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1.
Adv Mater ; : e2404001, 2024 Jun 05.
Artículo en Inglés | MEDLINE | ID: mdl-38838735

RESUMEN

High-dielectric-constant elastomers always play a critical role in the development of wearable electronics for actuation, energy storage, and sensing; therefore, there is an urgent need for effective strategies to enhance dielectric constants. The present methods mainly involve adding inorganic or conductive fillers to the polymer elastomers, however, the addition of fillers causes a series of problems, such as large dielectric loss, increased modulus, and deteriorating interface conditions. Here, the elastification of relaxor ferroelectric polymers is investigated through slight cross-linking, aiming to obtain intrinsic elastomers with high-dielectric constants. By cross-linking of the relaxor ferroelectric polymer poly(vinylidene fluoride-ter-trifluoroethylene-ter-chlorofluoroethylene) with a long soft chain cross-linker, a relaxor ferroelectric elastomer with an enhanced dielectric constant is obtained, twice that of the pristine relaxor ferroelectric polymer and surpassing all reported intrinsic elastomers. This elastomer maintains its high-dielectric constant over a wide temperature range and exhibits robust mechanical fatigue resistance, chemical stability, and thermal stability. Moreover, the ferroelectricity of the elastomer remains stable under strains up to 80%. This study offers a simple and effective way to enhance the dielectric constant of intrinsic elastomers, thus facilitating advancements in soft robots, biosensors, and wearable electronics.

2.
Am J Hum Genet ; 110(9): 1509-1521, 2023 09 07.
Artículo en Inglés | MEDLINE | ID: mdl-37619562

RESUMEN

Understanding dosage sensitivity or why Mendelian diseases have dominant vs. recessive modes of inheritance is crucial for uncovering the etiology of human disease. Previous knowledge of dosage sensitivity is mainly based on observations of rare loss-of-function mutations or copy number changes, which are underpowered due to ultra rareness of such variants. Thus, the functional underpinnings of dosage constraint remain elusive. In this study, we aim to systematically quantify dosage perturbations from cis-regulatory variants in the general population to yield a tissue-specific dosage constraint map of genes and further explore their underlying functional logic. We reveal an inherent divergence of dosage constraints in genes by functional categories with signaling genes (transcription factors, protein kinases, ion channels, and cellular machinery) being dosage sensitive, while effector genes (transporters, metabolic enzymes, cytokines, and receptors) are generally dosage resilient. Instead of being a metric of functional dispensability, we show that dosage constraint reflects underlying homeostatic constraints arising from negative feedback. Finally, we employ machine learning to integrate DNA and RNA metrics to generate a comprehensive, tissue-specific map of dosage sensitivity (MoDs) for autosomal genes.


Asunto(s)
Benchmarking , Citocinas , Humanos , Homeostasis , Patrón de Herencia , Aprendizaje Automático
3.
J Craniofac Surg ; 34(8): 2246-2251, 2023.
Artículo en Inglés | MEDLINE | ID: mdl-37470720

RESUMEN

Cranioplasty is a common neurosurgical procedure; however, the optimal material choice remains controversial. At the time of this writing, autologous bone, the preferred choice for primary cranioplasty, has a high incidence of complications such as infection and resorption, thus requiring frequent use of synthetic materials. Therefore, this study aimed to compare the clinical benefits of titanium mesh (Ti), polyetheretherketone (PEEK), and composite bone cement (CBC) in cranioplasty to provide a clear selection basis for clinicians and patients. This study retrospectively collected data from 207 patients who underwent cranioplasty with Ti (n=129), PEEK (n=54), and CBC (n=24) between January 2018 and December 2020 at Henan Provincial People's Hospital. Postoperative follow-up information after 6 months was used to compare the long-term effects of the 3 materials on the patients. There were no significant differences in the overall complication rate after cranioplasty among the 3 materials. However, subcutaneous effusion was more frequent with PEEK (24.07%) and CBC (20.83%) than with Ti (2.33%). Second, there were no significant differences in the increase in Glasgow Outcome Scale and Karnofsky Performance Status scores after cranioplasty among the 3 materials. Finally, we found that PEEK had the highest patient satisfaction and hospitalization cost, whereas the opposite was true for Ti. Although the surgical outcomes of the 3 implant materials were similar, an examination of clinical outcomes such as patient satisfaction showed significant differences, deepening people's perceptions of the 3 materials.


