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1.
Anal Bioanal Chem ; 408(6): 1679-85, 2016 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-26753984

RESUMO

Protein removal process is always time-consuming for the analysis of milk samples. In this work, hollow fiber membrane-coated functionalized polymeric ionic liquid (HF-PIL) capsules were synthesized and used as solid-phase microextraction (SPME) sorbent for direct analysis of estrogens in milk samples. The functionalized PIL monolith sorbent was obtained by copolymerization between 1-(3-aminopropyl)-3-(4-vinylbenzyl)imidazolium 4-styrenesulfonate IL monomer and 1,6-di(3-vinylimidazolium) hexane bishexafluorophosphate IL-crosslinking agent. A group of four capsules were installed as SPME device, to determine four kinds of estrogens (estrone, diethylstilbestrol, hexestrol, and 17α-ethynylestradiol) in milk samples, coupled to high performance liquid chromatography. Extraction and desorption conditions were optimized to get satisfactory extraction efficiency. Good linearity was obtained in the range of 5-200 µg L(-1). The limits of detection were 1 µg L(-1) for diethylstilbestrol and 2 µg L(-1) for 17α-ethynylestradiol, estrone, and hexestrol. The present method was applied to analyze the model analytes in different milk samples. Relative recoveries were in the range of 85.5-112%. The HF-PIL SPME capsules showed satisfactory extraction efficiency and high resistance to sample matrix interference.


Assuntos
Estrogênios/análise , Análise de Alimentos/métodos , Líquidos Iônicos/química , Leite/química , Microextração em Fase Sólida/métodos , Animais , Cápsulas/química , Cromatografia Líquida de Alta Pressão/métodos , Desenho de Equipamento , Estrona/análise , Contaminação de Alimentos/análise , Hexestrol/análise , Limite de Detecção , Membranas Artificiais , Microextração em Fase Sólida/instrumentação
2.
Anal Bioanal Chem ; 408(20): 5567-76, 2016 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-27255103

RESUMO

An electrochemical sensor of acetaminophen based on poly(diallyldimethylammonium chloride) (PDDA)-functionalized reduced graphene-loaded Al2O3-Au nanoparticles coated onto glassy carbon electrode (Al2O3-Au/PDDA/reduced graphene oxide (rGO)/glass carbon electrode (GCE)) were prepared by layer self-assembly technique. The as-prepared electrode-modified materials were characterized by scanning electron microscopy, X-ray powder diffraction, and Fourier transform infrared spectroscopy. The electrocatalytic performances of Al2O3-Au/PDDA/rGO-modified glassy carbon electrode toward the acetaminophen were investigated by cyclic voltammetry and differential pulse voltammetry. The modified electrodes of graphene oxide (GO)/GCE, PDDA/rGO/GCE, and Al2O3-Au/PDDA/rGO/GCE were constructed for comparison and learning the catalytic mechanism. The research showed Al2O3-Au/PDDA/rGO/GCE having good electrochemical performance, attributing to the synergetic effect that comes from the special nanocomposite structure and physicochemical properties of Al2O3-Au nanoparticles and graphene. A low detection limit of 6 nM (S/N = 3) and a wide linear detection range from 0.02 to 200 µM (R (2) = 0.9970) was obtained. The preparation of sensor was successfully applied for the detection of acetaminophen in commercial pharmaceutical pills. Graphical abstract Schematic diagram of synthesis of Al2O3-Au/PDDA/rGO/GCE.


Assuntos
Acetaminofen/análise , Técnicas Biossensoriais/instrumentação , Condutometria/instrumentação , Grafite/química , Nanopartículas Metálicas/química , Polietilenos/química , Compostos de Amônio Quaternário/química , Acetaminofen/química , Óxido de Alumínio/química , Eletrodos , Desenho de Equipamento , Análise de Falha de Equipamento , Ouro/química , Nanopartículas Metálicas/ultraestrutura , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
3.
Anal Bioanal Chem ; 407(23): 7025-35, 2015 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-26220716

