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1.
Nanomaterials (Basel) ; 11(1)2020 Dec 24.
Artigo em Inglês | MEDLINE | ID: mdl-33374367

RESUMO

Non-magnetic and magnetic low-cost biochar (BC) from date pits (DP) were applied to remove tigecycline (TIGC) from TIGC-artificially contaminated water samples. Pristine biochar from DP (BCDP) and magnetite-decorated biochar (MBC-DP) were therefore prepared. Morphologies and surface chemistries of BCDP and MBC-DP were explored using FT-IR, Raman, SEM, EDX, TEM, and BET analyses. The obtained IR and Raman spectra confirmed the presence of magnetite on the surface of the MBC-DP. SEM results showed mesoporous surface for both adsorbents. BET analysis indicated higher amount of mesopores in MBC-DP. Box-Behnken (BB) design was utilized to optimize the treatment variables (pH, dose of the adsorbent (AD), concentration of TIGC [TIGC], and the contact time (CT)) and maximize the adsorptive power of both adsorbents. Higher % removal (%R), hitting 99.91%, was observed using MBC-DP compared to BCDP (77.31%). Maximum removal of TIGC (99.91%) was obtained using 120 mg/15 mL of MBC-DP for 10 min at pH 10. Equilibrium studies showed that Langmuir and Freundlich isotherms could best describe the adsorption of TIGC onto BCDP and MBC-DP, respectively, with a maximum adsorption capacity (qmax) of 57.14 mg/g using MBC-DP. Kinetics investigation showed that adsorption of TIGC onto both adsorbents could be best-fitted to a pseudo-second-order (PSO) model.

2.
Molecules ; 25(22)2020 Nov 19.
Artigo em Inglês | MEDLINE | ID: mdl-33228258

RESUMO

In the current study, eco-structured and efficient removal of the veterinary fluoroquinolone antibiotic sarafloxacin (SARA) from wastewater has been explored. The adsorptive power of four agro-wastes (AWs) derived from pistachio nutshells (PNS) and Aloe vera leaves (AV) as well as the multi-walled carbon nanotubes (MWCNTs) has been assessed. Adsorbent derived from raw pistachio nutshells (RPNS) was the most efficient among the four tested AWs (%removal '%R' = 82.39%), while MWCNTs showed the best adsorptive power amongst the five adsorbents (%R = 96.20%). Plackett-Burman design (PBD) was used to optimize the adsorption process. Two responses ('%R' and adsorption capacity 'qe') were optimized as a function of four variables (pH, adsorbent dose 'AD' (dose of RPNS and MWCNTs), adsorbate concentration [SARA] and contact time 'CT'). The effect of pH was similar for both RPNS and MWCNTs. Morphological and textural characterization of the tested adsorbents was carried out using FT-IR spectroscopy, SEM and BET analyses. Conversion of waste-derived materials into carbonaceous material was investigated by Raman spectroscopy. Equilibrium studies showed that Freundlich isotherm is the most suitable isotherm to describe the adsorption of SARA onto RPNS. Kinetics' investigation shows that the adsorption of SARA onto RPNS follows a pseudo-second order (PSO) model.


Assuntos
Agricultura , Ciprofloxacina/análogos & derivados , Nanotubos de Carbono/química , Águas Residuárias/química , Poluentes Químicos da Água/isolamento & purificação , Adsorção , Análise de Variância , Ciprofloxacina/química , Ciprofloxacina/isolamento & purificação , Concentração de Íons de Hidrogênio , Cinética , Nanotubos de Carbono/ultraestrutura , Pistacia/química , Espectroscopia de Infravermelho com Transformada de Fourier , Análise Espectral Raman , Termogravimetria
3.
Appl Spectrosc ; 72(2): 241-250, 2018 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-28905634

