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1.
J Chem Phys ; 160(4)2024 Jan 28.
Artigo em Inglês | MEDLINE | ID: mdl-38284656

RESUMO

Lithium bis(fluorosulfonyl)imide (Li-TFSI) is an efficient p-dopant that has been used to enhance the conductivity of perovskite solar cells (PSCs). However, the performance of the corresponding devices is still not satisfactory due to the impact of Li-TFSI on the fill factor and the short-circuit current density of these PSCs. Herein, a new Mn complex [(Mn(Me-tpen)(ClO4)2-)]2+ was introduced as a p-type dopant into spiro-OMeTAD and was successfully applied as a hole transport material (HTM) for PSCs. Analytical studies used for device characterization included scanning electron microscopy, UV-Vis spectroscopy, current-voltage (IV) characteristics, incident photon to current efficiency, power conversion efficiency (PCE), and electrochemical impedance spectroscopy. The UV-Vis spectra displayed oxidation in the HTM by the addition of a dopant. Moreover, the movement of electrons from the higher orbital of the spiro-OMeTAD to the dopant stimulates the generation of the hole carriers in the HTM, enhancing its conductivity with outstanding long-term stability under mild conditions in a humid (RH ∼ 30%) environment. The incorporation of the Mn complex into the composite improved the material's properties and the stability of the fabricated devices. The Mn complex as a p-type dopant for spiro-OMeTAD exhibits a perceptible PCE of 16.39% with an enhanced conductivity of 98.13%. This finding may pave a rational way for developing efficient and stable PSCs in real environments.

2.
Electrophoresis ; 45(5-6): 400-410, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38100198

RESUMO

The coupling of capillary electrophoresis (CE) with capacitively coupled contactless conductivity detection (C4 D) has become convenient analytical method for determination of small molecules that do not possess chromogenic or fluorogenic group. The implementations of CE with C4 D in the determination of inorganic and organic ions and amino acids in biomedical field are demonstrated. Attention on background electrolyte composition, sample treatment procedures, and the utilize of multi-detection systems are described. A number of tables summarizing highly developed CE-C4 D methods and the figures of merit attained are involved. Lastly, concluding remarks and perspectives are argued.


Assuntos
Aminoácidos , Eletroforese Capilar , Eletroforese Capilar/métodos , Condutividade Elétrica , Íons/análise , Aminoácidos/análise
3.
Pharmaceutics ; 15(6)2023 May 23.
Artigo em Inglês | MEDLINE | ID: mdl-37376021

RESUMO

Raman spectroscopy is a well-established technique for the molecular characterisation of samples and does not require extensive pre-analytical processing for complex cosmetic products. As an illustration of its potential, this study investigates the quantitative performance of Raman spectroscopy coupled with partial least squares regression (PLSR) for the analysis of Alginate nanoencapsulated Piperonyl Esters (ANC-PE) incorporated into a hydrogel. A total of 96 ANC-PE samples covering a 0.4% w/w-8.3% w/w PE concentration range have been prepared and analysed. Despite the complex formulation of the sample, the spectral features of the PE can be detected and used to quantify the concentrations. Using a leave-K-out cross-validation approach, samples were divided into a training set (n = 64) and a test set, samples that were previously unknown to the PLSR model (n = 32). The root mean square error of cross-validation (RMSECV) and prediction (RMSEP) was evaluated to be 0.142% (w/w PE) and 0.148% (w/w PE), respectively. The accuracy of the prediction model was further evaluated by the percent relative error calculated from the predicted concentration compared to the true value, yielding values of 3.58% for the training set and 3.67% for the test set. The outcome of the analysis demonstrated the analytical power of Raman to obtain label-free, non-destructive quantification of the active cosmetic ingredient, presently PE, in complex formulations, holding promise for future analytical quality control (AQC) applications in the cosmetics industry with rapid and consumable-free analysis.

