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Rapid, quantitative determination of polar compounds in fats and oils by solid-phase extraction and size-exclusion chromatography using monostearin as internal standard

Márquez-Ruiz, G.; Jorge, N.; Martín-Polvillo, M.; Dobarganes, M. C.
Fonte: Universidade Estadual Paulista Publicador: Universidade Estadual Paulista
Tipo: Artigo de Revista Científica Formato: 55-60
ENG
Relevância na Pesquisa
96.18%
A rapid and simple method was developed for quantitation of polar compounds in fats and oils using monostearin as internal standard. Starting from 50 mg of oil sample, polar compounds were obtained by solid-phase extraction (silica cartridges) and subsequently separated by high-performance size-exclusion chromatography into triglyceride polymers, triglyceride dimers, oxidized triglyceride monomers, diglycerides, internal standard and fatty acids. Quantitation of total polar compounds was achieved through the internal standard method and then amounts of each group of compounds could be calculated. A pool of polar compounds was used to check linearity, precision and accuracy of the method, as well as the solid-phase extraction recovery. The procedure was applied to samples with different content of polar compounds and good quantitative results were obtained, especially for samples of low alteration level.

Avaliação de diferentes sorventes na extração em fase solida de pesticidas em agua : desenvolvimento e validação de metodologia; Evaluation of different sorbents for the solid phase extraction of pesticides in water: development and validation of the methodology

Leonardo Jardim da Silva Faria
Fonte: Biblioteca Digital da Unicamp Publicador: Biblioteca Digital da Unicamp
Tipo: Dissertação de Mestrado Formato: application/pdf
Publicado em 19/08/2004 PT
Relevância na Pesquisa
96.11%
Muitos contaminantes orgânicos estão presentes em água em baixas concentrações. Devido a isso, tem crescido o interesse em desenvolver técnicas de preparo de amostra que possibilitem pré-concentrar os analitos presentes na matriz para adequação ao sistema de detecção. Neste trabalho foi empregada a extração em fase sólida (EFS) com diferentes sorventes, tubos de extração C-18 e de poliestireno-divinilbenzeno (PS-DVB) e coluna de PS-DVB, para extrair pesticidas presentes em água. Os pesticidas estudados foram: bentazona, cianazina, simazina, 2,4-D, atrazina, diuron e linuron. Para a separação dos pesticidas utilizou-se a cromatografia líquida de alta eficiência (CLAE), com coluna analítica C-18 Nova Pak-Waters, 150 mm x 3,9 mm d.i., tamanho de partícula de 4 mm e 6 nm de diâmetro de poro. A fase móvel utilizada foi MeOH:H2O 50:50 v/v pH 3,75 (ajustado com ácido fosfórico) e a detecção foi feita por um detector por arranjo de diodos. Na separação cromatográfica obtiveram bons valores de resolução, maiores que 3,0 para todos os pesticidas, os fatores de retenção também foram adequados, estando numa faixa de 1,0 a 14. Os melhores volumes de amostras utilizados na extração foram de 200 mL para tubos C18 ( fator de pré-concentração de 400 vezes ) e de 750 mL para tubos e colunas de PS-DVB ( fator de pré-concentração de 1500 vezes ). A adição de sal na amostra não melhorou os resultados de recuperação para todos os pesticidas em comparação com a amostra isenta de sal. A extração com tubos e colunas de PS-DVB mostrou-se mais adequada para recuperações de pesticidas polares do que os tubos C18...

Aplicação de campos elétricos em procedimentos de extração em fase sólida; Application of electric fields in solid phase extraction procedures

Ricardo Mathias Orlando
Fonte: Biblioteca Digital da Unicamp Publicador: Biblioteca Digital da Unicamp
Tipo: Tese de Doutorado Formato: application/pdf
Publicado em 03/06/2011 PT
Relevância na Pesquisa
96.16%
O preparo de amostra representa uma etapa determinante e crítica no processo de análise e a extração em fase sólida (SPE) é uma técnica amplamente empregada no preparo de matrizes complexas. O objetivo deste trabalho foi o desenvolvimento de dispositivos e procedimentos que permitem aplicar campos elétricos em SPE empregando cartuchos (E-SPE®), visando adicionar os mecanismos da eletroforese ao processo cromatográfico. Para tanto, foram desenvolvidos eletrodos e cartuchos que possibilitam a aplicação de campos elétricos, além de um sistema para monitorar e controlar parâmetros eletrocromatográficos tais como: vazão, corrente elétrica, potencial elétrico e temperatura. Com esses dispositivos foram realizadas extrações com aplicação de campo elétrico empregando compostos modelo aniônicos, catiônicos e anfotéricos. Para permitir uma melhor compreensão dos fenômenos envolvidos foram avaliados diversos parâmetros de extração, entre esses: concentração de íons em solução, pH, modificador orgânico, volume de solução de lavagem e tipo de sorvente. O sistema foi avaliado também na determinação de antimicrobianos em leite. Dependendo da polaridade empregada sobre os eletrodos, a aplicação do campo elétrico foi capaz de modular (acelerar ou retardar) a saída dos compostos modelo do cartucho. Os resultados de extração obtidos demonstraram a eficácia dos dispositivos desenvolvidos...