Asunto(s)
Implantes Dentales , Procedimientos de Cirugía Plástica , Humanos , Estudios Retrospectivos , Cementos para Huesos , Titanio , Mallas Quirúrgicas/efectos adversos , Polietilenglicoles , Cetonas , Cráneo/cirugía , Complicaciones Posoperatorias/etiología
4.
Adv Sci (Weinh) ; 10(9): e2206483, 2023 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-36683182

RESUMEN

The conversion of ubiquitous hygrothermal resources into renewable energy offers significant potential for cable-free, self-powered systems that can operate worldwide without regard to climatic or geographic limitations. Here, an all-printed flexible hygro-thermoelectric paper generator is demonstrated that uses bifunctional mobile ions and electrons to make the moist-diffusion effect, the Soret effect, and the Seebeck effect work synergistically. In the ordinary hygrothermal settings, it generates an unconventional hygro-thermoelectric output pattern and shows almost a dozen-fold increase in positive hygro-thermopower of 26.70 mV K-1 and also another negative hygro-thermopower of -15.71 mV K-1 compared to pure thermopower. A single paper generator can produce a giant 680 mV displaying typical cyclic sinusoidal waveform characters with volt-sized amplitudes. The ion-electron conductive ink is easily printable and consists primarily of a Bi2 Te3 /PEDOT:PSS thermoelectric matrix modulated with a hygroscopic glycerol that releases ion charges for moist-diffusion effect and Soret effect, as well as electron charges for Seebeck effect. The emerged hygro-thermoelectric harvesting strategy from surrounding hygrothermal resources offers a revolutionary approach to the next generation of hybrid energy with cost-efficiency, flexibility, and sustainability, and also enables large-scale roll-to-roll production.

5.
Food Chem ; 378: 132093, 2022 Jun 01.
Artículo en Inglés | MEDLINE | ID: mdl-35032807

RESUMEN

This work demonstrated an ultrasensitive and simple microfluidic immunosensor for point-of-care test of Staphylococcus aureus (S. aureus) based on the stir bar enrichment and DNAzyme-assisted click reaction. Initially, S. aureus was enriched by the 4-mercaptophenylboronic acid-functionalized stir bar. The yolk antibody (immunoglobulin Y) and copper-labeled polydopamine nanoparticles were then specifically conjugated with the captured target. The Cu(II) was released under acidic conditions and effectively catalyzed the copper-catalyzed azide-alkyne cycloaddition (CuAAC) between the alkyne group-labeled DNAzyme and the streptavidin-biotin-azido with the assistance of DNAzyme. Finally, the DNAzyme-streptavidin complexes were detected by microfluidic chips to quantify S. aureus. Under optimum conditions, this immunosensor showed good detection performances toward S. aureus within 10 to 2.5 × 104 CFU/mL with a limit of detection of 3 CFU/mL. Moreover, the satisfying detection results of real samples of animal origin also implied that this immunosensor owned great potential in practical applications.


Asunto(s)
Técnicas Biosensibles , ADN Catalítico , Animales , Química Clic , Cobre , Inmunoensayo , Microfluídica , Pruebas en el Punto de Atención , Staphylococcus aureus
6.
Small Methods ; 5(12): e2100834, 2021 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-34928041

RESUMEN

Electrocatalytic oxygen evolution reaction (OER), an important electrode reaction in electrocatalytic and photoelectrochemical cells for a carbon-free energy cycle, has attracted considerable attention in the last few years. Metal oxides have been considered as good candidates for electrocatalytic OER because they can be easily synthesized and are relatively stable during the OER process. However, inevitable structural variations still occur to them due to the complex reaction steps and harsh working conditions of OER, thus impending the further insight into the catalytic mechanism and rational design of highly efficient electrocatalysts. The aim of this review is to disclose the current research progress toward the structural variations of metal oxide-based OER electrocatalysts. The origin of structural variations of metal oxides is discussed. Based on some typical oxides performing OER activity, the external and internal factors that influence the structural stability are summarized and then some general approaches to regulate the structural variation process are provided. Some operando methods are also concluded to monitor the structural variation processes and to identify the final active structure. Additionally, the unresolved problems and challenges are presented in an attempt to get further insight into the mechanism of structural variations and establish a rational structure-catalysis relationship.