4.
Molecules ; 28(4)2023 Feb 07.
Artigo em Inglês | MEDLINE | ID: mdl-36838576

RESUMO

In this study, a carboxylated carbon nanotube-grafted Ag3PO4@AgIO4 (CNT-COO-/Ag3PO4@AgIO4) composite was synthesized through an in situ electrostatic deposition method. The synthesized composite was characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), diffuse reflectance spectroscopy (DRS), and energy-dispersive X-ray spectroscopy (EDS). The electron transfer ability of the synthesized composite was studied using electrochemical impedance spectroscopy (EIS). The CNT-COO-/Ag3PO4@AgIO4 composite exhibited higher activity than CNT/Ag3PO4@AgIO4, Ag3PO4@AgIO4, and bare Ag3PO4. The material characterization and the detailed study of the various parameters thataffect the photocatalytic reaction revealed that the enhanced catalytic activity is related to the good interfacial interaction between CNT-COO and Ag3PO4. The energy band structure analysis is further considered as a reason for multi-electron reaction enhancement. The results and discussion in this study provide important information for the use of the functionalized CNT-COOH in the field of photocatalysis. Moreover, providinga new way to functionalize CNT viadifferent functional groups may lead to further development in the field of photocatalysis. This work could provide a new way to use natural sunlight to facilitate the practical application of photocatalysts toenvironmental issues.


Assuntos
Nanotubos de Carbono , Luz Solar , Espectroscopia de Infravermelho com Transformada de Fourier , Microscopia Eletrônica de Varredura , Espectroscopia Dielétrica
5.
Molecules ; 28(3)2023 Jan 23.
Artigo em Inglês | MEDLINE | ID: mdl-36770803

RESUMO

The inclusion complexes of cucurbit[n]uril, CB[n] (n = 6-8), with poly aromatic hydrocarbon (PAH) Benzo(a)Pyrene (BaP), and fluoranthene (FLT) were investigated carefully in aqueous media. Fluorescence and 1H NMR spectroscopy were used to characterize and investigate the inclusion complexes that were prepared in the aqueous media. The most predominant complexes of both guests with hosts were the 1:1 guest: host complexes. Stability constants of 2322 ± 547 M-1, 7281 ± 689 M-1, 3566 ± 473 M-1 were obtained for the complexes of BaP with CB[6], CB[7], and CB[8], respectively. On the other hand, stability constants of 5900.270 ± 326 M-1, 726.87 ± 78 M-1, 3327.059 ± 153 M-1 were obtained for the complexes of FLT with CB[6], CB[7], and CB[8], respectively. Molecular dynamic (MD) simulations were used to study the mode and mechanism of the inclusion process and to monitor the stability of these complexes in aqueous media at an atomistic level. Analysis of MD trajectories has shown that both BaP and FLT form stable inclusion complexes with CB[7] and CB[8] in aqueous media throughout the simulation time, subsequently corroborating the experimental results. Nevertheless, the small size of CB[6] prohibited the encapsulation of the two PAHs inside the cavity, but stable exclusion complex was observed between them. The main driving forces for the stability of these complexes are the hydrophobic forces, van der Waals interactions, electrostatic effect, the π····π and C-H···π interaction. These results suggest that BaP and FLT can form stable complexes with CB[n] (n = 6-8) in solution.

