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1.
Front Neurol ; 13: 946593, 2022.
Artigo em Inglês | MEDLINE | ID: mdl-35968302

RESUMO

Background and purpose: This study sought to improve methods to identify biomarkers in the neuroendocrine system related to stroke progression to improve the accuracy of traditional tools for evaluating stroke prognosis. Methods: Seventy-four stroke patients and 237 healthy controls were prospectively included. We measured urinary epinephrine (E), noradrenaline (NE), dopamine (DA) and cortisol (F) on days 1, 3, and 5 after stroke onset and plasma F, adrenocorticotropic hormone (ACTH), thyrotropin (TSH), prolactin (PRL), follicle-stimulating hormone (FSH), luteinizing hormone (LH) and growth hormone (GH). The correlation between these hormone levels and 90-day prognosis was analyzed, their value in assessing prognosis was compared with lesion volume and National Institutes of Health Stroke Scale (NIHSS) scores using receiver operating characteristic (ROC) curves, and their correlation with conventional clinical variables was assessed. Results: Levels of F, 24-h urinary free cortisol(UFC), E, NE, DA, and GH on days 1, 3, and 5 were significantly higher in stroke patients than in controls (P < 0.01), while ACTH and TSH decreased, gradually approaching normal within 5 days of onset. Levels of E, NE, F, and 24-h UFC were proportional to severity, and all gradually decreased within 5 days of onset in patients with a good prognosis and gradually increased or remained high in those with a poor prognosis. After adjustment for age, sex, NIHSS, or Glasgow Coma Scale (GCS) score, F > 13.6 µg/dL, ACTH > 22.02 pg/mL and NE > 123.5 µg/ 24 h were identified as risk factors for a poor prognosis 90 days after stroke (P < 0.05). The combination of F, ACTH, NE, white blood cell count (WBC), glucose (Glu), and hemoglobin (Hb) was significantly more accurate than lesion volume (AUC: 0.931 vs. 0.694 P = 0.019) and NIHSS score (AUC: 0.931 vs. 0.746 P = 0.034) in predicting poor prognosis of stroke 1 day after onset. Hormones and traditional clinical variables were correlated to varying degrees, with NE correlating most strongly with 24-h UFC (r = 0.54) and moderately positively with lesion volume (r = 0.40) and NIHSS score (r = 0.45). Conclusions: Stroke causes significant time-phased dynamic changes in the hypothalamic-pituitary-adrenal axis and sympathetic nervous system, and plasma F, ACTH, and urinary NE levels can be used to assess stroke severity and prognosis. Chinese clinical trial registry: Registration Number: ChiCTR1900024992. Registration Date: 2019/8/6.

2.
Guang Pu Xue Yu Guang Pu Fen Xi ; 34(2): 450-4, 2014 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-24822419

RESUMO

The fluorescence properties of dissolved organic matter (DOM) in Fu River in Baoding were investigated by three-dimensional fluorescence spectrometry. The type, distribution and origin of the DOM were estimated on basis of the position, number and intensity of fluorescence peaks in the spectra. Two types of fluorescence peaks were detected from Fu River. There are protein-like fluorescence peaks A with Ex/Em = 225-230/340 nm and soluble microbial metabolites peaks B with Ex/Em=275/340-350 nm. The protein-like fluorescence peaks and soluble microbial metabolites peaks were founded in different times and stations in Fu River. Certain correlation was observed between the fluorescence intensity of DOM and the water quality parameters of Fu River. Good correlation of different fluorescence peaks showed the same of source. The fluorescence intensity of the two types had a significant positive relationship with COD, TN, TP and NH3-N concentration, this phenomenon indicating that the fluorescence peaks can speculate the level of pollution of Fu River. These results provided a reference for the pollution control in Fu River.