RESUMO

Ionic liquids (ILs) have been efficiently used as a "designer sorbent" in sample preparation. A novel 1-(3-aminopropyl)-3-(4-vinylbenzyl)imidazolium 4-styrenesulfonate IL monomer was synthesized and copolymerized with 1,6-di(3-vinylimidazolium) hexane bishexafluorophosphate IL as cross-linking agent to prepare a cross-linked polymeric ionic liquids (PILs) monolith. Coupled to high-performance liquid chromatography (HPLC), the PILs monolith was used as a solid-phase microextraction (SPME) sorbent to extract some polar endocrine disrupting chemical (EDCs) such as estrogens, bisphenol A, and phthalate esters in aqueous samples. Preparation and extraction conditions were investigated and optimized to obtain satisfactory extraction efficiency. Limits of detection (LODs) of the proposed method for three steroid estrogens and bisphenol A were 0.25 and 0.2 µg L(-1), respectively, which were lower than or comparable to some other sample preparation methods. Intra- and inter-day repeatability for all the analytes was 2.2-12%. The monolith-to-monolith repeatability was 7.4-15%. The extraction performance of the method for analysis of target estrogens in treated domestic wastewater was investigated and compared with a dispersive liquid-liquid microextraction (DLLME) method. The proposed SPME method provided better sensitivity and higher resistance to matrix interferences.


Assuntos
Cromatografia Líquida de Alta Pressão/instrumentação , Disruptores Endócrinos/isolamento & purificação , Líquidos Iônicos/química , Microextração em Fase Sólida/instrumentação , Poluentes Químicos da Água/isolamento & purificação , Água/química , Adsorção , Disruptores Endócrinos/análise , Disruptores Endócrinos/química , Desenho de Equipamento , Análise de Falha de Equipamento , Polímeros/química , Manejo de Espécimes/instrumentação , Integração de Sistemas , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/química
4.
Anal Bioanal Chem ; 404(1): 79-88, 2012 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-22653423

RESUMO

This paper reports the preparation of dapsone (DDS) imprinted polymer layer-coated silica submicron particles (SiO(2)) combined with chemiluminescence (CL) toward analysis of tracing DDS in practical samples. To induce the selective occurrence of surface polymerization, the amino groups were first grafted at the surface of SiO(2) by the (3-aminopropyl)triethoxysilane (APTES). The molecularly imprinted polymers (MIP) were coated at the surface of modified SiO(2) by the graft copolymerization. After the removal of templates, recognition sites of DDS were exposed in the polymer layers. The DDS-imprinted products were characterized by FT-IR, SEM, TEM, dynamic adsorption, and static adsorption tests. The proximity between the thickness of MIP layer and the spatial size of DDS indicated that the imprinted sites almost situated at the surface of MIP, leading to rapid adsorption saturation within 90 min. The apparent maximum binding amount of MIP toward DDS was evaluated as 14.98 mg·g(-1), which was much higher than that of non-molecularly imprinted polymers. The CL sensor provided a wide linear range for DDS within 1.0 × 10(-6) to 1.0 × 10(-4) mol·L(-1) with a detection limit of 5.27 × 10(-7) mol·L(-1) and the relative standard deviation of 1.8 % (n = 11) by determinations of 5.0 × 10(-6) mol·L(-1) DDS. This method was applied to determine DDS in urine samples and satisfactory results were obtained.


Assuntos
Antibacterianos/análise , Técnicas Biossensoriais/métodos , Dapsona/análise , Análise de Injeção de Fluxo/métodos , Polímeros/química , Adsorção , Antibacterianos/urina , Técnicas Biossensoriais/instrumentação , Dapsona/urina , Análise de Injeção de Fluxo/instrumentação , Luminescência , Impressão Molecular , Polímeros/síntese química , Dióxido de Silício/química , Urina/química
5.
Talanta ; 186: 238-247, 2018 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-29784355

RESUMO

In this work, a highly selective and sensitive chemiluminescence (CL) biosensor was prepared for adenosine (AD) detection based on carbon quantum dots (CQDs) catalyzing the CL system of luminol-H2O2 under alkaline environment and CQDs was released from the surface of AD aptamers functionalized graphene @ magnetic ß-cyclodextrin polymers (GO@Fe3O4@ß-CD@A-Apt). Firstly, GO@Fe3O4@ß-CD and CQDs were prepared and characterized by transmission electron microscopy (TEM), scanning electron microscope (SEM), UV-Vis absorption spectra (UV), fluorescence spectra (FL), fourier transform infrared (FTIR) and X-ray powder diffraction (XRD). For GO@Fe3O4@ß-CD, Fe3O4 was easy to separate, GO had good biocompatibility and large specific surface area, and ß-CD further increased the specific surface area of the adenosine polymers (A-Apt) to provided larger binding sites to A-Apt. Then, A-Apt was modified on the surface of GO@Fe3O4@ß-CD while CQDs was modified by ssDNA (a single stranded DNA partially complementary to A-Apt). The immobilization property (GO@Fe3O4@ß-CD to A-Apt) and the adsorption property (GO@Fe3O4@ß-CD@A-Apt to CQDs-ssDNA) were sequentially researched. The base-supported chain-like polymers - GO@Fe3O4@ß-CD@A-Apt/CQDs-ssDNA was successfully obtained. When AD existed, CQDs-ssDNA was released from the surface of GO@Fe3O4@ß-CD@A-Apt and catalyzed CL. After that, under optimized CL conditions, AD could be measured with the linear concentration range of 5.0 × 10-13-5.0 × 10-9 mol/L and the detection limit of 2.1 × 10-13 mol/L (3δ) while the relative standard deviation (RSD) was 1.4%. Finally, the GO@Fe3O4@ß-CD@A-Apt/CQDs-ssDNA-CL biosensor was used for the determination of AD in urine samples and recoveries ranged from 98.6% to 101.0%. Those satisfactory results illustrated the proposed CL biosensor could achieve highly selective, sensitive and reliable detection of AD and revealed potential application for AD detection in monitoring and diagnosis of human cancers.