6.
Molecules ; 27(15)2022 Jul 27.
Artigo em Inglês | MEDLINE | ID: mdl-35956767

RESUMO

Vibrational spectroscopic techniques, i.e., attenuated total reflectance infrared (ATR-IR), near infrared spectroscopy (NIRS) and Raman spectroscopy (RS), coupled with Partial Least Squares Regression (PLSR), were evaluated as cost-effective label-free and reagent-free tools to monitor water content in Levulinic Acid/L-Proline (LALP) (2:1, mol/mol) Natural Deep Eutectic Solvent (NADES). ATR-IR delivered the best outcome of Root Mean Squared Error (RMSE) of Cross-Validation (CV) = 0.27% added water concentration, RMSE of Prediction (P) = 0.27% added water concentration and mean % relative error = 2.59%. Two NIRS instruments (benchtop and handheld) were also compared during the study, respectively yielding RMSECV = 0.35% added water concentration, RMSEP = 0.56% added water concentration and mean % relative error = 5.13% added water concentration, and RMECV = 0.36% added water concentration, RMSEP = 0.68% added water concentration and mean % relative error = 6.23%. RS analysis performed in quartz cuvettes enabled accurate water quantification with RMECV = 0.43% added water concentration, RMSEP = 0.67% added water concentration and mean % relative error = 6.75%. While the vibrational spectroscopic techniques studied have shown high performance in relation to reliable determination of water concentration, their accuracy is most likely related to their sensitivity to detect the LALP compounds in the NADES. For instance, whereas ATR-IR spectra display strong features from water, Levulinic Acid and L-Proline that contribute to the PLSR predictive models constructed, NIRS and RS spectra are respectively dominated by either water or LALP compounds, representing partial molecular information and moderate accuracy compared to ATR-IR. However, while ATR-IR instruments are common in chemistry and physics laboratories, making the technique readily transferable to water quantification in NADES, Raman spectroscopy offers promising potential for future development for in situ, sample withdrawal-free analysis for high throughput and online monitoring.


Assuntos
Solventes Eutéticos Profundos , Água , Análise dos Mínimos Quadrados , Prolina , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Espectroscopia de Luz Próxima ao Infravermelho/métodos
7.
Anal Methods ; 14(20): 1973-1981, 2022 05 27.
Artigo em Inglês | MEDLINE | ID: mdl-35531873

RESUMO

Attenuated total reflectance-infrared spectroscopy (ATR-IR) coupled with partial least squares regression (PLSR) was evaluated as a rapid, label free and cost-effective tool to quantify water content in extracts obtained from spirulina wet biomass using a glucose glycerol natural deep eutectic solvent (NADES). NADESs are green, renewable and biodegradable solvents with unique properties outcompeting existing organic solvents, for instance, for plant or biomass extraction. The properties of NADESs depend critically on their water concentration, and therefore, it is essential to develop methods to monitor it, to ensure optimal extraction efficiency and experimental repeatability to achieve a better standardization of extraction protocols. First, Karl Fischer titration was performed on a set of 20 NADES extracts in order to obtain reference water concentrations. Secondly, ATR-IR spectra were collected and subjected to datamining to construct PLSR predictive models. An R2 value of 0.9996, a mean root mean square error of cross validation of 0.136% w/w and a root mean square error of prediction of 0.130% w/w highlight the feasibility and reliability to perform quantitative analysis using ATR-IR. Moreover, the mean relative error percentage achieved, ∼0.5%, confirms the high accuracy of water concentration determination in NADES extracts. This work demonstrates that powerful alternatives are available to provide more environmentally responsible analytical protocols. ATR-IR spectroscopy applied to NADES extracts does not require any sample preparation, reagents or solvents and has minimal requirements for single use consumables. The technique is consistent with current concerns to develop greener chemistry, especially in the field of extraction of natural compounds from plants which currently represents a major focus of interest in both research and industry.


Assuntos
Biomassa , Spirulina , Água , Reprodutibilidade dos Testes , Solventes/química , Análise Espectral , Água/química
8.
Molecules ; 26(18)2021 Sep 09.
Artigo em Inglês | MEDLINE | ID: mdl-34576961

