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1.
Genet Sel Evol ; 56(1): 3, 2024 Jan 03.
Artículo en Inglés | MEDLINE | ID: mdl-38172694

RESUMEN

BACKGROUND: The natural abundance of nitrogen (δ15N) and carbon (δ13C) isotopes in animal tissues are used to estimate an animal's efficiency in nitrogen utilization, and their feed conversion efficiency, especially in tropical grazing systems with prolonged protein restriction. It is postulated that selection for improving these two characteristics (δ15N and δ13C) would assist the optimisation of the adaptation in ever-changing environments, particularly in response to climate change. The aim of this study was to determine the heritability of δ15N and δ13C in the tail hair of tropically adapted beef cattle to validate their inclusion in genetic breeding programs. METHODS: In total, 492 steers from two breeds, Brahman (n = 268) and Droughtmaster (n = 224) were used in this study. These steers were managed in two mixed breed contemporary groups across two years (year of weaning): steers weaned in 2019 (n = 250) and 2020 (n = 242). Samples of tail switch hair representing hair segments grown during the dry season were collected and analysed for δ15N and δ13C with isotope-ratio mass spectrometry. Heritability and variance components were estimated in a univariate multibreed (and single breed) animal model in WOMBAT and ASReml using three generations of full pedigree. RESULTS: The estimated heritability of both traits was significantly different from 0, i.e. 0.43 ± 0.14 and 0.41 ± 0.15 for δ15N and δ13C, respectively. These traits had favourable moderate to high genetic and phenotypic correlations (- 0.78 ± 0.16 and - 0.40 ± 0.04, respectively). The study also provides informative single-breed results in spite of the limited sample size, with estimated heritability values of 0.37 ± 0.19 and 0.19 ± 0.17 for δ15N and δ13C in Brahman, and 0.36 ± 0.21 and 0.46 ± 0.22 for δ15N and δ13C in Droughtmaster, respectively. CONCLUSIONS: The findings of this study show, for the first time, that the natural abundances of both nitrogen and carbon isotopes in the tail hair in cattle may be moderately heritable. With further research and validation, tail hair isotopes can become a practical tool for the large-scale selection of more efficient cattle.


Asunto(s)
Nitrógeno , Cola (estructura animal) , Bovinos/genética , Animales , Isótopos de Carbono , Cola (estructura animal)/química , Fenotipo , Cabello
2.
Sensors (Basel) ; 22(23)2022 Dec 01.
Artículo en Inglés | MEDLINE | ID: mdl-36502062

RESUMEN

Assessment of cultural heritage assets is now extremely important all around the world. Non-destructive inspection is essential for preserving the integrity of artworks while avoiding the loss of any precious materials that make them up. The use of Infrared Thermography is an interesting concept since surface and subsurface faults can be discovered by utilizing the 3D diffusion inside the object caused by external heat. The primary goal of this research is to detect defects in artworks, which is one of the most important tasks in the restoration of mural paintings. To this end, machine learning and deep learning techniques are effective tools that should be employed properly in accordance with the experiment's nature and the collected data. Considering both the temporal and spatial perspectives of step-heating thermography, a spatiotemporal deep neural network is developed for defect identification in a mock-up reproducing an artwork. The results are then compared with those of other conventional algorithms, demonstrating that the proposed approach outperforms the others.


Asunto(s)
Redes Neurales de la Computación , Termografía , Termografía/métodos , Algoritmos , Calefacción
3.
J Sep Sci ; 42(8): 1620-1628, 2019 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-30758140

RESUMEN

In the present study, a supramolecular solvent was formed from reverse micelle aggregates of octanol. The proposed supramolecular solvent was used for rapid extraction of some antidepressants drugs including amitriptyline, imipramine, desipramine, maprotiline, sertraline, and doxepin from biological samples. Alkanol-based supramolecular solvents have a unique array of physicochemical properties, making them a very attractive alternative to replace organic solvents in analytical extractions. The parameters affecting the extraction of target analytes (i.e., the volume of tetrahydrofuran and octanol as the major components comprising the supramolecular solvent, chain length of alkanols, sample solution pH, salt addition, and ultrasonic time) were investigated and optimized by factor by factor optimization method. Under the optimum conditions, preconcentration factors of 470, 490, 460, 385, 370, and 430 were obtained for amitriptyline, doxepin, imipramine, desipramine, maprotiline, and sertraline, respectively. The linear ranges and coefficients of determination (R2 ) were obtained in the range of 0.01-100 µg/L and 0.9974-0.9991, respectively. Also the limits of detection (S/N = 3) of 0.003-0.03 µg/L, and precisions (n = 5) of 4.9-8.9% were calculated. Finally, the method was successfully applied for the extraction of antidepressant drugs in biological samples, and relative recoveries in the range of 91-102% were obtained.