Assuntos
Compostos Orgânicos/análise , Rios/química , Proteínas/análise , Espectrometria de Fluorescência , Poluição da Água/análise
3.
J Sep Sci ; 36(16): 2656-63, 2013 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-23780651

RESUMO

A magnetic dispersion extraction method was developed based on a molecularly imprinted magnetic microsphere (MIMM) for the selective clean-up and enrichment of tetracycline antibiotics from milk samples. The MIMMs were prepared by inverse-emulsion suspension polymerization, using doxycycline, trimethylolpropane trimethacrylate, acrylamide, methacrylic acid, and surface-modified Fe3 O4 as a template molecule, crosslinker, functional monomer, and magnetic component, respectively. Synthesis and extraction conditions were optimized for obtaining excellent affinity and high selectivity. The magnetism, covering amount, and selectivity of the magnetic microspheres were characterized by a vibrating sample magnetometer, thermogravimetric analysis, and a competitive recognition experiment. The MIMMs were applied to separate tetracycline antibiotics from milk samples by magnetic dispersion extraction, and an enrichment factor of 9.28 and a good sample clean-up were obtained. The average recoveries of four tetracycline antibiotics were obtained in the range of 74.5-93.8% with a precision of 1.2-5.2%. The LODs and LOQs of the proposed method were in the range of 7.4-19.4 and 24.7-64.7 µg/kg, respectively. The results indicated that magnetic dispersion extraction using MIMMs is a powerful tool for food-sample pretreatment with high selectivity and a simplified procedure.


Assuntos
Antibacterianos/isolamento & purificação , Doxiciclina/química , Contaminação de Alimentos/análise , Leite/química , Polímeros/química , Extração em Fase Sólida/métodos , Tetraciclinas/isolamento & purificação , Adsorção , Animais , Bovinos , Emulsões/química , Magnetismo , Microesferas , Impressão Molecular , Polimerização , Polímeros/síntese química , Extração em Fase Sólida/instrumentação
4.
Guang Pu Xue Yu Guang Pu Fen Xi ; 33(1): 102-5, 2013 Jan.
Artigo em Chinês | MEDLINE | ID: mdl-23586235

RESUMO

A rapid method was developed for discrimination of the geographical origins of rice with pattern recognition technique by near infrared spectrocopy (NIRS). A total of 119 geography signs product Xiangshui rice samples and 90 rice (Non-Xiangshui rice) samples produced from other places were analyzed by NIRS. After first derivative and smooth processing, principal component analysis (PCA) was used to reduce the dimensionality of the spectral data. Through the loading graph of the first three principal components, characteristic wave band (7 700-6 700, 5 700-4 300 cm(-1)) with max-relativity was determined. In whole wave, using agglomerative hierarchical cluster analysis and Fisher's linear discriminant, the discrimination of Xiangshui rice and Non-Xiangshui rice was all 100%. The correct rate of specific geographical origins of Non-Xiangshui rice was 91.9% by cluster analysis and 96.7% by discriminant analysis. For analysis in the characteristic wave bands, the correct rate of discriminant by cluster analysis was higher than the analysis result through the range of the whole band. Therefore, characteristic wave band has strong representativeness. The results indicate that it is feasible to discriminate the geographical origins of rice with pattern recognition technique by NIRS, and selecting characteristic wave band is one of the validated methods to improve the precision of the discrimination mode.


Assuntos
Oryza/química , Reconhecimento Automatizado de Padrão/métodos , Espectroscopia de Luz Próxima ao Infravermelho/métodos , China , Análise por Conglomerados , Análise Discriminante , Geografia , Oryza/classificação , Análise de Componente Principal
5.
Guang Pu Xue Yu Guang Pu Fen Xi ; 32(8): 2157-61, 2012 Aug.
Artigo em Chinês | MEDLINE | ID: mdl-23156772

RESUMO

The exponentially modified Gaussian (EMG) model-based genetic algorithm was used as a fitness function for fitting fluorescence spectrogram. The method was effective for solving the interference of fluorescent substance in the course of the multi-component quantitative analysis. As an example, the interference of endogenous fluorophores in different urines with the fluorescence of gatifloxacin (GFLX) was examined. A good eradicating efficacy was achieved by using the fitting fluorescence spectrogram. Under the optimized experimental conditions, the good linear relationship between the fluorescence intensity and GFLX concentration was obtained in the range of 0.06-3.5 microg x mL(-1) with a correlation coefficient of 0.9994. The detection limit and recovery were 0.02 microg x mL(-1) and 99.2%-109.4%, respectively, with the relative standard deviation from 1.3% to 2.7%. The proposed fitting fluorescence spectrometric method was rapid, simple and highly sensitive for the determination of GFLX in different human urine without preseparation. The recovery, selectivity, linearity, precision and accuracy of the method are convenient for routine assays and pharmacokinetic studies.