RESUMO

Raman spectroscopy is a label-free, non-destructive, non-invasive analytical tool that provides insight into the molecular composition of samples with minimum or no sample preparation. The increased availability of commercial portable Raman devices presents a potentially easy and convenient analytical solution for day-to-day analysis in laboratories and production lines. However, their performance for highly specific and sensitive analysis applications has not been extensively evaluated. This study performs a direct comparison of such a commercially available, portable Raman system, with a research grade Raman microscope system for the analysis of water content of Natural Deep Eutectic Solvents (NADES). NADES are renewable, biodegradable and easily tunable "green" solvents, outcompeting existing organic solvents for applications in extraction from biomass, biocatalysis, and nanoparticle synthesis. Water content in NADES is, however, a critical parameter, affecting their properties, optimal use and extraction efficiency. In the present study, portable Raman spectroscopy coupled with Partial Least Squares Regression (PLSR) is investigated for rapid determination of water content in NADES samples in situ, i.e., directly in glassware. Three NADES systems, namely Betaine Glycerol (BG), Choline Chloride Glycerol (CCG) and Glucose Glycerol (GG), containing a range of water concentrations between 0% (w/w) and 28.5% (w/w), were studied. The results are directly compared with previously published studies of the same systems, using a research grade Raman microscope. PLSR results demonstrate the reliability of the analysis, surrendering R2 values above 0.99. Root Mean Square Errors Prediction (RMSEP) of 0.6805%, 0.9859% and 1.2907% w/w were found for respectively unknown CCG, BG and GG samples using the portable device compared to 0.4715%, 0.3437% and 0.7409% w/w previously obtained by analysis in quartz cuvettes with a Raman confocal microscope. Despite the relatively higher values of RMSEP observed, the comparison of the percentage of relative errors in the predicted concentration highlights that, overall, the portable device delivers accuracy below 5%. Ultimately, it has been demonstrated that portable Raman spectroscopy enables accurate quantification of water in NADES directly through glass vials without the requirement for sample withdrawal. Such compact instruments provide solvent and consumable free analysis for rapid analysis directly in laboratories and for non-expert users. Portable Raman is a promising approach for high throughput monitoring of water content in NADES that can support the development of new analytical protocols in the field of green chemistry in research and development laboratories but also in the industry as a routine quality control tool.

9.
Anal Bioanal Chem ; 413(19): 4785-4799, 2021 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-34061244

RESUMO

Natural deep eutectic solvents (NADES) are ionic solutions, of great interest for extraction from biomass, biocatalysis, and nanoparticle synthesis. They are easily synthesised and eco-friendly, have low volatility and high dissolution power, and are biodegradable. However, water content in NADES is a critical parameter, affecting their optimal use and extraction efficiency. Vibrational spectroscopic techniques are rapid, label-free, non-destructive, non-invasive, and cost-effective analytical tools that can probe the molecular composition of samples. A direct comparison between a previous study using attenuated total reflectance infrared (ATR-IR) spectroscopy for water quantification in NADES and the same investigation performed with Raman spectroscopy is presently reported. Three NADES systems, namely betaine-glycerol (BG), choline chloride-glycerol (CCG), and glucose-glycerol (GG), containing a range of water concentrations between 0% (w/w) and 40% (w/w), have been analysed with Raman spectroscopy coupled to partial least squares regression multivariate analysis. The values of root mean square error of cross-validation (RMSECV) obtained from analysis performed on the pre-processed spectra over the full spectral range (150-3750 cm-1) are respectively 0.2966% (w/w), 0.4703% (w/w), and 0.2351% (w/w) for BG, GG, and CCG. While the direct comparison to previous ATR-IR results shows essentially similar outcomes for BG, the RMSECV is 33.14% lower and 65.84% lower for CG and CCG. Furthermore, mean relative errors obtained with Raman spectroscopy, and calculated from a set of samples used as independent samples, were 1.452% (w/w), 1.175% (w/w), and 1.188% (w/w). Ultimately, Raman spectroscopy delivered performances for quantification of water in NADES with similar accuracy to ATR-IR. The present demonstration clearly highlights the potential of Raman spectroscopy to support the development of new analytical protocols in the field of green chemistry.