Asunto(s)
Antidepresivos/aislamiento & purificación , Cromatografía de Gases y Espectrometría de Masas/métodos , Microextracción en Fase Líquida/métodos , Ultrasonido/métodos , Antidepresivos/sangre , Antidepresivos/orina , Furanos/química , Humanos , Límite de Detección , Octanoles/química , Solventes/química
4.
J Sep Sci ; 40(24): 4788-4795, 2017 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-29067793

RESUMEN

Liquid-phase microextraction based on gemini-based supramolecular solvent was successfully applied as a preconcentration step before gas chromatography with mass spectrometry. To eliminate the interferences of gemini surfactant, the analytes were back-extracted into an immiscible organic solvent in the presence of ultrasonic sound waves. Three phthalate esters (di-n-butyl-, butylbenzyl-, bis(2-ethylhexyl)-, and di-n-octyl phthalatic esters) were used as target analytes. The effective parameters on extraction efficiency of the target analytes (i.e., the amount of surfactant and volume of propanol as major components making up the supramolecular solvent, ionic strength, hexane volume, and ultrasound time) were investigated and optimized by a one-variable-at-a-time method. Under the optimum conditions, the preconcentration factors of the analytes were in the range of 95-182. The linear dynamic range of 0.05-200.00 µg/L with a correlation of determination of (R2 ) ≥ 0.9935 was obtained. The proposed method had an excellent limit of detection (S/N = 3) of 0.01 for di-n-octyl and 0.02 µg/L for butylbenzyl- and di-n-butyl-phthalatic ester. Good relative recoveries in the range of 85.7-105.2% guaranteed the accuracy of the amount of phthalates distinguished in the nonspiked samples.

5.
J Sep Sci ; 39(17): 3400-9, 2016 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-27384254

RESUMEN

A novel supramolecular solvent-based microextraction followed by high-performance liquid chromatography with ultraviolet detection method has been developed for the extraction and determination of two pyrethroid analytes, cyhalothrin and fenvalerate, in water and soil samples. The liquid-liquid-phase separation of surfactants has been used in analytical extraction. The surfactant-rich phase is a nano-structured liquid, recently named as a supramolecular solvent, generated from the amphiphiles. The alkyl carboxylic acid based supramolecular solvents were introduced before. Coacervates made up of gemini surfactant, consisting of two amphiphilic moieties, were first used as solvent. The effective parameters on extraction (i.e., type of organic solvent, the amount of surfactant and volume of tetrahydrofuran, sample solution pH, salt addition, ultrasonic and centrifugation time) were investigated and optimized. Under the optimum conditions, preconcentration factors of 110 and 145 were obtained for the analytes. The linearity was 0.5-200.0 µg/L with the correlation of determination of (R(2) ) ≥ 0.9984. The limit of detection of the method was (S/N = 3) 0.2 µg/L, and precisions in the range of 6.3-10.3% (RSDs, n = 5) were obtained. This method has been successfully applied to analyze real samples, and good recoveries in the range of 101.2-108.8% were obtained.

6.
J Sep Sci ; 38(2): 276-82, 2015 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-25376392

RESUMEN

A supramolecular solvent made up of nano-sized inverted hexagonal aggregates of 1-octanol is proposed for the microextraction of diphenylamine and its mono-nitrated derivatives in unburned single-base propellants. The procedure included the extraction of sub-gram quantities (30 mg) of homogenized propellant with 1.5 mL of the supramolecular solvent. Several conditions affecting extraction efficiency, for example the concentrations of the major components of the supramolecular solvent (tetrahydrofuran and alkanol), alkanol type, solvent pH, and extraction time, were investigated and optimized. The main forces for the microextraction of analytes in the nanostructured supramolecular solvent include both dispersion and hydrogen bond interactions. This mixed-mode mechanism resulted in high extraction efficiencies reaching low method detection limits (0.005-0.012 mg/g) without the need for extract evaporation. Under the optimum conditions, recoveries in samples ranged between about 82.6 and 98.7%. Compared to the reference method, the proposed method is simple and rapid, delivering accurate and precise results, and can be applied for routine determination of diphenylamine and its derivatives in propellants. The precision of the method, expressed as relative standard deviation, was about 4.3-10.9%.