6.
Water Sci Technol ; 66(12): 2695-701, 2012.
Artigo em Inglês | MEDLINE | ID: mdl-23109588

RESUMO

A central composite factorial design methodology was employed to optimize the degradation of naproxen (NPX) by the combination of Fenton reagent and ultrasound (US) irradiation. In this study, the variables considered for the process optimization were the hydrogen peroxide, ferrous ion and NPX initial concentrations, while ultrasonic power amplitude was adjusted at 90% and initial pH was 3. An appropriate quadratic model was developed in order to plot the response surface and contour curves. Optimum dosage of Fenton reagent for NPX removal was found to be hydrogen peroxide concentration = 9.98 mmol L⁻¹, ferrous ion concentration = 4.83 mg L⁻¹ while NPX concentration was equal to 20 mg L⁻¹. A degradation efficiency of 100% was achieved within 10 min under US.


Assuntos
Peróxido de Hidrogênio/química , Ferro/química , Naproxeno/química , Ultrassom , Purificação da Água/métodos , Análise de Variância , Concentração de Íons de Hidrogênio , Espectrometria de Fluorescência
7.
Guang Pu Xue Yu Guang Pu Fen Xi ; 32(3): 809-12, 2012 Mar.
Artigo em Chinês | MEDLINE | ID: mdl-22582658

RESUMO

A method for determining 9 heavy metal elements in soil and sediment was developed by using microwave digestion-ICP-MS. The mixture of HNO3-H2O2-HF was found to give the best digestion results for soil and sediment of samples. Under the optimized conditions, the samples were analyzed by ICP-MS with the triple internal standard elements Ge, In and Bi. The results showed that all their correlation coefficients were over 0.999. The national standard soil referenee material (ESS-1 GSBZ50011-88) was analyzed by the described method and the results were accorded with the reference values. The measurement precision range was from 0.48% to 5.73% in terms of relative standard deviation. The recoveries and the limits of detection were in the ranges of 98.0% to 100.7% and 0.011 to 0.328 microg x L(-1) respectively, and 11 sediment samples were determined by the proposed method. It was indicated that the method was reliable for determining heavy metal elements in soil and sediment samples.

8.
J Chromatogr A ; 1227: 48-53, 2012 Mar 02.
Artigo em Inglês | MEDLINE | ID: mdl-22281508

RESUMO

A novel molecularly imprinted organic-inorganic hybrid composite material (MIP-HCM) was developed based on molecular imprinting technique in combination with hybrid composite synthesis and sol-gel technology for selective solid-phase extraction (SPE) of tetracyclines residues in milk. The MIP-HCM was prepared using oxytetracycline as the template, methacrylic acid as organic functional monomer, tetraethoxysilane as inorganic precursor and methacryloxypropyltrimethoxysilane as the coupling agent. Synthesis conditions are optimized by changing some factors to obtain sorbent with the controllable adsorption capacity, selectivity, hardness and toughness. Binding study demonstrated that the imprinted hybrid composites showed excellent affinity and high selectivity to oxytetracycline. An enrichment factor of 18.8 along with a good sample clean-up was obtained under the optimized SPE conditions. The average recoveries of three tetracyclines antibiotics spiked milk at 0.1, 0.2 and 0.5 mg kg⁻¹ were in the range of 80.9-104.3% with the precision of 1.5-5.0%. The limits of detection and quantitation of the proposed method were in a range of 4.8-12.7 µg kg⁻¹ and 16.0-42.3 µg kg⁻¹, respectively.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Drogas/análise , Leite/química , Impressão Molecular/métodos , Oxitetraciclina/análise , Extração em Fase Sólida/métodos , Animais , Limite de Detecção , Modelos Lineares , Ácidos Polimetacrílicos/química , Reprodutibilidade dos Testes
9.
Talanta ; 89: 270-5, 2012 Jan 30.
Artigo em Inglês | MEDLINE | ID: mdl-22284491