10.
Artigo em Inglês | MEDLINE | ID: mdl-29328953

RESUMO

The inclusion complexes of imazapyr (IMA) with cucurbit[n]uril, CB[n] (n=6-8), have been investigated. Fluorescence spectroscopy, MALDI-TOF, and 1HNMR were used to investigate and characterize the inclusion complexation of IMA and CB[n] in solutions. Whereas the solid state complexes have been characterized by Fourier transform infrared spectroscopy (FTIR), and powder X-ray diffraction (PXRD). IMA was found to form 1:1 complexes with CB[n] with association constants ranging from 5.80×102-2.65×103. The guest molecule IMA was found to encapsulate into the larger cavities of CB[7] and CB[8], whereas with CB[6] the molecule remains outside the cavity. Molecular dynamic (MD) simulations were used to follow the inclusion process at an atomistic level to study the mechanism and stability of inclusion. The results obtained showed that inclusion complexes of IMA with both CB[7] and CB[8] are highly stable in aqueous media, but the CB[6] smaller cavity size prohibited the formation of an inclusion complex with IMA. The results clearly show that in addition to hydrophobic effects the presence of hydrogen bonding has added greatly to the stability of these complexes.

11.
Biomed Chromatogr ; 31(9)2017 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-28178368

RESUMO

Capacitively coupled contactless conductivity detection (C4 D) has appeared as a powerful technique for the detection of compounds lacking chromogenic or fluorogenic group. Since our last review (Biomedical Chromatography 2014; 28: 1502-1506) several new capillary electrophoresis (CE)-C4 D methods have been reported. This review provides an update of the most recent utilization of CE-C4 D in the field of pharmaceutical, biomedical and food analysis covering the period from February 2014 to October 2016. The use of CE with C4 D in the pharmaceutical field has been shown in many papers. Examples illustrate the applicability of CE-C4 D in the fields of pharmaceutical, biomedical and food analysis. Finally, general conclusions and perspectives are provided.


Assuntos
Eletroforese Capilar/métodos , Biotecnologia , Condutividade Elétrica , Análise de Alimentos , Preparações Farmacêuticas/análise
12.
Artigo em Inglês | MEDLINE | ID: mdl-26143328

RESUMO

The solid inclusion complex of gemifloxacin (GFX) and hydroxyl propyl ß-cyclodextrin (HPß-CD) was prepared and examined by UV-visible, FTIR, NMR, electrospray ionization mass spectrometry (ESI-MS) and fluorescence spectroscopy. The formation of inclusion complex has been confirmed on the basis of changes of spectroscopic properties. Further the interaction between GFX and HPß-CD was studied using molecular modeling approaches. The results showed that HPßCD reacted with GFX to form a 1:1 host-guest inclusion complex. Based on the enhancement of the fluorescence intensity of GFX produced through complex formation, a simple, accurate, rapid and highly sensitive spectrofluorometric method for the determination of GFX in pharmaceutical formulation was developed. The linear relationships between the intensity and GFX concentration was obtained in the concentration range of 20-140 ng/mL with good correlation coefficients (0.9997). The limit of detection (LOD) was found to be 4 ng/mL. The proposed method was successfully applied to the analysis of GFX in pharmaceutical preparation.


Assuntos
Fluoroquinolonas/química , Fluoroquinolonas/metabolismo , Modelos Moleculares , Naftiridinas/química , Naftiridinas/metabolismo , beta-Ciclodextrinas/química , beta-Ciclodextrinas/metabolismo , 2-Hidroxipropil-beta-Ciclodextrina , Excipientes/química , Excipientes/metabolismo , Fluoroquinolonas/análise , Gemifloxacina , Concentração de Íons de Hidrogênio , Limite de Detecção , Espectroscopia de Ressonância Magnética , Simulação de Acoplamento Molecular , Estrutura Molecular , Naftiridinas/análise , Espectrometria de Fluorescência , Espectrofotometria Ultravioleta , Espectroscopia de Infravermelho com Transformada de Fourier , Termodinâmica , Inibidores da Topoisomerase II/química , Inibidores da Topoisomerase II/metabolismo
13.
Crit Rev Anal Chem ; 45(3): 226-40, 2015.
Artigo em Inglês | MEDLINE | ID: mdl-25849823