7.
Artículo en Inglés | MEDLINE | ID: mdl-38241106

RESUMEN

Identifying motifs within sets of protein sequences constitutes a pivotal challenge in proteomics, imparting insights into protein evolution, function prediction, and structural attributes. Motifs hold the potential to unveil crucial protein aspects like transcription factor binding sites and protein-protein interaction regions. However, prevailing techniques for identifying motif sequences in extensive protein collections often entail significant time investments. Furthermore, ensuring the accuracy of obtained results remains a persistent motif discovery challenge. This paper introduces an innovative approach-a branch and bound algorithm-for exact motif identification across diverse lengths. This algorithm exhibits superior performance in terms of reduced runtime and enhanced result accuracy, as compared to existing methods. To achieve this objective, the study constructs a comprehensive tree structure encompassing potential motif evolution pathways. Subsequently, the tree is pruned based on motif length and targeted similarity thresholds. The proposed algorithm efficiently identifies all potential motif subsequences, characterized by maximal similarity, within expansive protein sequence datasets. Experimental findings affirm the algorithm's efficacy, highlighting its superior performance in terms of runtime, motif count, and accuracy, in comparison to prevalent practical techniques.

8.
Anal Bioanal Chem ; 405(12): 4235-43, 2013 May.
Artículo en Inglés | MEDLINE | ID: mdl-23417551

RESUMEN

Novel ultrasonically enhanced supramolecular solvent microextraction (USESSM) then high-performance liquid chromatography with ultraviolet detection have been used for extraction and determination of phthalates in water and cosmetics. Coacervates consisting of decanoic acid-based nano-structured aggregates, specifically reverse micelles, have been used the first time as solvents for ultrasound-assisted emulsification microextraction (USAEME). Sonication accelerated mass transfer of the target analytes into the nano-structured solvent from the aqueous sample, thus reducing extraction time. Several conditions affecting extraction efficiency, for example the concentrations of major components of the supramolecular solvent (tetrahydrofuran and decanoic acid), sample solution pH, salt addition, and ultrasonication time, were investigated and optimized. Under the optimum conditions, preconcentration of the analytes ranged from 176 to 412-fold and the linear range was 0.5-100 µg L(-1), with correlation coefficients (R(2)) ≥ 0.9984. The detection sensitivity of the method was excellent, with limits of detection (LOD, S/N = 3) in the range 0.10-0.70 µg L(-1) and precision in the range 4.1-11.7 % (RSD, n = 5). This method was successfully used for analysis of phthalates in water and cosmetics, with good recovery of spiked phthalates (91.0-108.5 %).

9.
Adv Colloid Interface Sci ; 313: 102865, 2023 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-36868169

RESUMEN

Over the past years, metal-organic frameworks (MOF) have been directly used as electrodes or as a precursor for MOF-derived materials in energy storage and conversion systems. In the wide range of existing MOF derivatives, MOF-derived layered double hydroxides (LDHs) are determined to be promising materials due to their unique structure and features. However, MOF-derived LDHs (MDL) materials can suffer from insufficient intrinsic conductivity and agglomeration during formation. Various techniques and approaches were designed and applied to tackle these problems, such as using ternary LDHs, ion-doping, sulphurization, phosphorylation, selenization, direct growth, and conductive substrates. All the mentioned enhancement techniques aim to create the ideal electrode materials with maximum performance. In this review, we gathered and discussed the most recent progressive advances, different synthesis methodologies, unsolved challenges, applications, and electrochemical and electrocatalytic performance of MDL materials. We hope this work will be a reliable source for future progress and synthesis of these materials.