RESUMO

A high-density imprinted polymeric membrane was immobilized on a porous silica-gel support by polymerization of methacrylic acid with vinyl-silanized silica gel for the selective solid-phase extraction (SPE) of norfloxacin (NOR) in fish samples. The imprinted membranes showed high adsorption capacity (423.2 µmol g(-1)), significant selectivity (k=14.64, k'=9.61) and good site accessibility (2h) for NOR. The conditions of SPE were investigated, and water (pH=6), methanol:water (1:1, v/v) and methanol-acetic acid-trifluoroacetic acid (90:9:1, v/v) were selected as the sample solvent, the washing solution and the eluting solution, respectively. Under the optimal SPE condition, three fluoroquinolone residues in fish were separated and detected by an off-line MIP-SPE-HPLC with better clean up and enrichment. The recoveries of norfloxacin, ofloxacin and ciprofloxacin were 89.3-94.8%, 69.3-102.8% and 85-90.5%, respectively, with relative standard deviations lower than 6.5%. The limits of detection (LOD) of the proposed method (S/N=3) were in a range of 2.65-3.65 µg kg(-1), and the limits of quantification (LOQ, S/N=10) were in a range of 8.82-12.16 µg kg(-1).


Assuntos
Ciprofloxacina/análise , Peixes/metabolismo , Norfloxacino/análise , Ofloxacino/análise , Adsorção , Animais , Cromatografia Líquida de Alta Pressão , Limite de Detecção , Membranas Artificiais , Metacrilatos/química , Impressão Molecular , Polímeros/química , Porosidade , Silanos/química , Sílica Gel , Extração em Fase Sólida , Solventes , Compostos de Vinila/química
10.
Guang Pu Xue Yu Guang Pu Fen Xi ; 30(2): 391-4, 2010 Feb.
Artigo em Chinês | MEDLINE | ID: mdl-20384131

RESUMO

It is the first time ionic liquid was applied to gas solvent sublation, which established a new method for separation/enrichment of tetracyclines (TCs) antibiotic based on ionic liquid gas solvent sublation. The optimizing experimental conditions were as follows: the mixture of ionic liquid 1-hexyl-3-methylimidazo lium hexafluorophosphats and ethyl acetate ([Hmim] PF6-EA, phi = 1/0.9) can be used as flotation solvent, Fe(III) ion was as trapping agent, pH of test solution was 7.6, the gas flow rate was 40 mL x min(-1), and the flotation time was 50 min. The complexes of TCs- Fe (III) were pre-concentrated in the [Hmim] PF6-EA layer and this was used to determine analytes by fluorescence method directly. The linear regression equation was F = 246.5c+4.32 (c: microg x 10 mL(-1)), and correlation coefficient was 0.999 1. Recoveries between 94.2% and 100.4% were achieved from surface water and sediment samples in ponder by using this method and the relative standard deviation of 5 microg x mL(-1) TCs for 5 parallel determinations was less than 3.2%. FTIR spectroscopy demonstrated that no chemical (bonding) interactions occurred between the ionic liquid and the complexes functional groups, and the ionic liquid was only solvent. The experimental result indicated that utilizing ionic liquid to float TCs in environmental sample is feasible.