Assuntos
Adenosina/análise , Aptâmeros de Nucleotídeos/química , Técnicas Biossensoriais , Medições Luminescentes , Polímeros/química , beta-Ciclodextrinas/química , Carbono/química , Catálise , Grafite/química , Humanos , Luminescência , Campos Magnéticos , Pontos Quânticos/química
6.
Anal Chim Acta ; 1043: 132-141, 2018 Dec 28.
Artigo em Inglês | MEDLINE | ID: mdl-30392661

RESUMO

In this work, a highly sensitive and selective chemiluminescence (CL) aptasensor was prepared for thrombin (THR) detection based on aptamer-conjugated and hemin/G-quadruplex DNAzyme signal-amplified carbon fiber composite (HG-DNAzyme/T-Apt/SiO2@GO@CF). Initially, SiO2@GO@CF was successfully prepared and characterized by Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). Thrombin aptamer (T-Apt) as an identification element and simulated enzyme - hemin/G-quadruplex DNAzyme (HG-DNAzyme) as a signal-amplified material, were applied in the CL aptasensor. Then, the immobilization properties of SiO2@GO@CF and adsorption properties of T-Apt/SiO2@GO@CF were studied. Lastly, HG-DNAzyme/T-Apt/SiO2@GO@CF was applied in construction of the CL aptasensor. When THR existed, HG-DNAzyme was desorbed from the surface of T-Apt/SiO2@GO@CF and catalyzed the CL system of luminol-H2O2. Under optimized CL conditions, THR was measured with the linear concentration range of 1.5 × 10-14 to 2.5 × 10-11 moL/L and the detection limit of 6.3 × 10-15 moL/L (3δ). The proposed CL aptasensor was used to the determination of THR in human serum samples and recoveries ranged from 99.0% to 102.4%. Those satisfactory results illustrated the CL aptasensor could achieve highly sensitive and selective detection of THR and revealed potential application in practical samples.


Assuntos
Aptâmeros de Nucleotídeos/química , Carbono/química , DNA Catalítico/metabolismo , Medições Luminescentes/métodos , Trombina/análise , Técnicas Biossensoriais , Fibra de Carbono , DNA Catalítico/química , Quadruplex G , Hemina/química , Humanos , Peróxido de Hidrogênio/química , Limite de Detecção , Luminol/química , Dióxido de Silício/química
7.
Int J Biol Macromol ; 107(Pt A): 957-964, 2018 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-28939516

RESUMO

Magnetic hydroxyethyl cellulose/ionic liquid (MHEC/IL) materials were fabricated through a facile and fast process and their application as excellent adsorbents for hydroquinone was also demonstrated. The thermal stability, chemical structure and magnetic property of the MHEC/IL were characterized by the Scanning electron microscope (SEM), Transmission Electron Microscope (TEM), Fourier transform infrared spectrometer (FT-IR) and X-ray diffraction (XRD), respectively. The adsorbents were used for the removal of hydroquinone from simulated wastewater with a fast solid-liquid separation in the presence of external magnetic field. The influence of various analytical parameters on the adsorption of hydroquinone such as pH, contact time and initial ion concentration were studied in detail. The results showed that the maximum adsorption capacity was 335.68mgg-1, observed at pH 5 and temperature 30°C. Equilibrium adsorption was achieved within 30min. The kinetic data, obtained at the optimum pH 5, could be fitted with a pseudo-second order equation. Adsorption process could be well described by Freundlich adsorption isotherms. The obtained results indicated that the impregnation of the room temperature IL significantly enhances the removal efficiency of hydroquinone. The MHEC/IL may be suitable materials in phenols pollution cleanup if they are synthesized in largescale and at low price in near future.