7.
J Chromatogr A ; 1655: 462508, 2021 Oct 11.
Artículo en Inglés | MEDLINE | ID: mdl-34492579

RESUMEN

High hydrophilic anion stationary phases play a crucial role in the separation behavior of ion chromatography. Herein, we report novel polymeric anion exchangers grafted with polyethylene polyamines, including ethylenediamine, diethylenetriamine, triethylenetetramine and tetraethylene pentaamine, via a facile epoxy-amine polymerization method. The anion exchangers were characterized by scanning electron microscopy, thermogravimetry, Fourier transform infrared spectrometry and elemental analysis. The chromatographic performance of the stationary phases was evaluated with the separation of common inorganic anions, organic weak acids and highly polarizable anions. Seven common anions (F-, Cl-, NO2-, Br-, NO3-, SO42- and HPO42-) can be separated within 18 min by using hydroxide eluent in isocratic mode. By adopting different polyethylene polyamines as hyperbranched units, the four types of new stationary phases displayed high efficiencies and good reproducibility. The columns exhibit large exchange capacities at 76.5-184.8 µmol•column-1 (4.6 × 150 mm, i.d.) with efficiency up to 20293 plate m-1 (Cl-). The RSDs of the retention time were less than 0.27% and the RSDs of the efficiency were less than 1.95% by consecutive injections after working for two months. The self-fabricated column was successfully applied to determine the chloride content in exhaled breath condensate.


Asunto(s)
Poliaminas , Polietilenos , Aniones , Cromatografía por Intercambio Iónico , Reproducibilidad de los Resultados
8.
J Chromatogr A ; 1614: 460715, 2020 Mar 15.
Artículo en Inglés | MEDLINE | ID: mdl-31759640

RESUMEN

It is challenging to greatly increase of the extraction selectivity and efficiency by stir bar sorptive extraction of ultra-trace polychlorinated biphenyls (PCBs) in complex environmental matrix, e.g., soils. To fulfill this purpose, one of the critical works is to prepare some coatings with high selectivity, adsorptive capacity and reusability. It is also important to develop some green, simple methods for preperation the coatings. In this work, a kind of highly efficient and bioactive coating based on hyperbranched aptamer (HB-Apt) was constructed via hybridization chain reaction (HCR). Then, the HB-Apt was coated on a magnetic stir bar and applied to headspace extraction of PCB72 and PCB106 in soils. The core-shell gold magnetic particles (Fe3O4@AuNPs, AuMNPs for short) was employed as the substrate to immobilize the HB-Apt. The extracted PCBs on the stir bar could be easily eluted in ethanol by stirring, and then sampled in gas chromatography-mass spectrometry (GC-MS) for qualification. The ultra-low detection limit (0.003-0.005 ng•g-1), good linearity (0.01-500 ng•g-1, R2≥0.994) and reproducibility (RSD: 4.58-6.53%) were obtained. Compared with the common aptamer coating, the HB-Apt coating exhibited good selectivity and higher extraction capacity. The results might be related to the fact that there are more aptamer fragments grated on the HB-Apt coating than those of the common aptamer coating. The magnetic stir bar can not only be employed for easy headspace extraction, but also facilitate separation and elution. Moreover, the coating could be recycled for at least 60 times before recoveries of the PCB72 and PCB106 in the spiked samples drop below 90%. All these indicated that the assay is simple, robust, environment friendly and promising for detection of trace PCBs in complex environmental samples.