RESUMO

Gas chromatography (GC) and high-performance liquid chromatography (HPLC) coupled to different detectors, and in combination with different sample extraction methods, are most widely used for analysis of triazine herbicides in different environmental samples. Nowadays, many variations and modifications of extraction and sample preparation methods such as solid-phase microextraction (SPME), hollow fiber-liquid phase microextraction (HF-LPME), stir bar sportive extraction (SBSE), headspace-solid phase microextraction (HS-SPME), dispersive liquid-liquid microextraction (DLLME), dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO), ultrasound-assisted emulsification microextraction (USAEME), and others have been introduced and developed to obtain sensitive and accurate methods for the analysis of these hazardous compounds. In this review, several analytical properties such as linearity, sensitivity, repeatability, and accuracy for each developed method are discussed, and excellent results were obtained for the most of developed methods combined with GC and HPLC techniques for the analysis of triazine herbicides. This review gives an overview of recent publications of the application of GC and HPLC for analysis of triazine herbicides residues in various samples.


Assuntos
Cromatografia/métodos , Herbicidas/análise , Triazinas/análise
14.
Luminescence ; 30(8): 1250-6, 2015 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-25808072

RESUMO

The supramolecular interaction of protonated mesalazine (MSZ) and 18-crown-6 ether (18C6) has been examined by Ultraviolet-visible, FT-IR and fluorescence spectroscopy. The formation of the inclusion complex has been confirmed based on the changes of the spectral properties. The MSZ-18C6 host-guest complex formed in (1:1) stoichiometry and the inclusion constant (K = 1.411 × 10(2) L mol(-1)) was ascertained by the typical double reciprocal plots. Furthermore, the thermodynamic parameters (ΔG°, ΔH° and ΔS°) of (MSZ-18C6) were obtained. Based on the remarkable enhancement of the fluorescence intensity of MSZ produced through complex formation, a simple, accurate, rapid and highly sensitive spectrofluorometric method for the determination of MSZ in aqueous solution in the presence of 18C6 was developed. The measurement of relative fluorescence intensity was carried with excitation at 298 nm, emission 410 nm. All variables affecting the reactions were studied and optimized. Beer's law was obeyed in the concentration range of 0.1-0.9 µg/mL. The absorbance was found to increase linearly with increasing concentration of MSZ. The molar absorptivity, Sandell sensitivity, limit of detection (LOD) and limit of quantification (LOQ) were calculated. The validity of the described method was assessed, and the method was successfully applied to the determination of MSZ in its pharmaceutical formulation. In addition, a solid inclusion complex was synthesized by the coprecipitation method.


Assuntos
Éteres de Coroa/química , Mesalamina/química , Preparações Farmacêuticas/química , Cinética , Espectrometria de Fluorescência , Espectrofotometria Ultravioleta , Espectroscopia de Infravermelho com Transformada de Fourier
15.
Artigo em Inglês | MEDLINE | ID: mdl-25277628

RESUMO

The supramolecular interaction of Moxifloxacin (Moxi) and ß-cyclodextrin (ß-CD) has been examined by UV-VIS, FTIR, H(1)NMR, SEM and fluorescence spectroscopy. The formation of inclusion complex has been confirmed on the base of changes of spectroscopy properties. The results showed that ß-CD reacted with Moxi to form an inclusion complex. The Moxi and ß-CD complex formed a host-guest complex in 1:1 stoichiometry and inclusion constant (K=3.95×10(2) L mol(-1)) was ascertained by the typical double reciprocal plots. Furthermore, the thermodynamic parameters (ΔH°, ΔS° and ΔG°) associated with the inclusion process were also determined. Based on the significant enhancement of the fluorescence intensity of Moxi produced through complex formation, a simple, accurate, rapid and highly sensitive spectrofluorometric method for the determination of Moxi in pharmaceutical formulation was developed. The measurement of relative fluorescence intensity was carried out at 464 nm with excitation at 289 nm. The factors affecting the inclusion complex formation were studied and optimized. Under the optimum reaction conditions, linear relationships with good correlation coefficients (0.99973) were in the concentration range of 10-60 ng/mL for spectrofluorimetry. The limit of detection (LOD) was found to be 1.6 ng/mL. The proposed method was successfully applied to the analysis of Moxi in pharmaceutical preparation.