Assuntos
Celulose/análogos & derivados , Hidroquinonas/isolamento & purificação , Líquidos Iônicos/química , Águas Residuárias/química , Adsorção , Celulose/química , Quitosana/química , Concentração de Íons de Hidrogênio , Hidroquinonas/química , Hidroquinonas/toxicidade , Magnetismo , Fenóis/química , Fenóis/toxicidade , Espectroscopia de Infravermelho com Transformada de Fourier , Temperatura , Águas Residuárias/toxicidade , Poluentes Químicos da Água/química , Poluentes Químicos da Água/toxicidade , Difração de Raios X
8.
J Chromatogr A ; 1517: 209-214, 2017 Sep 29.
Artigo em Inglês | MEDLINE | ID: mdl-28844301

RESUMO

Carbon fibers (CFs) were functionalized with graphene oxide (GO) by an electrophoretic deposition (EPD) method for in-tube solid-phase microextraction (SPME). GO-CFs were filled into a poly(ether ether ketone) (PEEK) tube to obtain a fibers-in-tube SPME device, which was connected with high performance liquid chromatography (HPLC) equipment to build online SPME-HPLC system. Compared with CFs, GO-CFs presented obviously better extraction performance, due to excellent adsorption property and large surface area of GO. Using ten polycyclic aromatic hydrocarbons (PAHs) as model analytes, the important extraction conditions were optimized, such as sample flow rate, extraction time, organic solvent content and desorption time. An online analysis method was established with wide linear range (0.01-50µgL-1) and low detection limits (0.001-0.004µgL-1). Good sensitivity resulted from high enrichment factors (1133-3840) of GO-CFs in-tube device towards PAHs. The analysis method was used to online determination of PAHs in wastewater samples. Some target analytes were detected and relative recoveries were in the range of 90.2-112%. It is obvious that the proposed GO-CFs in-tube device was an efficient extraction device, and EPD could be used to develop nanomaterials functionalized sorbents for sample preparation.


Assuntos
Carbono/química , Monitoramento Ambiental/métodos , Grafite/química , Microextração em Fase Sólida/métodos , Adsorção , Fibra de Carbono , Cromatografia Líquida de Alta Pressão , Cetonas/química , Limite de Detecção , Óxidos/química , Hidrocarbonetos Policíclicos Aromáticos/análise , Solventes/química , Águas Residuárias/química
9.
Int J Biol Macromol ; 99: 578-585, 2017 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-28283454

RESUMO

A simple chemical bonding method to synthesize magnetic cellulose-poly(dopamine) (Fe3O4@CMC@PDA) was reported. The adsorption behaviors of resorcinol in aqueous solution on Fe3O4@CMC@PDA were systematically investigated. As the results shown that, with the advantage of high surface area, abundant hydroxyl and amino groups of Fe3O4@CMC@PDA, and the magnetic property of Fe3O4, the resorcinol can be easily and rapidly extracted from the water by magnetic attraction under investigation. The adsorption equilibrium of Fe3O4@CMC@PDA for resorcinol corresponded with Freundlich isotherm, and the novel adsorbent exhibited better resorcinol removal efficiency in solutions with low pH. It was found that the resorcinol adsorption performance of Fe3O4@CMC@PDA strongly depends on their surface charge concentration and specific surface area. These results provide evidences for estimating and optimizing the removal of phenols from the wastewater by using of Fe3O4@CMC@PDA composites in the future.


Assuntos
Celulose/química , Indóis/química , Imãs/química , Polímeros/química , Resorcinóis/química , Resorcinóis/isolamento & purificação , Poluentes Químicos da Água/química , Purificação da Água/métodos , Adsorção , Compostos Férricos/química , Concentração de Íons de Hidrogênio , Cinética , Modelos Moleculares , Conformação Molecular , Termodinâmica , Águas Residuárias/química
10.
Artigo em Inglês | MEDLINE | ID: mdl-28147299

RESUMO

In this work, a chemiluminescence (CL) biosensor was prepared for ultrasensitive determination of deoxyribonucleic acid (DNA) based on the adsorption recognition function between core-shell Fe3O4@SiO2 - graphene oxide (Fe3O4@SiO2@GO) polymers and DNA. The Fe3O4@SiO2@GO polymers were composed by GO and magnetite nanoparticles. And the core-shell polymers were confirmed by Scanning Electron Microscope (SEM), X-Ray Powder Diffraction (XRD) and Fourier Transform Infrared (FTIR). Then Fe3O4@SiO2@GO was modified by DNA. Based on the principle of complementary base, Fe3O4@SiO2@GO-DNA was introduced to the CL system and the selectivity, sensitivity of DNA detection was significantly improved. The adsorption properties of Fe3O4@SiO2@GO to DNA were researched through the adsorption equilibrium, adsorption kinetic and thermodynamics. Under optimized CL conditions, DNA could be assayed with the linear concentration range of 5.0×10-12-2.5×10-11mol/L. The detection limit was 1.7×10-12mol/L (3δ) and the relative standard deviation (RSD) was 3.1%. The biosensor was finally used for the determination of DNA in laboratory samples and recoveries ranged from 99% to 103%. The satisfactory results revealed the potential application of Fe3O4@SiO2@GO-DNA-CL biosensor in the diagnosis and the treatment of human genetic diseases.