Asunto(s)
Bifenilos Policlorados/análisis , Contaminantes del Suelo/análisis , Adsorción , Cromatografía de Gases y Espectrometría de Masas , Oro , Límite de Detección , Fenómenos Magnéticos , Nanopartículas del Metal , Bifenilos Policlorados/aislamiento & purificación , Reproducibilidad de los Resultados , Contaminantes del Suelo/aislamiento & purificación
9.
ACS Sens ; 4(8): 2131-2139, 2019 08 23.
Artículo en Inglés | MEDLINE | ID: mdl-31366194

RESUMEN

The development of multiplex assays to simultaneously monitor multiclass chemical contaminants that commonly coexist in foods, such as heavy metal ions, antibiotics, and estrogen residues, is gaining attention. Here, a microfluidic chip (MC)-based multianalysis method coupled with magnetic encoded aptamer probes was used for simultaneous detection of kanamycin, 17ß-estradiol, and lead ion (Pb2+). Using this innovative strategy, the magnetic bead (MB)-based encoded probes labeled with aptamer hybrid chains were first used to selectively capture multiple targets, followed by generating single-stranded primers. The primers triggered a multibranched hybridization chain reaction (mHCR). Finally, three kinds of complementary strands (C-DNAs) with different lengths were hybridized with the arms of the mHCR products to form three types of multibranched DNA nanostructures. The decrement signals of C-DNAs were employed for qualification of targets. As the signal tags corresponded to different targets, the DNA nanostructures realized "one target for the decrease of massive C-DNAs" to improve sensitivity. The use of MB-based encoded probes could achieve magnetic separation to eliminate interference in the complex. The detection limits of this method were 1.76 × 10-4 nM (kanamycin), 1.18 × 10-4 nM (17ß-estradiol), and 1.29 × 10-4 nM (lead ion). Furthermore, the MC platform is reusable and can be used for more than 4000 samples. The assay combining the MC with MB-based encoded probes with multibranched DNA signal tags offers a universal, reusable, and high-throughput detection platform for screening multiclass chemical contaminants in food samples with complex matrices.


Asunto(s)
Aptámeros de Nucleótidos/química , Técnicas Biosensibles , ADN/química , Contaminación de Alimentos/análisis , Técnicas Analíticas Microfluídicas , Nanoestructuras/química , Técnicas Electroquímicas , Estradiol/análisis , Humanos , Iones/análisis , Kanamicina/análisis , Plomo/análisis , Fenómenos Magnéticos
10.
Anal Chim Acta ; 1046: 208, 2019 01 10.
Artículo en Inglés | MEDLINE | ID: mdl-30482301

RESUMEN

This article has been retracted at the request of the Editor after the corresponding author pointed the Editor to comments from an anonymous reader. The article reports electron micrographs of different preparations while showing identical images as used in previous publications by the same authors. The particles in Fig. 4C (SEM image of Fe3O4@SiO2) are identical to each other and the corresponding author confirmed that these have been copy-pasted. In addition, these particles have previously been communicated as different substances in Fig. 1B from Pan et al., J. Mater. Chem. A, 2015,3, 23042-23052 (DOI: 10.1039/C5TA05840F) and Fig. 3F from Pan et al., Anal. Methods, 2017,9, 5281-5292 (DOI: 10.1039/C7AY01444A). Furthermore, the curves in Fig. 7, especially the baseline, shows a remarkable similarity to Fig. 8 from Pan et al., J. Mater. Chem. A, 2015,3, 23042-23052 (DOI: 10.1039/C5TA05840F) and Fig. 5F from Pan et al., J. Mater. Chem. A, 2014,2, 15345-15356 (DOI: 10.1039/c4ta02600d). The manipulation of images and data in this way is a serious offense to the integrity of the scientific community and casts doubts on all the data, and accordingly also the conclusions based on that data, in this publication. As such this article represents a severe abuse of the scientific publishing system. The scientific community takes a very strong view on this matter and apologies are offered to readers of the journal that this was not detected during the submission process. This article has been retracted: please see Elsevier Policy on Article Withdrawal (https://www.elsevier.com/about/our-business/policies/article-withdrawal).