Assuntos
Fluoroquinolonas/química , beta-Ciclodextrinas/química , Soluções Tampão , Química Farmacêutica , Concentração de Íons de Hidrogênio , Cinética , Limite de Detecção , Espectroscopia de Ressonância Magnética , Microscopia Eletrônica de Varredura , Conformação Molecular , Estrutura Molecular , Moxifloxacina , Preparações Farmacêuticas , Espectrometria de Fluorescência , Espectrofotometria Ultravioleta , Espectroscopia de Infravermelho com Transformada de Fourier , Temperatura , Termodinâmica
16.
Luminescence ; 30(4): 444-50, 2015 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-25204628

RESUMO

The supramolecular interaction of mesalazine (MSZ) and ß-cyclodextrin (ß-CD) has been examined by ultraviolet-visible (UV-vis) light, infra-red (IR) light and fluorescence spectroscopy. The formation of an inclusion complex has been confirmed based on the changes of the spectral properties. MSZ-ß-CD host-guest complex was formed in (1:1) stoichiometry and the inclusion constant (K = 1.359 × 10(2) L mol(-1) ) was ascertained by typical double reciprocal plots. Furthermore, the thermodynamic parameters (ΔG°, ΔH° and ΔS°) of (MSZ-ß-CD) were obtained. Based on the remarkable enhancement of the fluorescence intensity of MSZ produced through complex formation, a simple, accurate, rapid and highly sensitive spectrofluorometric method for the determination of MSZ in aqueous solution in the presence of ß-CD was developed. The measurement of relative fluorescence intensity was carried with excitation at 330 nm and emission 493 nm. All variables affecting the reactions were studied and optimized. Beer's law was obeyed in the concentration range 0.1-0.45 µg/mL. Absorbance was found to increase linearly with increasing concentration of MSZ, which is corroborated by the calculated correlation coefficient values of 0.99989. The molar absorptivity, Sandell's sensitivity, detection and quantification limits were calculated. The validity of the described methods was assessed, and the method was successfully applied to the determination of MSZ in its pharmaceutical formulation. In addition, a solid inclusion complex was synthesized by co-precipitation method.


Assuntos
Mesalamina/análise , Mesalamina/química , Espectrometria de Fluorescência/métodos , beta-Ciclodextrinas/química , Concentração de Íons de Hidrogênio , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Espectrofotometria Infravermelho , Espectrofotometria Ultravioleta , Temperatura , Termodinâmica
17.
Biomed Chromatogr ; 29(6): 835-42, 2015 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-25515940

RESUMO

Triazines are widely used in agriculture around the world as selective pre- and post-emergence herbicides for the control of broad leaf and grassy weeds. With high toxicity and persistence, triazines can contaminate the environment and crops, so the development of rapid and sensitive methods for the determination of different triazines is necessary. Capillary electrophoresis comprises a group of techniques used to separate chemical mixtures. Analytical separation is based on different electrophoretic mobilities. This review focuses on the analysis of triazine herbicides with different modes of capillary electrophoresis, including capillary zone electrophoresis, micellar electrokinetic capillary electrophoresis, capillary electrochromatography and nonaqueous capillary electrophoresis. Determinations of triazines in various matrices such as surface water, groundwater, vegetables, soil and grains are emphasized.