Assuntos
Técnicas Biossensoriais/métodos , DNA/análise , Compostos Férricos/química , Grafite/química , Medições Luminescentes/métodos , Polímeros/química , Dióxido de Silício/química , Adsorção , Cinética , Espectroscopia de Infravermelho com Transformada de Fourier , Temperatura
11.
J Chromatogr A ; 1393: 8-17, 2015 May 08.
Artigo em Inglês | MEDLINE | ID: mdl-25840662

RESUMO

In situ anion exchange has been proved to be an efficient method for facile modification of polymeric ionic liquids (PILs)-based stationary phases. In this work, an on-fiber anion exchange process was utilized to tune the extraction performance of a multi-walled carbon nanotubes (MWCNTs)-poly(1-vinyl-3-octylimidazolium bromide) (poly(VOIm(+)Br(-)))-coated solid-phase microextraction (SPME) fiber. MWCNTs were first coated onto the stainless steel wire through a layer-by-layer fabrication method and then the PILs were coated onto the MWCNTs physically. Anion of the MWCNTs-poly(VOIm(+)Br(-)) fiber was changed into bis(triflroromethanesulfonyl)imide (NTf2(-)) and 2-naphthalene-sulfonate (NapSO3(-)) by on-fiber anion exchange. Coupled to gas chromatography, the MWCNTs-poly(VOIm(+)Br(-)) fiber showed acceptable extraction efficiency for hydrophilic and hydrogen-bonding-donating alcohols, with limits of detection (LODs) in the range of 0.005-0.05µgmL(-1); after the anion exchange with NTf2(-), the obtained MWCNTs-poly(VOIm(+)NTf2(-)) fiber brought wide linear ranges for hydrophobic n-alkanes with correlation coefficient (R) ranging from 0.994 to 0.997; aromatic property of the fiber was enhanced by aromatic NapSO3(-) anions to get sufficient extraction capacity for phthalate esters and halogenated aromatic hydrocarbons. The MWCNTs-poly(VOIm(+)NapSO3(-)) fiber was finally applied to determine several halogenated aromatic hydrocarbons in groundwater of industrial park.


Assuntos
Líquidos Iônicos/química , Nanotubos de Carbono/química , Polivinil/química , Microextração em Fase Sólida/métodos , Álcoois/análise , Ânions , Cromatografia Gasosa/métodos , Ésteres , Água Subterrânea/química , Hidrocarbonetos Halogenados/análise , Ligação de Hidrogênio , Troca Iônica , Limite de Detecção , Ácidos Ftálicos/análise , Poluentes Químicos da Água/análise
12.
Talanta ; 131: 354-60, 2015 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-25281114

RESUMO

A novel composite of magnetic graphene oxide @ gold nanoparticles-molecular imprinted polymers (MGO@AuNPs-MIPs) was synthesized and applied as a molecular recognition element to construct dibutyl phthalate (DBP) electrochemical sensor. The composite of MGO@AuNPs was first synthesized using coprecipitation and self-assembly technique. Then the template molecules (DBP) were absorbed at the MGO@AuNPs surface due to their excellent affinity, and subsequently, selective copolymerization of methacrylic acid and ethylene glycol dimethacrylate was further achieved at the MGO@AuNPs surface. Potential scanning was presented to extract DBP molecules from the imprinted polymers film rapidly and completely. As a consequence, an electrochemical sensor for highly sensitive and selective detection of DBP was successfully constructed as demonstration based on the synthesized MGO@AuNPs-MIPs composite. Under optimal experimental conditions, selective detection of DBP in a linear concentration range of 2.5 × 10(-9)-5.0 × 10(-6)mol/L was obtained. The new DBP electrochemical sensor also exhibited excellent repeatability, which expressed as relative standard deviation (RSD) was about 2.50% for 30 repeated analyses of 2.0 × 10(-6)mol/L DBP.