11.
RSC Adv ; 8(19): 10686-10697, 2018 Mar 13.
Artículo en Inglés | MEDLINE | ID: mdl-35540459

RESUMEN

A tetraethylenepentamine (TEPA)-functionalized nano-Fe3O4 magnetic composite material (nFe3O4@TEPA) was synthesized by a facile one-pot solvothermal method. It was characterized by elementary analysis (EA), powder X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). The results show that the nFe3O4@TEPA has an average size of ∼20 nm, with a saturation magnetization intensity of 48.2 emu g-1. Its adsorption properties were investigated by adsorbing fluorine ions, phosphate, Cr(vi) and their co-existing water system. The adsorption performance was studied as a function of solution pH, initial concentration of ions, contact time and temperature for each ion. The adsorption of the multi-ion co-existing system was studied via batch tests, XPS and FTIR analyses. The effect of co-existing ions was studied through Box-Behnken Design (BBD) and response surface methodology (RSM). It can be deducted that the adsorption mechanism of an individual fluorine ion or phosphate was mainly related to electrostatic attraction, while that of Cr(vi) might be mainly related to electrostatic attraction and coordination interactions. For the fluorine ion and phosphate bi-component system, their adsorption was competitive via ion exchange. For the Cr(vi), fluorine ion and phosphate tri-component co-existing system, Cr(vi) took priority for adsorption and could replace the absorbed fluorine ion or phosphate by competitive reaction, but not vice versa.

12.
RSC Adv ; 8(52): 29928-29938, 2018 Aug 20.
Artículo en Inglés | MEDLINE | ID: mdl-35547276

RESUMEN

A series of ethylenediamine-grafted ion imprinted magnetic polymers (Fe3O4@IIPs) were synthesized via ultrasonic assisted suspension polymerization with perchlorate (ClO4 -) as an ion imprinting template. They were characterized by XRD, EA, VSM, FTIR and XPS and applied as adsorbents for ClO4 - removal from aqueous solutions. The effects of the usage amount of crosslinking agent divinylbenzene (DVB) used for preparation on the structure and the adsorptive performance of Fe3O4@IIPs were investigated. The results show that the Fe3O4@IIPs have an average size of 200-800 nm, which increases with the increase of the amount of DVB from 0 to 2 g during the preparation process. The saturation magnetization intensities are at 35.6-42.8 emu g-1, which decrease with the increase of the usage amount of DVB. The addition of DVB is beneficial to the formation and stability of the ion imprinted cavity of Fe3O4@IIPs. The effects of the solution pH value, initial concentration of ClO4 -, and adsorption time on the adsorption properties of ClO4 - in aqueous solutions were investigated. The results show that the adsorption capability is affected significantly by solution pH value and reaches the maximum adsorption capacity at pH 3.0. The best adsorption capacity and selectivity of Fe3O4@IIPs to ClO4 - can be obtained when the usage amount of DVB is at 0.5 g for synthesis. The adsorption mechanisms might include both ion exchange and electrostatic interaction. The isothermal adsorption curves mainly obey the Langmuir model with the theoretical maximum adsorption capacities (q m,c) at 76.92-111.1 mg g-1 and the experimental maximum adsorption capacities (q m,e) at 75.7-108.9 mg g-1, respectively, which are much higher than those of the non-ion imprinted material (Fe3O4@NIP, q m,NIP: q m,c at 60.61 mg g-1 and q m,e at 59.0 mg g-1). The adsorption kinetic studies show that the adsorption processes reach equilibrium within 10 min and the kinetic data are well fitted to the pseudo-second-order model. There is almost no interference by the coexisting anions for the selective adsorption of ClO4 -, with a imprinting factor (α) at 1.8, and selectivity factor (ß) larger than 5.9 for several kinds of common co-existing anions, respectively. The Fe3O4@IIPs are ideal candidates for removal of ClO4 - from aqueous solution.

13.
Anal Chim Acta ; 919: 34-46, 2016 May 05.
Artículo en Inglés | MEDLINE | ID: mdl-27086097

RESUMEN

In this study, graphene oxide-encapsulated core-shell magnetic microspheres (GOE-CS-MM) were fabricated by a self-assemble approach between positive charged poly(diallyldimethylammonium) chloride (PDDA)-modified Fe3O4@SiO2 and negative charged GO sheets via electrostatic interaction. The as-prepared GOE-CS-MM was carefully characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), vibrating sample magnetometer analysis (VSM), and X-ray photoelectron spectroscopy (XPS), and was used as a cleanup adsorbent in magnetic solid-phase extraction (MSPE) for determination of 15 trace-level environmental phenols in seafood coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS). The obtained results showed that the GOE-CS-MM exhibited excellent cleanup efficiency and could availably reduce the matrix effect. The cleanup mechanisms were investigated and referred to π-π stacking interaction and hydrogen bond between GOE-CS-MM and impurities in the extracts. Moreover, the extraction and cleanup conditions of GOE-CS-MM toward phenols were optimized in detail. Under the optimized conditions, the limits of detection (LODs) were found to be 0.003-0.06 µg kg(-1), and satisfactory recovery values of 84.8-103.1% were obtained for the tested seafood samples. It was confirmed that the developed method is simple, fast, sensitive, and accurate for the determination of 15 trace environmental phenols in seafood samples.