10.
Analyst ; 137(15): 3549-57, 2012 Aug 07.
Artículo en Inglés | MEDLINE | ID: mdl-22733347

RESUMEN

Hollow fiber-based liquid phase microextraction (HF-LPME) using conventional solvents is limited by their relative instability and high volatility. The use of supramolecular solvents as a liquid membrane phase could overcome these inconveniences due to their negligible vapour pressure and high viscosity. In the present study, a novel and highly flexible method was developed based on supramolecular solvents constructed of vesicles of decanoic acid, which were used for the first time as a solvent in HF-LPME. This solvent is produced from the coacervation of decanoic acid aqueous vesicles by the action of tetrabutylammonium (Bu(4)N(+)). In this work, halogenated anilines as model compounds were extracted from water samples into a supramolecular solvent impregnated in the pores and also filled inside the porous polypropylene hollow fiber membrane. The extracted anilines were separated and determined by high-performance liquid chromatography. The technique requires minimal sample preparation time and toxic organic solvent consumption, and provides a significant advantage over conventional analytical methods. The important parameters influencing the extraction efficiency were studied and optimized utilizing two different optimization methods: one variable at a time and the Box-Behnken design. Under the optimum conditions, the preconcentration factors were in the range of 74 to 203. Linearity of the method was obtained in the range of 1.0-100 µg L(-1) with the correlation coefficients of determination (R(2)) ranging from 0.9901 to 0.9986. The limits of detection for the target anilines were 0.5-1.0 µg L(-1). The relative standard deviations varied from 3.9% to 6.0%. The relative recoveries of the three halogenated anilines from water samples at a spiking level of 20.0 µg L(-1) were in the range of 90.4-107.4%.


Asunto(s)
Compuestos de Anilina/análisis , Ácidos Decanoicos/química , Microextracción en Fase Líquida/instrumentación , Microextracción en Fase Líquida/métodos , Polipropilenos/química , Cromatografía Líquida de Alta Presión , Diseño de Equipo , Sustancias Macromoleculares/química , Tamaño de la Partícula , Porosidad , Compuestos de Amonio Cuaternario/química , Solventes/química , Propiedades de Superficie
11.
J Sep Sci ; 35(18): 2319-40, 2012 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-22887709

RESUMEN

The pressure to decrease organic solvent usage in laboratories is increasing. Thus miniaturization and improvement of sample handling using alternatives is a challenge that has been discussed by several researchers. From this perspective, surfactant-based sample preparations were an educated choice. Since the introduction of cloud point extraction by Watanabe, considerable studies have been focused on the chemical properties of surfactants in the extraction methods. The unique properties of surfactants make them flexible agents for different miniaturized sample preparation techniques based on solid- or liquid-phase extraction. As a result, the use of surfactants with different roles in sample-preparation methodologies (such as surfactant as an emulsifier, surfactant rich phase as an extraction medium, ion pair-based extraction, hemimicelle/admicelle extraction, surfactant-coated magnetic nanoparticle, solid-phase microextraction with micellar desorption) is an important contribution to minimizing the problems arising from preliminary operations, which are the weakest step in analytical measurement. This paper reviews the literature dealing with the application of surfactant-based sample preparations to the separation and the preconcentration of organic and inorganic species.


Asunto(s)
Métodos Analíticos de la Preparación de la Muestra/métodos , Cromatografía con Fluido Supercrítico , Extracción Líquido-Líquido , Extracción en Fase Sólida , Tensoactivos/química , Micelas
12.
J Sep Sci ; 35(18): 2491-8, 2012 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-22753042

RESUMEN

A supramolecular solvent consisting of reverse micelles of decanoic acid, dispersed in a continuous phase of tetrahydrofuran:water, was proposed as an efficient microextraction technique for extraction of selected chlorophenoxy acid herbicides from water samples prior to high-performance liquid chromatography UV determination. The disperser solvent (1.0 mL tetrahydrofuran) containing 20 mg decanoic acid was rapidly injected into 10.0 mL of water sample. After centrifugation, the reverse micelle-rich phase (25 ± 0.5 µL) was floated at top of the home-designed centrifuge tube. The solvent was collected and 20 µL of it was injected into high-performance liquid chromatography for analysis. The results showed that the in situ solvent formation and extraction process can be completed in a few seconds. Under the optimal conditions, limits of detection of the method for 4-chloro-2-methylphenoxyacetic acid and 2,4-dichlorophenoxyacetic acid were in the range of 0.5-0.8 µg L(-1) and the repeatability of the proposed method, expressed as relative standard deviation, varied in the range of 2.5-3.2%. Linearity was found to be in the range of 1-200 µg L(-1) and the preconcentration factors were between 148 and 157. The mean percentage recoveries exceeded 92.0% for all the spiking levels in real water samples.