Assuntos
Técnicas Biossensoriais/métodos , Dibutilftalato/análise , Técnicas Eletroquímicas/métodos , Ouro/química , Grafite/química , Magnetismo , Nanopartículas Metálicas/química , Impressão Molecular , Polímeros/química , Eletrodos , Limite de Detecção
13.
Artigo em Inglês | MEDLINE | ID: mdl-25574658

RESUMO

Based on silanized magnetic graphene oxide-molecularly imprinted polymer (Si-MG-MIP), a sensitive and selective chemiluminescence sensor for dopamine measurement was developed. Si-MG-MIP, in which silanes was introduced to improve the mass transfer, graphene oxide was employed to improve absorption capacity, Fe3O4 nanoparticles were applied for separation easily and molecularly imprinted polymer was used to improve selectivity, demonstrated the advantages of the sensor. All the composites were confirmed by SEM, TEM, XRD and FTIR. Under the optimal conditions of chemiluminescence, dopamine could be assayed in the range of 8.0-200.0 ng/mL with a correlation coefficient of linear regression of 0.9970. The detection limit was 1.5 ng/mL (3δ) and the precision for 11 replicate detections of 80.0 ng/mL dopamine was 3.4% (RSD). When the sensor was applied in determining dopamine in actual samples, recovery ranged from 94% to 110%, which revealed that the results were satisfactory.


Assuntos
Dopamina/análise , Grafite/química , Medições Luminescentes/instrumentação , Fenômenos Magnéticos , Impressão Molecular/métodos , Óxidos/química , Polímeros/química , Silanos/química , Dopamina/urina , Humanos , Reciclagem , Espectroscopia de Infravermelho com Transformada de Fourier , Difração de Raios X
14.
Talanta ; 114: 60-5, 2013 Sep 30.
Artigo em Inglês | MEDLINE | ID: mdl-23953442

RESUMO

A novel solid-phase microextraction (SPME) fiber based on carbon nanotubes-titanium oxide (CNT-TiO2) composite coating bonded onto stainless steel wire was prepared via electroless plating and sol-gel techniques. The SPME coating was characterized by scanning electron microscopy and Raman microscopy. Coupled to gas chromatography (GC), the fiber was investigated with seven polycyclic aromatic hydrocarbons (PAHs) in direct-immersion mode. The SPME-GC analytical method was evaluated under optimized extraction conditions. Compared with other reports, higher sensitivity (LODs, 0.002-0.004 µg L(-1)) and better linear range (0.01-100 and 0.01-200 µg L(-1)) were obtained by the proposed method. The fiber exhibited high thermal stability to 300 °C and excellent durability in HCl and NaOH solutions. The as-established SPME-GC method was used to analyze the real water samples and satisfactory results were obtained.


Assuntos
Nanotubos de Carbono/química , Hidrocarbonetos Policíclicos Aromáticos/análise , Aço Inoxidável/química , Titânio/química , Poluentes Químicos da Água/análise , Monitoramento Ambiental , Microscopia Eletrônica de Varredura , Nanotubos de Carbono/ultraestrutura , Concentração Osmolar , Chuva/química , Rios/química , Microextração em Fase Sólida/instrumentação
15.
J Chromatogr A ; 1300: 173-9, 2013 Jul 26.
Artigo em Inglês | MEDLINE | ID: mdl-23684146

RESUMO

A novel carbon nanoparticles-coated solid-phase microextraction (SPME) fiber was prepared via a simple and low-cost flame-based preparation process, with stainless steel wire as support. Surface characteristic of the fiber was studied with scanning electron microscope. A nano-scaled brushy structure was observed. Coupled to gas chromatography (GC), the fiber was used to extract phthalate esters (PAEs) and polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Analytical performances of the proposed method were investigated under the optimum extraction conditions (extraction temperature, 40°C; content of KCl, 30% (w/v); extraction time, 50min for PAEs and 40min for PAHs) and compared with other reports for the same analytes. Calibration ranges were 0.06-500µgL(-1) for di-n-butyl phthalate (DBP), and 0.1-300µgL(-1) for di-cyclohexyl phthalate (DCHP) and di-(2-ethyl-hexyl) phthalate (DEHP). For the eight PAHs, good linearity was obtained ranging from 0.01 to 150µgL(-1). Limits of detection were 0.005µgL(-1) for three PAEs and 0.001-0.003µgL(-1) for eight PAHs. The fiber exhibited excellent stability. It can be used for 100 times with RSDs of extraction efficiency less than 22.4%. The as-established SPME-GC method was applied to determine PAEs in food-wrap and PAHs in cigarette ash and snow water, and satisfactory results were obtained. The carbon nanoparticles-coated SPME fiber was efficient for sampling of organic compounds from aqueous samples.