Asunto(s)
Contaminantes Ambientales/análisis , Grafito/química , Imanes , Microesferas , Óxidos/química , Fenoles/análisis , Alimentos Marinos/análisis , Cromatografía Liquida , Espectrometría de Masas en Tándem
14.
J Chromatogr A ; 1422: 1-12, 2015 Nov 27.
Artículo en Inglés | MEDLINE | ID: mdl-26477521

RESUMEN

Microcystins (MCs), a group of cyclic heptapeptide heaptoxins and tumor promoters, are generated by cyanobacteria occurring in surface waters, such as eutrophic lakes, rivers, and reservoirs. In this present study, a novel double-sided magnetic molecularly imprinted polymer modified graphene oxide (DS-MMIP@GO) based magnetic solid-phase extraction (MSPE) method was developed for fast, effective and selective enrichment, and recognition of trace MCs in environmental water samples combined with high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The synthesized novel DS-MMIP@GO was used as the adsorbents in this work and was carefully characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and Raman spectra. The adsorption and desorption conditions of DS-MMIP@GO toward MCs were optimized in detail to obtain the highest binding capacity, selectivity, and release efficiency. Under the optimum conditions, the enrichment factors of the method for eight target MCs were found to be 2000. The limits of quantitation (LOQs) of the method for eight MCs were in range of 0.1-2.0ngL(-1). The double-sided MMIP modified structure provided DS-MMIP@GO with abundant adsorption sites and permitted it to exhibit excellent enrichment and selectivity toward trace-level MCs. The proposed method was successfully applied for the analysis of environmental water samples with recoveries ranging from 84.1 to 98.2%. Compared to conventional methods for MCs detection reported in literatures, the one developed in this work based on DS-MMIP@GO and LC-MS/MS showed much faster, more sensitive, and more convenient.


Asunto(s)
Cromatografía Liquida , Monitoreo del Ambiente/métodos , Agua Dulce/química , Microcistinas/análisis , Microcistinas/aislamiento & purificación , Óxidos/química , Espectrometría de Masas en Tándem , Grafito/química , Magnetismo , Microscopía Electrónica de Transmisión , Polímeros/química , Extracción en Fase Sólida , Espectroscopía Infrarroja por Transformada de Fourier , Contaminantes Químicos del Agua/análisis
15.
J Chromatogr A ; 1365: 35-44, 2014 Oct 24.
Artículo en Inglés | MEDLINE | ID: mdl-25218632

RESUMEN

A high-performance magnetic molecularly imprinted polymer (MIP) coating using zeolite imidazolate framework-8 coated magnetic iron oxide (Fe3O4@ZIF-8) as a carrier was developed for simultaneous automated solid phase microextraction of four estrogens in 24 food samples. The coating material, abbreviated as MZMIP, was synthesized through time-efficient layer-by-layer assembling of ZIF-8 and MIP film on Fe3O4 particles. It was characterized and automatically coated on the surface of SPME fibers by electromagnetic bonding. The extraction performance, reusability, repeatability, and validity of the MZMIP-SPME system was evaluated for high-throughput analysis of estrone (E1), estradiol (E2), estriol (E3), and ethinylestradiol (EE2). Various factors affecting the quality of MZMIP coating were optimized. Compared with traditional magnetic MIP coating based on Fe3O4@SiO2 carrier, the MZMIP coating exhibited high extraction capacity and quick adsorption and desorption kinetics to E1, E2, E3, and EE2 owing to the larger amount of imprinting sites in MZMIP. Under optimum conditions, the proposed system requires only 25min for pretreatment of all 24 samples (62.5s per sample). The limits of detection and quantitation of the proposed automated system for analysis were found to range from 0.4 to 1.7 and 1.1 to 6.2ngg(-1), respectively. During analysis of spiked fish and pork, the new coating showed better recovery and selectivity compared with Fe3O4@SiO2@MIP (MMIP) and commercially available SPME. The results indicated that the MZMIP coating could be effectively employed for pretreatment of ultra-trace level of estrogens in food.