Asunto(s)
Ácido 2,4-Diclorofenoxiacético/análisis , Ácido 2-Metil-4-clorofenoxiacético/análisis , Microextracción en Fase Líquida , Cromatografía Líquida de Alta Presión , Ácidos Decanoicos/química , Micelas , Contaminantes Químicos del Agua/química
13.
J Sep Sci ; 34(14): 1722-9, 2011 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-21608128

RESUMEN

The process of surfactant-assisted dispersive liquid-liquid microextraction (SA-DLLME) followed by high-performance liquid chromatography-UV detection was successfully applied for the extraction and determination of selected cannabinoids (cannabidiol, Δ(9)-tetrahydrocannabinol, and cannabinol) in urine samples. The effective parameters on the extraction efficiency were studied and optimized utilizing two different optimization methods: one variable at a time (OVAT) and face center design (FCD). Under the optimum conditions (extraction solvent and its volume, toluene, 85 µL; disperser agent and its concentration, 1.0 mL of ultra-pure water containing 0.5 mmol/L tetradecyl tremethyl ammonium bromide (TTAB); sample pH, 2.0 and salt concentration, 11% w/v NaCl), the limits of detection of the method were in the range of 0.1-0.5 µg/L and the repeatability and reproducibility of the proposed method, expressed as relative deviation, varied between 4.1 and 8.5% and 6.7 and 11.6%, respectively. Linearity was found to be in the range of 1.0-200 µg/L and under the optimum conditions, the preconcentration factors (PFs) were between 190 and 292. This proposed method was successfully applied in the analysis of three male advocate urine samples and good recoveries were obtained.


Asunto(s)
Fraccionamiento Químico/métodos , Drogas Ilícitas/aislamiento & purificación , Drogas Ilícitas/orina , Tensoactivos/química , Fraccionamiento Químico/instrumentación , Cromatografía Líquida de Alta Presión , Humanos , Solventes/química
14.
J Sep Sci ; 34(5): 585-93, 2011 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-21344646

RESUMEN

Electromembrane extraction coupled with high-performance liquid chromatography (HPLC) and ultraviolet (UV) detection was developed for the determination of levamisole in some human biological fluids. Levamisole migrated from 4 mL of different acidized biological matrices, through a thin layer of 2-nitrophenyl octyl ether containing 5% tris-(2-ethylhexyl) phosphate immobilized in the pores of a porous hollow fiber, into a 20-µL acidic aqueous acceptor solution present inside the lumen of the fiber. The parameters influencing electromigration were investigated and optimized. Within 15 min of operation at 200 V, levamisole was extracted from different biological fluid samples with recoveries in the range of 59-65%, which corresponded to preconcentration factors in the range of 118-130. The calibration curves showed linearity in the range of 0.5-10, 0.2-10 and 0.1-10 µg/mL for plasma, urine and saliva, respectively. Limits of detection of 0.1, 0.07 and 0.05 µg/mL and limits of quantification of 0.5, 0.2 and 0.1 µg/mL were obtained for plasma, urine and saliva, respectively. The relative standard deviations of the analysis were found to be in the range of 5.6-9.7% (n = 3). Electromembrane extraction was successfully processed for determination of levamisole in plasma, urine and saliva samples.


Asunto(s)
Líquidos Corporales/química , Levamisol/aislamiento & purificación , Extracción en Fase Sólida/métodos , Cromatografía Líquida de Alta Presión , Humanos , Levamisol/sangre , Levamisol/orina , Saliva/química , Extracción en Fase Sólida/instrumentación , Espectrofotometría Ultravioleta , Orina/química
15.
J Sep Sci ; 34(1): 98-106, 2011 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-21171182

RESUMEN

Dynamic three-phase hollow fiber liquid-liquid-liquid microextraction (HF-LLLME) based on two immiscible organic solvents, with automated movement of organic acceptor phase to facilitate mass transfer was introduced for the first time. Polycyclic aromatic hydrocarbons were used as model compounds and extracted from water and soil samples. The extraction involved filling an 8 cm length of hollow fiber with 25 µL of organic acceptor solvent using a microsyringe, followed by impregnation of the pores in the fiber wall with n-dodecane. The fiber was then immersed in 20 mL of aqueous sample solution. During extraction, the organic acceptor phase was repeatedly moved in the lumen of the hollow fiber by movement of the syringe plunger controlled by programmable syringe pump. Following this microextraction, 2 µL of organic acceptor phase was injected into gas chromatography-flame ionization detector. This new technique provided up to 554-fold preconcentration of the analytes under the optimized conditions. Good repeatabilities (with RSDs ≤8.4%) were obtained. Detection limits were in the range of 0.2-0.5 µg/L. The utilization of the proposed method for extraction of the polycyclic aromatic hydrocarbons from different real samples (such as water and soil samples) also gave good precision and recovery.

