluent type and volume, and the ultrasonication time were studied and established. The method showed good linearity for the determination of sulpiride in the concentration range of 10-1000 ng/mL in urine and blood. The recovery of the method was in the range between 91.2 and 97.5%, and the limit of detection was 2 ng/mL for sulpiride in human blood and urine. The results indicated that the present procedure is a suitable pretreatment method for biological samples.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Nanopartículas de Magnetita/química , Extração em Fase Sólida/métodos , Sulpirida/sangue , Sulpirida/urina , Adulto , Feminino , Humanos , Limite de Detecção , Modelos Lineares , Masculino , Pessoa de Meia-Idade , Reprodutibilidade dos Testes , Sulpirida/química , Sulpirida/isolamento & purificação
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