Assuntos
Carbono/química , Nanopartículas/química , Microextração em Fase Sólida/instrumentação , Microextração em Fase Sólida/métodos , Cromatografia Gasosa/métodos , Poluentes Ambientais/análise , Poluentes Ambientais/isolamento & purificação , Temperatura Alta , Limite de Detecção , Ácidos Ftálicos/análise , Ácidos Ftálicos/isolamento & purificação , Hidrocarbonetos Policíclicos Aromáticos/análise , Hidrocarbonetos Policíclicos Aromáticos/isolamento & purificação , Cloreto de Potássio/química , Reprodutibilidade dos Testes , Aço Inoxidável
16.
J Pharm Biomed Anal ; 75: 123-9, 2013 Mar 05.
Artigo em Inglês | MEDLINE | ID: mdl-23246931

RESUMO

A microflow chemiluminescence (CL) sensor for determination of dibutyl phthalate (DBP) based on magnetic molecularly imprinted polymer (MMIP) as recognition element was fabricated. Briefly, a hydrophilic molecularly imprinted polymer layer was produced at the surface of Fe3O4@SiO2 magnetic nanoparticles (MNPs) via combination of molecular imprinting and reversible stimuli responsive hydrogel. In this protocol, the initial step involved co-precipitation of Fe²âº and Fe³âº in an ammonia solution. Silica was then coated on the Fe3O4 nanoparticles using a sol-gel method to obtain silica shell magnetic nanoparticles. The MMIP was synthesized using methacrylic acid (MAA) as functional monomer and ethylene glycol dimethacrylate (EGDMA) as cross-linker and 2,2-azobisisobutyronitrile (AIBN) as initiator in chloroform. Then the synthesized MMIP and magnetic non-molecular imprinted polymers (MNIP) were employed as recognition by packing into lab-made straight shape tubes, connected in CL analyzer for establishing the novel sensor with a single channel syringe pump. And a mixer for hydrolyzing of DBP was followed. Based on this experiment principle, DBP was determined indirectly. And the MMIP showed satisfactory recognition capacity to DBP, resulting to the wide linear range of 3.84 × 10⁻8 to 2.08 × 10⁻5 M and the low detection limit of 2.09 × 10⁻9 M (3σ) for DBP. The relative standard deviation (RSD) for DBP (3.20 × 10⁻6 M) was 1.40% (n=11). Besides improving sensitivity and selectivity, the sensor was reusable. The proposed DBP-MMIP-CL sensor has been successfully applied to determine DBP in drink samples.


Assuntos
Carcinógenos Ambientais/análise , Dibutilftalato/análise , Plastificantes/análise , Bebidas/análise , Técnicas Biossensoriais , Carcinógenos Ambientais/química , Dibutilftalato/química , Contaminação de Alimentos , Frutas/química , Hidrogel de Polietilenoglicol-Dimetacrilato/química , Hidrólise , Interações Hidrofóbicas e Hidrofílicas , Limite de Detecção , Medições Luminescentes , Nanopartículas de Magnetita/química , Teste de Materiais , Impressão Molecular , Plastificantes/química , Polímeros/química , Reprodutibilidade dos Testes , Reologia/instrumentação , Dióxido de Silício/química , Propriedades de Superfície
17.
Artigo em Inglês | MEDLINE | ID: mdl-22112574

RESUMO

A novel molecular imprinting-chemiluminescence (MIP-CL) sensor for the determination of L-phenylalanine (Phe) using molecularly imprinted polymer (MIP) as recognition element is reported. The Phe-MIP was synthesized using acrylamide (AM) as functional monomer and ethylene glycol dimethacrylate (EGDMA) as cross-linker, 2,2-azobisisobutyronitrile (AIBN) as initiator and the polymers' properties were characterized. Then the synthesized MIP was employed as recognition element by packing into flow cell to establish a novel flow injection CL sensor. The CL intensity responded linearly to the concentration of Phe in the range 1.3 × 10(-6) to 5.44 × 10(-4) mol/L with a detection limit of 6.23 × 10(-7) mol/L (3σ), which is lower than that of conventional methods. The sensor is reusable and has a great improvement in sensitivity and selectivity for CL analysis. As a result, the new MIP-CL sensor had been successfully applied to the determination of Phe in samples.