Assuntos
Resíduos de Drogas/química , Espectrometria de Fluorescência , Tetraciclinas/química , Poluentes Químicos da Água/química , Antibacterianos/química , Monitoramento Ambiental , Compostos Férricos , Líquidos Iônicos , Íons , Solventes
11.
Environ Toxicol Pharmacol ; 29(3): 297-301, 2010 May.
Artigo em Inglês | MEDLINE | ID: mdl-21787616

RESUMO

Decabrominated diphenyl ether (BDE-209) is widely used as brominated flame retardants (BFRs). In order to investigate its direct neurotoxic effects on mice and its self repair, mice were repeatedly exposured to BDE-209. Different concentrations of BDE-209 (0, 0.1, 40, 80 and 160mg/kgbw/d) were administered daily to CD-1 Swiss mice by gavage for 15, 30 and 60 days. Body and brain weights were recorded after the exposure. And the self repair was studied. Levels of acetylcholinesterase (TchE), superoxide dismutase (SOD) and malonic dialdehyde (MDA) in brain were analyzed. Experimental results suggested that the nervous system was permanently damaged by BDE-209 through the cholinergic system enzyme.

12.
J Biomater Sci Polym Ed ; 20(12): 1675-86, 2009.
Artigo em Inglês | MEDLINE | ID: mdl-19723435

RESUMO

Poly(PEGMA-MAA)-coated superparamagnetic nanoparticles were synthesized by in situ photochemical polymerization in magnetite aqueous suspension under UV irradiation. The magnetic poly(PEGMA-MAA) nanoparticles were characterized by Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), photo correlation spectroscopy (PCS) and vibration sample magnetometry (VSM), respectively. The results indicated that the magnetic poly(PEGMA-MAA) nanoparticles were of regularly spherical shape and remained monodisperse. The average size measured in aqueous media was 96.4 nm, which was much bigger than that in dry state, the nanoparticles behaved superparamagnetic with saturated magnetization of 64.8 emu/g, the zeta potential was -18.3 mV at physiological pH 7.2, and the magnetic poly(PEGMA-MAA) nanoparticles had a high stability in vitro. A typical anti-inflammatory drug, ibuprofen, was used for drug loading, and the release behavior of ibuprofen in a simulated body fluid (SBF, pH 7.4) was studied. The results indicated that these novel magnetic nanoparticles had a high drug-loading capacity and favorable release properties for ibuprofen. The magnetic poly(PEGMA-MAA) nanoparticles are very promising for application in drug delivery.


Assuntos
Portadores de Fármacos/química , Portadores de Fármacos/metabolismo , Magnetismo , Metacrilatos/química , Nanopartículas/química , Processos Fotoquímicos , Polietilenoglicóis/química , Ácidos Polimetacrílicos/química , Biomimética , Líquidos Corporais/metabolismo , Portadores de Fármacos/síntese química , Concentração de Íons de Hidrogênio , Ibuprofeno/química , Ibuprofeno/metabolismo , Tamanho da Partícula , Análise Espectral , Termogravimetria
13.
Drug Test Anal ; 1(3): 128-34, 2009 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-20355186

RESUMO

A novel trivalence dysprosium(Dy(3+))-sensitized chemiluminescence method was developed for the first time for the determination of enoxacin (ENX) using flow-injection sampling based on the chemiluminescence (CL) associated with the reaction of the Dy(3+)-cerium(Ce(IV))-S(2)O(3) (2-)-ENX system and the Dy(3+)-MnO(4) (-) S(2)O(3) (2-)-ENX system. The analytical conditions for CL emission were investigated and optimized. The relationship between the CL intensity of ENX and its concentration has good linearity, with a correlation coefficient of 0.9984-0.9994. The limit of detection (LOD, 3sigma) was 0.20 ng/mL for the Dy(3+)-ENX-S(2)O(3)(2-)-Ce(IV)-H(2)SO(4) system and 0.22 ng/mL for the Dy(3+)-ENX-S(2)O(3)(2-)-MnO(4) (-)-HNO(3) system. The relative standard deviation (RSD, n = 11) was 1.8% for 11 determinations of 60 ng/mL ENX. The proposed method was applied to the analysis of ENX in injections, serum and urine samples with a recovery of 98%-105%. A possible mechanism for this sensitized CL reaction is discussed by comparing the CL spectra with the fluorescence emission spectra. The proposed method represents a wide linear range, high sensitivity and accuracy, and can be used for the routine determination of ENX in pharmaceutical preparations and biological fluids.