Asunto(s)
Estrógenos/aislamiento & purificación , Compuestos Férricos/química , Productos Pesqueros/análisis , Imidazoles/química , Carne/análisis , Polímeros/química , Microextracción en Fase Sólida/métodos , Adsorción , Animales , Estradiol/aislamiento & purificación , Estriol/aislamiento & purificación , Estrona/aislamiento & purificación , Peces , Imanes , Impresión Molecular , Porosidad , Porcinos , Zeolitas
16.
J Chromatogr A ; 1362: 34-42, 2014 Oct 03.
Artículo en Inglés | MEDLINE | ID: mdl-25160956

RESUMEN

A novel planar-structure amine-functional magnetic polymer modified graphene oxide nanocomposite (NH2-MP@GO) was synthesized. The properties were characterized by transmission electron microscopy (TEM) and Fourier-transform infrared spectrometry (FTIR). The obtained adsorption results showed that the NH2-MP@GO had great adsorptive ability toward five chlorophenols (CPs), including 2-chlorophenol (2-CP), 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP) and pentachlorophenol (PCP). Based on these, an effective magnetic solid-phase extraction (MSPE) procedure coupled with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the preconcentration and determination of the five CPs in environmental water samples was developed. Various experimental parameters that could affect the extraction efficiencies had been investigated in detail. Under the optimum conditions, the enrichment factors of the method for the target CPs were found to be 1000. The proposed method was successfully applied for the analysis of environmental water samples with recoveries ranging from 86.4 to 99.8% with correlation coefficients (R) higher than 0.9994. Good linearities were obtained ranging from 10 to 500ng/L for 2-CP, 5 to 500ng/L for 2,4-DCP, 2 to 500ng/L for 2,4,6-TeCP and 2,3,4,6-TeCP, and 1 to 500ng/L for PCP, respectively. The limits of quantitation for the five CPs were 0.6-9.2ng/L. It was confirmed that the planar-structure NH2-MP@GO was a kind of highly effective MSPE materials used for the trace CPs analyses.


Asunto(s)
Aminas/química , Clorofenoles/análisis , Cromatografía Liquida/métodos , Óxidos/química , Extracción en Fase Sólida/métodos , Espectrometría de Masas en Tándem/métodos , Agua/química , Adsorción , Cromatografía Liquida/instrumentación , Grafito/química , Concentración de Iones de Hidrógeno , Límite de Detección , Fenómenos Magnéticos , Polímeros/química , Extracción en Fase Sólida/instrumentación , Espectrometría de Masas en Tándem/instrumentación
17.
J Chromatogr A ; 1346: 123-8, 2014 Jun 13.
Artículo en Inglés | MEDLINE | ID: mdl-24797395

RESUMEN

A novel, simple and sensitive method based on the use of magnetic dispersive solid-phase extraction (M-dSPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) was developed to determine seven synthetic pigments (tartrazine, amaranth, carmine, sunset yellow, allura red, brilliant blue and erythrosine) in wines and soft drinks. An amino-functionalized low degrees of cross-linking magnetic polymer (NH2-LDC-MP) was synthesized via suspension polymerization, and characterized by transmission electron microscopy (TEM). The NH2-LDC-MP was used as the M-dSPE sorbent to remove the matrix from the solution, and the main factors affecting the extraction were investigated in detail. The obtained results demonstrated the higher extraction capacity of NH2-LDC-MP with recoveries between 84.0 and 116.2%. The limits of quantification (LOQs) for the seven synthetic pigments were between 1.51 and 5.0µg/L in wines and soft drinks. The developed M-dSPE UFLC-MS/MS method had been successfully applied to the real wines and soft drinks for food-safety risk monitoring in Zhejiang Province, China. The results showed that sunset yellow was in three out of thirty soft drink samples (2.95-42.6µg/L), and erythrosine in one out of fifteen dry red wine samples (3.22µg/L), respectively. It was confirmed that the NH2-LDC-MP was a kind of highly effective M-dSPE materials for the pigments analyses.