Assuntos
Cromatografia Capilar Eletrocinética Micelar/métodos , Eletroforese Capilar/métodos , Herbicidas , Resíduos de Praguicidas , Poluentes do Solo , Triazinas , Poluentes Químicos da Água , Herbicidas/análise , Herbicidas/química , Herbicidas/isolamento & purificação , Limite de Detecção , Resíduos de Praguicidas/análise , Resíduos de Praguicidas/química , Resíduos de Praguicidas/isolamento & purificação , Reprodutibilidade dos Testes , Poluentes do Solo/análise , Poluentes do Solo/química , Poluentes do Solo/isolamento & purificação , Triazinas/análise , Triazinas/química , Triazinas/isolamento & purificação , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/química , Poluentes Químicos da Água/isolamento & purificação
18.
Crit Rev Anal Chem ; 44(2): 107-41, 2014.
Artigo em Inglês | MEDLINE | ID: mdl-25391433

RESUMO

Acrylamide (AA) is a compound classified as carcinogenic to humans by the International Agency for Research on Cancer. It was first discovered to be present in certain heated processed food by the Swedish National Food Administration (SNFA) and University of Stockholm in early 2002. The major pathway for AA formation in food is the Maillard reaction between reducing sugar and the amino acid asparagine at high temperature. Since the discovery of AA's presence in food, many analytical methods have been developed for determination of AA contents in different food matrices. Also, several studies have been conducted to develop extraction procedures for AA from difficult food matrices. AA is a small, highly polar molecule, which makes its extraction and analysis challenging. Many articles and reviews have been published dealing with AA in food. The aim of the review is to discuss AA formation in food, the factors affecting AA formation and removal, AA exposure assessment, AA extraction and cleanup from food samples, and analytical methods used in AA determination, such as high-performance liquid chromatography (HPLC) and gas chromatography (GC). Special attention is given to sample extraction and cleanup procedures and analytical techniques used for AA determination.


Assuntos
Acrilamida/análise , Carcinógenos/análise , Cromatografia Gasosa/métodos , Cromatografia Líquida/métodos , Análise de Alimentos/métodos , Contaminação de Alimentos/análise , Acrilamida/isolamento & purificação , Carcinógenos/isolamento & purificação , Humanos
19.
Artigo em Inglês | MEDLINE | ID: mdl-24914599

RESUMO

This survey examined 60 samples of sorghum and 30 samples of sorghum products from three states (Khartoum, Kordofan and Gadarif) of Sudan for aflatoxin B1, B2, G1 and G2 (AFB1, AFB2, AFG1, AFG2), ochratoxin A and B (OTA, OTB) and zearalenone (ZEN), using high performance liquid chromatography with fluorescence detection. The limits of detection and limits of quantification were in the range 0.01-0.6 µg kg(-1) and 0.03-2.0 µg kg(-1), respectively. The frequency of contaminated samples with AFB1 from Khartoum, Gadarif and Kordofan state was 38.1%, 22.2% and 23.8%, respectively. Only two samples of sorghum from Khartoum state were contaminated with OTA (3.3%). Concentrations of OTA and OTB were low and may not cause problems. No sample of sorghum or sorghum products was contaminated with ZEN. Some sorghum samples contained AFB1 concentrations above the European Union regulatory limits. The highest contaminated samples were found in Khartoum state.


Assuntos
Aflatoxinas/análise , Dieta , Grão Comestível , Contaminação de Alimentos/análise , Ocratoxinas/análise , Sorghum , Zearalenona/análise , Aflatoxina B1/análise , Cromatografia Líquida de Alta Pressão , Grão Comestível/microbiologia , Humanos , Limite de Detecção , Sementes , Sorghum/microbiologia , Sudão
20.
Biomed Chromatogr ; 28(11): 1502-6, 2014 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-24816678

RESUMO

Capacitively coupled contactless conductivity detection (C4D) has emerged as a powerful technique for the detection of compounds lacking any distinct chromophores or fluorophores. This review provides an update of the most recent application in CE-C4D for pharmaceutical, biomedical and food covering the period from January 2012 to January 2014. The present review is an update of two previous review papers covering the years 2000-2010 (Biomedical Chromatography 2010; 24: 1038-1044 and Biomedical Chromatography 2012; 26: 990-1000). Representative examples illustrate the applicability of CE-C4D in the fields of pharmaceutical, biomedical and food. Finally, general conclusions and perspectives are provided.


Assuntos
Condutividade Elétrica , Eletroforese Capilar
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