Assuntos
Líquidos Corporais/metabolismo , Disprósio/metabolismo , Enoxacino/metabolismo , Luminescência , Preparações Farmacêuticas/metabolismo , Líquidos Corporais/química , Enoxacino/química , Análise de Injeção de Fluxo/métodos , Humanos , Preparações Farmacêuticas/química
14.
J Chromatogr A ; 1212(1-2): 1-9, 2008 Nov 28.
Artigo em Inglês | MEDLINE | ID: mdl-18950771

RESUMO

Novel water-compatible molecularly imprinted polymers (MIPs) were synthesized in methanol-water systems with ofloxacin as templates and methacryclic acid as functional monomers. The MIPs were used as a special sorbent for the selective solid-phase extraction (SPE) of nine quinolones from urine samples, showing high affinity to the quinolones in aqueous environment. Its molecular recognition mechanisms were investigated by the molecular simulation and the experimental validation with UV and infrared spectrogram as well as (1)H NMR. Binding capability and chromatographic characteristic were also evaluated. By using the water-compatible MIPs as SPE sorbents, the nine quinolones can be selectively extracted and enriched, while all matrices interferences were eliminated simultaneously. Under the optimal conditions of SPE and high performance liquid chromatography (HPLC), the good linearity of the method was obtained in a range of 0.05-30microg/mL with the correlation coefficient of >0.999 and the relative standard division of 2.0-7.4%. The detection limits (s/n=3) were in a range of 0.036-0.10microg/mL. The proposed method was successfully applied for the selective extraction and separation of the studied quinolones in urine samples.


Assuntos
Ofloxacino/síntese química , Polímeros/síntese química , Quinolonas/urina , Extração em Fase Sólida/métodos , Sítios de Ligação , Cromatografia Líquida de Alta Pressão , Simulação por Computador , Humanos , Ligação de Hidrogênio , Concentração de Íons de Hidrogênio , Metacrilatos/síntese química , Metacrilatos/química , Modelos Moleculares , Ofloxacino/química , Polímeros/química , Quinolonas/química , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Solventes/química , Água/química
15.
J Chromatogr Sci ; 46(4): 351-5, 2008 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-18402728

RESUMO

A liquid chromatographic method for the determination of closantel residues in milk and tissues is developed and validated. An acetonitrile-acetone solution (80:20, v/v) is used for the extraction of closantel residues from milk and animal tissues, and the extract is purified by solid-phase extraction with Oasis MAX cartridges and a mixture of formic acid-acetonitrile (5:95, v/v) as the elution solution. A C(18) bonded silica column is used for chromatographic separation. The mobile phase consists of acetonitrile-water (85:15, v/v) containing 0.05% triethylamine at pH 2.5, adjusted with phosphoric acid with the flow-rate set at 1.0 mL/min. Using the fluorescence emission of closantel at lambda(ex) = 335 nm and lambda(ex) = 510 nm, the calibration curve is linear, with a correlation coefficient of 0.9999 over the concentration range of 10-5000 microg/kg for the tissue sample and 10-5000 microg/L for the milk sample. The detection limit (s/n = 3) is 3 microg/kg for tissue sample and 3 microg/L for milk sample. The intra- and inter-day repeatabilities are between 3.35-7.66% and 4.04-8.67%, respectively. The proposed method enables the quantitative determination of closantel residues at levels as low as 10 microg/kg in animal tissue samples and 10 microg/L in milk samples.