RESUMO

Microspectroscopic techniques are widely used to complement histological studies. Due to recent developments in the field of chemical imaging, combined chemical analysis has become attractive. This technique facilitates a deepened analysis compared to single techniques or side-by-side analysis. In this study, rat brains harvested one week after induction of photothrombotic stroke were investigated. Adjacent thin cuts from rats' brains were imaged using Fourier transform infrared (FT-IR) microspectroscopy and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The LA-ICP-MS data were normalized using an internal standard (a thin gold layer). The acquired hyperspectral data cubes were fused and subjected to multivariate analysis. Brain regions affected by stroke as well as unaffected gray and white matter were identified and classified using a model based on either partial least squares discriminant analysis (PLS-DA) or random decision forest (RDF) algorithms. The RDF algorithm demonstrated the best results for classification. Improved classification was observed in the case of fused data in comparison to individual data sets (either FT-IR or LA-ICP-MS). Variable importance analysis demonstrated that both molecular and elemental content contribute to the improved RDF classification. Univariate spectral analysis identified biochemical properties of the assigned tissue types. Classification of multisensor hyperspectral data sets using an RDF algorithm allows access to a novel and in-depth understanding of biochemical processes and solid chemical allocation of different brain regions.


Assuntos
Isquemia Encefálica/diagnóstico por imagem , Isquemia Encefálica/patologia , Processamento de Imagem Assistida por Computador/métodos , Espectrometria de Massas/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Algoritmos , Animais , Encéfalo/diagnóstico por imagem , Encéfalo/patologia , Árvores de Decisões , Análise dos Mínimos Quadrados , Masculino , Ratos , Ratos Sprague-Dawley
4.
Phys Med ; 30(2): 221-7, 2014 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-23850104

RESUMO

Stability and molecular size of the DNA double helical structure were studied on an aqueous solution of DNA after exposure to high power doses of continuous wave ultrasound at frequency of 20 kHz. Thermal transition spectrophotometry (UV-melting), constant-field gel electrophoresis (CFGE), differential scanning calorimetry (DSC) and dielectric properties measurements were used to evaluate the ultrasound-induced changes in the DNA double helical structure. The thermal transition spectrophotometry (UV-melting) and differential scanning calorimetry (DSC) results showed that ultrasound power caused loss of DNA double helical structure and the DNA double strands melting temperature decreased as the ultrasound power increased, indicating a decrease in the stability of the double helical structure of DNA. The constant-field gel electrophoresis (CFGE) results showed that the molecular size of the DNA fragments decreased as the ultrasound power increased. The dielectric data in the frequency range from 20 Hz to 100 kHz for the native DNA showed that dispersion at frequency of about 500 Hz resulted from polarization induced by counterions. The decrease in the dielectric increment indicated a decrease in length of DNA molecule after exposure to ultrasound power.


Assuntos
Fenômenos Biofísicos , DNA/química , DNA/genética , Sonicação/efeitos adversos , Animais , Bovinos , Fragmentação do DNA , Conformação de Ácido Nucleico , Risco , Soluções
5.
Biol Trace Elem Res ; 140(1): 103-13, 2011 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-20358307

RESUMO

The determinations of selenium isotopes in biological samples were performed using both inductively coupled plasma collision/reaction cell quadruple mass spectrometer (CRC-ICP-QMS) and inductively coupled plasma sector field mass spectrometers (SF-ICP-MS). To significantly decrease the argon-based interferences at m/z 74 ((36)Ar(38)Ar), 76 ((38)Ar(38)Ar, (40)Ar(36)Ar), 78 ((38)Ar(40)Ar), and 80 ((40)Ar(40)Ar), the gas-flow rates of a helium and hydrogen mixture used in the collision cell were optimized to 1.0 mL/min H(2) and 3.5 mL/min He. Under the optimized condition, the precisions for natural selenium isotope ratio measurements of both instruments were evaluated and compared using 100 ppb Se standard solution. A modified external calibration quantification method was applied for the simultaneous determination of clinically used enriched selinocompounds ((77)Se-selenate, (82)Se-selenite, (76)Se-methylseleninic acid(IV), (78)Se-methylselenonic acid(VI)) and to examine their fate in rat organs (liver, kidney, and lung).