16.
J Sep Sci ; 34(8): 957-64, 2011 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-21480523

RESUMEN

An automated dynamic two-phase hollow fiber microextraction apparatus combined with high-performance liquid chromatography was developed for extraction and determination of chlorophenoxy acid (CPA) herbicides from environmental samples. The extraction device, called TT-extractor, consists of a polypropylene hollow fiber mounted inside a stainless steel tube by means of two tee-connectors in flow system. An organic solvent, which fills the lumen and the pores of the hydrophobic fiber, is pumped through the fiber repeatedly and the sample is pumped along the outer side of the fiber. The factors affecting the dynamic hollow fiber liquid-phase microextraction (DHF-LPME) of target analytes were investigated and the optimal extraction conditions were established. To test the applicability of the designed instrument, CPAs were extracted from environmental aqueous samples. The limits of detection (LODs) as low as 0.5 µg/L, linear dynamic range in the range of 1-100 µg/L and the relative standard deviations of <7% were obtained. The developed method can provide perconcentration factors as large as 230. A hollow fiber membrane can be used at least 20 times with neither loss in the efficiency nor carryover of the analytes between runs. The system is cheap and convenient and requires minimal manual handling.

17.
Sci Rep ; 11(1): 4926, 2021 Mar 01.
Artículo en Inglés | MEDLINE | ID: mdl-33649374

RESUMEN

In this study, new nanocomposite membranes from sulfonated poly (ether ether ketone) (SPEEK) and proton-conducting Fe2TiO5 nanoparticles are prepared by the solution casting method. Sulfonated core-shell Fe2TiO5 nanoparticles are synthesized by redox polymerization. Therefore, 4-Vinyl benzene sulfonate (VBS) and 2-acrylamide-2-methyl-1-propane sulfonic acid (AMPS) are grafted on the surface of nanoparticles through radical polymerization. The different amounts of hybrid nanoparticles (PAMPS@Fe2TiO5 and PVBS@Fe2TiO5) are incorporated into the SPEEK matrix. The results show higher proton conductivity for all prepared nanocomposites than that of the SPEEK membrane. Embedding the sulfonated Fe2TiO5 nanoparticles into the SPEEK membrane improves proton conductivity by creating the new proton conducting sites. Besides, the nanocomposite membranes showed improved mechanical and dimensional stability in comparison with that of the SPEEK membrane. Also, the membranes including 2 wt% of PAMPS@Fe2TiO5 and PVBS@Fe2TiO5 nanoparticles indicate the maximum power density of 247 mW cm-2 and 226 mW cm-2 at 80 °C, respectively, which is higher than that of for the pristine membrane. Our prepared membranes have the potential for application in polymer electrolyte fuel cells.

18.
Anal Chim Acta ; 953: 1-9, 2017 02 08.
Artículo en Inglés | MEDLINE | ID: mdl-28010737

RESUMEN

A new supramolecular solvent (SUPRAS) made up of aggregates of gemini surfactant was introduced. A microextraction method, based on the SUPRAS followed with high performance liquid chromatography-ultraviolet detection, was applied for the determination of parabens in cosmetics, beverages and water samples. A SUPRAS is a nano-structured liquid made up of surfactant aggregates synthesized through a self-assembly process. In the present work, a new gemini-based SUPRAS was introduced. Methyl paraben (MP), ethyl paraben (EP), and propyl paraben (PP) were extracted on the basis of π-cation and Van der Waals interactions into the SUPRAS. The parameter affecting the extraction of target analytes (i.e., the amount of surfactant and volume of propanol as major components comprising the supramolecular solvent, sample solution pH, salt addition, ultrasonic and centrifugation time) were investigated and optimized by one-variable-at-a-time method. Under the optimum conditions, the preconcentration factors of 98, 143 and 156 were obtained for MP, EP and PP, respectively. The linearity ranged from 0.5 to 0.7-200 µg L-1 with the correlation of determination of (R2) ≥ 0.9938. The gemini-based SUPRAS followed by HPLC-UV has been found to have excellent detection sensitivity with a limit of detection (LOD, S/N = 3) of 0.5 µg L-1 for EP and PP, and 0.7 µg L-1 for MP. Good recoveries over the range of 92.0-108.3% assured the accuracy of the amount of parabens distinguished in the non-spiked samples.