Assuntos
Anti-Helmínticos/análise , Cromatografia Líquida de Alta Pressão/métodos , Rim/química , Fígado/química , Leite/química , Músculo Esquelético/química , Salicilanilidas/análise , Animais , Bovinos , Feminino , Fluorescência , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Extração em Fase Sólida/instrumentação , Extração em Fase Sólida/métodos
16.
Guang Pu Xue Yu Guang Pu Fen Xi ; 28(11): 2684-90, 2008 Nov.
Artigo em Chinês | MEDLINE | ID: mdl-19271518

RESUMO

A mechanism of hydride generation based on disassembly reaction of hydrogen-transferred interim state [M(BH4)m]* was developed by investigating the effect of reaction medium acidity on hydride generation. The effects of Co2+ and Ni2+, phenanthroline and 8-hydroxyquinoline on hydride generation-atomic fluorescence signals of Zn, Cd, Cu and Ni were studied, respectively, and their enhancing mechnism was discussed. The enhancing effect Co2+ and Ni2+ on the fluorescence signals of Zn and Cd was due to the increase in transmission efficiency of hydride of Zn and Cd. There was a synergic enhancing effect between phenanthroline or 8-hydroxyquinoline and Co2+ on the fluorescence signals of Zn and Cd, however no synergic enhancing effect between phenanthroline and 8-hydroxyquinoline on the fluorescence signals of Zn and Cd. The simulative action of cationic surfactant, anion surfactant and non-ionic surfactant surfactant to hydride generation was investigated. It is shown that both cationic surfactant and non-ionic surfactant have obvious enhancing effect on the fluorescence signals of analytes because of the decrease in surface tension of reaction solution. The release characteristics of hydride from the absorption solution containing surfactant was ulteriorly examined by using graphite furnace atomic absorption spectrometry, and the mechanism of enhancing effect of surfactant on hydride generation and transmission was proposed.


Assuntos
Espectrometria de Fluorescência , Elementos de Transição/química , Cádmio/química , Cobre/química , Oxiquinolina/química , Fenantrolinas/química , Zinco/química
17.
Ultrason Sonochem ; 15(5): 717-23, 2008 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-17998169

RESUMO

At its natural pH (6.95), the decolorization of Reactive red 24 in ultrasound, ultrasound/H2O2, exfoliated graphite, ultrasound/exfoliated graphite, exfoliated graphite/H2O2 and ultrasound/exfoliated graphite/H2O2 systems were compared. An enhancement was observed for the decolorization in ultrasound/exfoliated graphite/H2O2 system. The effect of solution pH, H2O2 and exfoliated graphite dosages, and temperature on the decolorization of Reactive red 24 was investigated. The sonochemical treatment in combination with exfoliated graphite/H2O2 showed a synergistic effect for the decolorization of Reactive red 24. The results indicated that under proper conditions, there was a possibility to remove Reactive red 24 very efficient from aqueous solution. The decolorization of other azo dyes (Reactive red 2, Methyl orange, Acid red 1, Acid red 73, Acid red 249, Acid orange 7, Acid blue 113, Acid brown 75, Acid green 20, Acid yellow 42, Acid mordant brown 33, Acid mordant yellow 10 and Direct green 1) was also investigated, at their natural pH.

18.
Ultrason Sonochem ; 15(1): 37-42, 2008 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-17350318

RESUMO

The decolorization of acid black 210 by ultrasonic irradiation in the presence of exfoliated graphite was investigated. Low pH value and large exfoliation volume of exfoliated graphite favored the ultrasonic decolorization of acid black 210. The combination method of ultrasonic waves and exfoliated graphite achieved better results than either exfoliated graphite or ultrasound alone. Improved decolorization efficiency has been observed in the present system compared to the process using a combination of ultrasound and activated carbon. In the combination method of ultrasonic waves and exfoliated graphite, approximately 99.5% of acid black 210 was removed using 0.8 g/l exfoliated graphite at a pH of 1 within 120 min at 51 degrees C.


Assuntos
Compostos Azo/química , Carbono/química , Corantes/química , Grafite/química , Naftalenossulfonatos/química , Compostos de Enxofre/química , Ultrassom , Compostos Azo/isolamento & purificação , Peróxido de Hidrogênio/química , Concentração de Íons de Hidrogênio , Microscopia Eletrônica de Varredura , Modelos Químicos , Naftalenossulfonatos/isolamento & purificação , Espectrofotometria Ultravioleta , Temperatura , Fatores de Tempo
19.
J Chromatogr B Analyt Technol Biomed Life Sci ; 857(2): 296-300, 2007 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-17719280