Assuntos
Isótopos/análise , Espectrometria de Massas/instrumentação , Espectrometria de Massas/métodos , Selênio/análise , Distribuição Tecidual , Animais , Gases/química , Hélio/química , Hidrogênio/química , Isótopos/administração & dosagem , Rim/química , Fígado/química , Pulmão/química , Masculino , Ratos , Ratos Wistar , Selênio/administração & dosagem
6.
J Am Soc Mass Spectrom ; 14(4): 373-82, 2003 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-12686484

RESUMO

The utility of post-source decay (PSD) matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) was investigated for the structural analysis of phosphatidylcholine (PC). PC did not produce detectable negative molecular ion from MALDI, but positive ions were observed as both [PC+H](+) and [PC+Na](+). The PSD spectra of the protonated PC species contained only one fragment corresponding to the head group (m/z 184), while the sodiated precursors produced many fragment ions, including those derived from the loss of fatty acids. The loss of fatty acid from the C-1 position (sn-1) of the glycerol backbone was favored over the loss of fatty acid from the C-2 position (sn-2). Ions emanating from the fragmentation of the head group (phosphocholine) included [PC+Na-59](+), [PC+Na-183](+) and [PC+Na-205](+), which corresponded to the loss of trimethylamine (TMA), non-sodiated choline phosphate and sodiated choline phosphate, respectively. Other fragments reflecting the structure of the head group were observed at m/z 183, 146 and 86. The difference in the fragmentation patterns for the PSD of [PC+Na](+) compared to [PC+H](+) is attributed to difference in the binding of Na(+) and H(+). While the proton binds to a negatively charged oxygen of the phosphate group, the sodium ion can be associated with several regions of the PC molecule. Hence, in the sodiated PC, intermolecular interaction of the negatively charged oxygen of the phosphate group, along with sodium association at multiple sites, can lead to a complex and characteristic ion fragmentation pattern. The preferential loss of sn-1 fatty acid group could be explained by the formation of an energetically favorable six-member ring intermediate, as apposed to the five-member ring intermediate formed prior to the loss of sn-2 fatty acid group.


Assuntos
Fosfatidilcolinas/química , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por Matriz/métodos , Estrutura Molecular , Reprodutibilidade dos Testes
7.
Rapid Commun Mass Spectrom ; 17(1): 87-96, 2003.
Artigo em Inglês | MEDLINE | ID: mdl-12478559

RESUMO

Ionization and prompt fragmentation patterns of triacylglycerols, phospholipids (PLs) and galactolipids were investigated using matrix-assisted laser desorption/ionization (MALDI). Positive ions of non-nitrogen-containing lipids appeared only in the sodiated form, while nitrogen-containing lipids were detected as both sodiated and protonated adducts. Lipids containing acidic hydroxyls were detected as multiple sodium adducts or deprotonated ions in the positive and negative modes, respectively, with the exception of phosphatidylcholines. The positive MALDI spectra of triacylglycerols contained prompt fragments equivalent to the loss of RCOO(-) from the neutral molecules. Prompt fragment ions [PL-polar head](+) were observed in the positive MALDI spectra of all phospholipids except phosphatidylcholines. The phosphatidylcholines produced only a minor positive fragment corresponding to the head group itself (m/z 184). Galactolipids did not undergo prompt fragmentation. Post-source decay (PSD) was used to examine the source of prompt fragments. PSD fragment patterns indicated that the lipid prompt fragment ions did not originate from the observed molecular ions (sodiated or protonated), and suggested that the prompt fragmentation followed the formation of highly unstable, probably protonated, precursor ions. Pathways leading to the formation of prompt fragment ions are proposed.


Assuntos
Galactolipídeos/química , Fosfolipídeos/química , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por Matriz/métodos , Triglicerídeos/química , Íons , Estrutura Molecular , Prótons , Reprodutibilidade dos Testes
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