Asunto(s)
Microextracción en Fase Líquida , Propanoles/química , Solventes/química , Tensoactivos/química , Bebidas/análisis , Cromatografía Líquida de Alta Presión , Cosméticos/análisis , Agua Potable/análisis , Aguas Residuales/análisis
19.
J Chromatogr A ; 1465: 38-46, 2016 Sep 23.
Artículo en Inglés | MEDLINE | ID: mdl-27592610

RESUMEN

In the current study, a graphene/polyvinylchloride nanocomposite was successfully coated on a stainless steel substrate by a simple dip coating process and used as a novel headspace solid phase microextraction (HS-SPME) fiber for the extraction of phthalate esters (PEs) from drinking water and edible vegetable oil samples. The prepared SPME fibers exhibited high extractability for PEs (due to the dominant role of π-π stacking interactions and hydrophobic effects) yielding good sensitivity and precision when followed by a gas chromatograph with a flame ionization detector (GC-FID). The optimization strategy of the extraction process was carried out using the response surface method based on a central composite design. The developed method gave a low limit of detection (0.06-0.08µgL(-1)) and good linearity (0.2-100µgL(-1)) for the determination of the PEs under the optimized conditions (extraction temperature, 70±1°C; extraction time, 35min; salt concentration, 30% w/v; stirring rate, 900rpm; desorption temperature, 230°C; and desorption time, 4min) whereas the repeatability and fiber-to-fiber reproducibility were in the range 6.1-7.8% and 8.9-10.2%, respectively. Finally, the proposed method was successfully applied to the analysis of PEs in drinking water and edible oil samples with good recoveries (87-112%) and satisfactory precisions (RSDs<8.3%), indicating the absence of matrix effects in the proposed HS-SPME method.


Asunto(s)
Técnicas de Química Analítica/métodos , Agua Potable/química , Ésteres/análisis , Nanocompuestos/química , Aceites de Plantas/química , Microextracción en Fase Sólida , Técnicas de Química Analítica/instrumentación , Cromatografía de Gases , Ionización de Llama , Grafito/química , Límite de Detección , Ácidos Ftálicos/análisis , Cloruro de Polivinilo/química , Reproducibilidad de los Resultados , Acero Inoxidable/química , Temperatura , Verduras/química
20.
Anal Chim Acta ; 884: 52-60, 2015 Jul 16.
Artículo en Inglés | MEDLINE | ID: mdl-26073809

RESUMEN

In this work, ZnO/PPy nanocomposite coating was fabricated on stainless steel and evaluated as a novel headspace solid phase microextraction (HS-SPME) fiber coating for extraction of ultra-trace amounts of environmental pollutants; namely, aliphatic hydrocarbons in water and soil samples. The ZnO/PPy nanocomposite were prepared by a two-step process including the electrochemical deposition of PPy on the surface of stainless steel in the first step, and the synthesis of ZnO nanorods by hydrothermal process in the pores of PPy matrix in the second step. Porous structure together with ZnO nanorods with the average diameter of 70 nm were observed on the surface by using scanning electron microscopy (SEM). The effective parameters on HS-SPME of hydrocarbons (i.e., extraction temperature, extraction time, desorption temperature, desorption time, salt concentration, and stirring rate) were investigated and optimized by one-variable-at-a-time method. Under optimized conditions (extraction temperature, 65±1°C; extraction time, 15 min; desorption temperature, 250°C; desorption time, 3 min; salt concentration, 10% w/v; and stirring rate, 1200 rpm), the limits of detection (LODs) were found in the range of 0.08-0.5 µg L(-1), whereas the repeatability and fiber-to-fiber reproducibility were in the range 5.4-7.6% and 8.6-10.4%, respectively. Also, the accuracies obtained for the spiked n-alkanes were in the range of 85-108%; indicating the absence of matrix effects in the proposed HS-SPME method. The results obtained in this work suggest that ZnO/PPy can be promising coating materials for future applications of SPME and related sample preparation techniques.

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