RESUMO

A method was developed for the determination of the seven nitroimidazoles including metronidazole (MNZ), ronidazole (RNZ), dimetridazole (DMZ), tinidazole (TNZ), ornidazole (ONZ), secnidazole (SNZ) and the common metabolite of RNZ and hydroxydimetridazole (DMOHZ) in poultry and pork muscles by high-performance liquid chromatography (HPLC) with ultraviolet detection (UV). After extraction with ethyl acetate and evaporation, the nitroimidazoles were redissolved in ethyl acetate and purified using strong cation exchange (SCX) solid-phase extraction (SPE) column. The HPLC separation was carried through on a C(18) bonded silica column with a deionized water-methanol-acetonitrile mobile phase using a gradient elution procedure. The limit of detection of all the seven nitroimidazoles was 0.2 microg/kg. The recoveries of the seven nitroimidazoles for chicken, pork and bacon samples spiked with 1-20 microg/kg were in the range of 71.4-99.5%. The linearity is satisfactory with a correlation coefficient of >0.998 at concentrations ranging from 0.7 to 60 microg/kg. The relative standard deviations of 10 measurements for spiked chicken, pork and bacon samples at the concentration of 1 and 20 microg/kg were in the range of 6.2-13.9% and 4.0-8.7%, respectively. The intra-day precision (n=5) for nitroimidazoles residues in chicken spiked at 20 microg/kg is 6.9%, and the inter-day precision for 5 days (n=25) is 11%. The method is capable of identifying nitroimidazole residues at > or =0.7 microg/kg levels and was applied in the determination of nitroimidazole residues in meat sample.


Assuntos
Carne/análise , Nitroimidazóis/análise , Extração em Fase Sólida/métodos , Animais , Cromatografia Líquida de Alta Pressão , Nitroimidazóis/química , Nitroimidazóis/isolamento & purificação , Padrões de Referência , Reprodutibilidade dos Testes , Soluções , Espectrofotometria Ultravioleta , Fatores de Tempo
20.
J Chromatogr A ; 1164(1-2): 120-8, 2007 Sep 14.
Artigo em Inglês | MEDLINE | ID: mdl-17692322

RESUMO

An accurate method based on the use of gel permeation chromatography (GPC)-liquid chromatography-tandem mass spectrometry interfaced with electrospray ionization (GPC-LC-ESI-MS/MS) was devised for the simultaneous determination of Sudan (I-IV), Sudan Orange G, Sudan Red B, Sudan Red G, Sudan Red 7B, Butter Yellow and Para Red in hot chili products. A GPC clean-up procedure was developed for simultaneous quantification of 10 dyes in hot chili and hot chili products avoiding some interference and permitting multiple injections without damaging the column. A HPLC was performed on an Inertsil C18 column using a multistep gradient elution with 0.1% formic acid and methanol as the mobile phase. Mass spectral acquisition was done in positive ion mode. Linearity of around three orders in the magnitude of concentration was generally obtained with the correlation coefficients (r2) of 0.9984-0.9997. Limit of detection (LOD) and limit of quantification (LOQ) for the investigated dyes were in the ranges of 0.1-1.8 and 0.4-5.0 microg/kg depending on matrices, respectively. The recoveries of the 10 synthetic dyes in five matrices ranged from 81.7 to 92.9%. The intra- and inter-day precision (RSDs) was between 2.9-7.8 and 3.9-8.1%, respectively. This method has been applied successfully for the determination of the studied 10 banned dyes in hot chili products.


Assuntos
Compostos Azo/análise , Cromatografia em Gel/métodos , Cromatografia Líquida de Alta Pressão/métodos , Espectrometria de Massas por Ionização por Electrospray/métodos , Especiarias/análise , Espectrometria de Massas em Tandem/métodos , Compostos Azo/química , Capsicum/química , Análise de Alimentos/métodos , Corantes de Alimentos/análise , Corantes de Alimentos/química , Estrutura Molecular , Naftóis/análise , Naftóis/química , Reprodutibilidade dos Testes
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