Asunto(s)
Bebidas Gaseosas/análisis , Cromatografía Liquida , Colorantes/análisis , Tecnología de Alimentos/métodos , Extracción en Fase Sólida , Espectrometría de Masas en Tándem , Vino/análisis , China , Fenómenos Magnéticos
18.
Talanta ; 115: 787-97, 2013 Oct 15.
Artículo en Inglés | MEDLINE | ID: mdl-24054663

RESUMEN

A novel, simple and sensitive method was developed for the simultaneous determination of eight phenolic environmental estrogens in blood by using the dispersive micro-solid-phase extraction (d-µ-SPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS). The excellent nanomaterials tetraethylenepentamine-functionalized magnetic polymer was used as an adsorbent, and the main factors affecting the extraction efficiency were investigated in detail. All target compounds showed good linearities in the tested range with correlation coefficients (r) higher than 0.999. The mean recoveries were in the range of 85.0-105.0%. The intra-day and inter-day relative standard deviations (RSDs) were lower than 4.9% and 5.2%, respectively. The limits of quantification for the eight phenolic environmental estrogens were between 0.075 and 0.42 µg L(-1). The developed method can be applied to the routine analyses for the determination of the eight phenolic environmental estrogens in blood samples.


Asunto(s)
Disruptores Endocrinos/sangre , Contaminantes Ambientales/sangre , Estrógenos/sangre , Etilenodiaminas/química , Nanoestructuras/química , Fenoles/sangre , Adsorción , Animales , Cromatografía Liquida/métodos , Límite de Detección , Imanes , Polimerizacion , Rana catesbeiana , Reproducibilidad de los Resultados , Extracción en Fase Sólida/métodos , Espectrometría de Masas en Tándem
19.
J Chromatogr A ; 1263: 34-42, 2012 Nov 09.
Artículo en Inglés | MEDLINE | ID: mdl-23044217

RESUMEN

A novel and effective dispersive solid-phase extraction (dSPE) procedure with rapid magnetic separation using ethylenediamine-functionalized magnetic polymer as an adsorbent was developed. The new procedure had excellent clean-up ability for the selective removal of the matrix in red wine. An accurate, simple, and rapid analytical method using ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) for the simultaneous determination of nine food additives (i.e., acesulfame, saccharin, sodium cyclamate, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid, and neotame) in red wine was also used and validated. Recoveries ranging from 78.5% to 99.2% with relative standard deviations ranging from 0.46% to 6.3% were obtained using the new method. All target compounds showed good linearities in the tested range with correlation coefficients (r) higher than 0.9993. The limits of quantification for the nine food additives were between 0.10 µg/L and 50.0 µg/L. The proposed dSPE-UFLC-MS/MS method was successfully applied in the food-safety risk monitoring of real red wine in Zhejiang Province, China.


Asunto(s)
Cromatografía Liquida/métodos , Aditivos Alimentarios/análisis , Espectrometría de Masas/métodos , Vino/análisis , Microscopía Electrónica de Transmisión , Reproducibilidad de los Resultados , Extracción en Fase Sólida
20.
Anal Sci ; 28(9): 887-92, 2012.
Artículo en Inglés | MEDLINE | ID: mdl-22975917

RESUMEN

An efficient analytical method for the preconcentration and determination of phosphate in water samples at trace levels was proposed. The method was based on sample enrichment using dispersive solid-phase extraction (dSPE) with tetraethylenepentamine (TEPA)-functionalized nano-size composite materials (TEPA-NCMs) as sorbents, which were fully characterized. Various parameters affecting the extraction efficiency were systematically investigated. After extraction, the post-adsorbed TEPA-NCMs were eluted by a NaOH solution for desorption of the phosphate. The resulting eluate containing phosphate was determined by a spectrophotometric method. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.29 and 0.96 µg L(-1), respectively. The relative standard deviations (RSDs) were lower than 8.0% with average recoveries ranging from 91 to 118%. The present method was successfully applied to the determination of phosphate at trace levels in real water samples, and it was confirmed that the TEPA-NCMs are highly effective dSPE materials.


Asunto(s)
Etilenodiaminas/química , Nanoestructuras/química , Fosfatos/aislamiento & purificación , Extracción en Fase Sólida , Agua/química , Tamaño de la Partícula , Soluciones
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