Assuntos
Luminescência , Microesferas , Impressão Molecular/métodos , Sistemas On-Line , Fenilalanina/análise , Polímeros/química , Animais , Técnicas Biossensoriais , Análise de Injeção de Fluxo , Microscopia Eletrônica de Varredura , Leite/química , Fenilalanina/química , Reciclagem , Análise de Regressão , Espectrofotometria Infravermelho
18.
Anal Chim Acta ; 718: 84-91, 2012 Mar 09.
Artigo em Inglês | MEDLINE | ID: mdl-22305902

RESUMO

A novel flow injection chemiluminescence (FI-CL) sensor for determination of sulfadiazine (SDZ) using core-shell magnetic molecularly imprinted polymers (MMIPs) as recognition element is developed. Briefly, a hydrophilic MMIPs layer was produced at the surface of Fe(3)O(4)@SiO(2) magnetic nanoparticles (MNPs) via combination of molecular imprinting and reversible stimuli responsive hydrogel. And it provided the MMIPs with excellent adsorption capacity and rapid adsorption rate due to the imprinted sites mostly situated on the surface of MMIPs. Then the prepared SDZ-MMIPs were packed into flow cell to establish a novel FI-CL sensor. The sensor provided a wide linear range for SDZ of 4.0×10(-7) to 1.0×10(-4) mol L(-1) with a detection limit of 1.54×10(-7) mol L(-1). And the relative standard deviation (RSD) for the determination of 1.0×10(-6) mol L(-1) SDZ was 2.56% (n=11). The proposed method was applied to determine SDZ in urine samples and satisfactory results were obtained.


Assuntos
Anti-Infecciosos/análise , Análise de Injeção de Fluxo/instrumentação , Medições Luminescentes/instrumentação , Impressão Molecular , Nanopartículas/química , Sulfadiazina/análise , Desenho de Equipamento , Análise de Injeção de Fluxo/métodos , Limite de Detecção , Medições Luminescentes/métodos , Imãs/química , Nanopartículas/ultraestrutura , Polímeros/química
19.
Anal Chim Acta ; 744: 75-81, 2012 Sep 26.
Artigo em Inglês | MEDLINE | ID: mdl-22935377

RESUMO

A chemiluminescence (CL) array sensor for determination of benzenediol isomers simultaneously using the system of luminol-NaOH-H(2)O(2) based on a graphene-magnetite-molecularly imprinted polymer (GM-MIP) is described. Use of graphene in the GM-MIP thus prepared is helpful to improve the adsorption capacity, while use of magnetite nanoparticles can facilitate the isolation of GM-MIP at end of their synthesis, and rendering easier the use of the polymers in the array sensor. The adsorption performance and properties were characterized. The GM-MIP was used to increase the selectivity in CL analysis. In addition, the sensor was reusable and of good selectivity and adsorption capacity. The array sensor was finally used for the determination of hydroquinone, resorcinol and catechol in waste water samples simultaneously.


Assuntos
Catecóis/análise , Óxido Ferroso-Férrico/química , Grafite/química , Hidroquinonas/análise , Medições Luminescentes/métodos , Impressão Molecular , Resorcinóis/análise , Adsorção , Peróxido de Hidrogênio/química , Medições Luminescentes/instrumentação , Luminol/química , Polímeros/síntese química , Polímeros/química , Hidróxido de Sódio/química , Propriedades de Superfície
20.
Talanta ; 98: 226-30, 2012 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-22939151

RESUMO

A new method for determination of L-tryptophan (L-try) using the flow injection chemiluminescence (FI-CL) system of KMnO(4)-SnCl(2)-CHOH based on a graphene oxide-magnetite-molecularly imprinted polymer (GM-MIP) is described. The L-try GM-MIP was synthesized using graphene oxide (G) which improved the adsorption capacity as carrier, and magnetite nanoparticles which made the polymers easier to use in the sensor. The adsorption performance and properties were characterized. The GM-MIP was used in CL analysis to increase the selectivity and the possible mechanism was also discussed. The CL sensor responded linearly to the concentration of L-try over the range from 2.10×10(-7) to 7.09×10(-4) M with a detection limit of 2.11×10(-8) M (3σ). The relative standard deviation (RSD) for the determination of 3.0×10(-5) M L-try was 2.40% (n=11). On the basis of speediness and sensitivity, the sensor is reusable and shows a great improvement in selectivity and adsorption capacity over other sensors. The sensor has been used for the determination of L-try in drug samples.


Assuntos
Óxido Ferroso-Férrico/química , Grafite/química , Impressão Molecular , Polímeros/química , Medicamentos sob Prescrição/química , Triptofano/análise , Adsorção , Análise de Injeção de Fluxo , Humanos , Limite de Detecção , Luminescência , Medições Luminescentes , Óxidos , Permanganato de Potássio/química , Compostos de Estanho/química
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