Preparação, caracterização e aplicação de sorvente C8 imobilizado termicamente sobre sílica zirconizada para extração em fase sólida; Preparation, characterization and application of thermally immobilized C8 onto zirconized silica as sorbent for solid-phase extraction

Renata da Costa Magueta
Fonte: Biblioteca Digital da Unicamp Publicador: Biblioteca Digital da Unicamp
Tipo: Dissertação de Mestrado Formato: application/pdf
Publicado em 07/06/2013 PT
Relevância na Pesquisa
96.2%
Um novo sorvente para extração em fase sólida foi preparado utilizando a imobilização térmica do polímero poli(metiloctilsiloxano) sobre sílica zirconizada. Foram estudadas as etapas de preparo do sorvente, avaliando-se a quantidade de polímero, a temperatura e o tempo de imobilização e a extração do excesso de polímero não imobilizado. Também se determinou o volume de breakthrough e a eficiência de extração dos cartuchos preparados. Para avaliação da eficiência de extração dos sorventes, foram utilizadas amostras de água fortificadas com uma mistura dos agrotóxicos carbendazim, imidacloprido, acetamiprido, cimoxanil, carbofuram, carbaril, metiocarbe, tebuconazol, difenoconazol, pirimifós-metílico e piriproxifem. Os resultados de cada estudo realizado foram comparados com os obtidos para o sorvente preparado sobre sílica não modificada e foram consideradas adequadas as eficiências de extração entre 70 e 120%, com coeficiente de variação de até 20%. Com a sílica zirconizada, os melhores resultados foram obtidos com 50% de polímero sobre o suporte, imobilização a 120 °C por 4 horas e extração do excesso de polímero utilizando n-hexano, numa proporção de 36 mL de solvente para cada 1 g de material...

Solid Phase Extraction of Fluoroquinolone Antibiotics from Wastewaters – Assessment of Different Commercial Sorbents

Maia, Alexandra S.; Ribeiro, Ana R.; Castro, Paula M.L.; Tiritan, Maria E.
Fonte: Universidade Católica Portuguesa Publicador: Universidade Católica Portuguesa
Tipo: Artigo de Revista Científica
Publicado em /06/2013 ENG
Relevância na Pesquisa
96.07%
Microbial degradation of fluorinated pharmaceuticalsduring wastewater treatment processes remains inadequate in most situations. Due to incomplete elimination, these residues are continually being introduced into the aquatic environments in which they settle throughout time since many of them are resistant to degradation. Fluoroquinolone antibiotics due to its persistence and implication on resistant-bacteria development, pose special interest in environmental analysis. Due to their zwitterionic characteristics, the extraction/pre-concentration process of fluoroquinolones prior analyses is an unquestionable challenge. This work compares the solid phase extraction efficiency of four fluoroquinolones (Ofloxacin, Norfloxacin, Ciprofloxacin and Moxifloxacin) from wastewater effluents by different commercial sorbents. Prior to wastewater analysis, preliminary tests were conducted in distilled water with a larger number of sorbents. Different experimental protocols and sorbents, namely OASIS® HLB, OASIS® WAX, OASIS® WCX (500 mg) and the molecularly imprinted polymer SupelMIP TM were applied to wastewater samples collected from a municipal wastewater treatment plant from the north of Portugal. The extracts were analyzed by a HPLC withFluorescence Detection validated method using a Luna PFP (2) 3µm column. Despite good results obtained with the molecularly imprinted polymer in distilled water...

Development of a selective sorbent for the solid-phase extraction of terbuthylazine in olive oil samples: A molecular imprinting strategy

Garcia, Raquel; Martins, Nuno; Carreiro, Elisabete; Simões, Marco; Ribeiro Carrot, Maria ML; Carrot, Peter J.M..; Burke, Anthony; Cabrita, Maria Joao
Fonte: Wiley Publicador: Wiley
Tipo: Artigo de Revista Científica
ENG
Relevância na Pesquisa
96.09%
Aiming to implement an analytical methodology that is highly selective for the extraction and quantification of terbuthylazine from olive oil, we successfully achieved: (i) the development of a molecularly imprinted polymer by bulk polymerization using terbuthylazine as template molecule,methacrylic acid as functionalmonomer, ethylene glycol dimethacrylate as cross-linker, and dichloromethane as porogen; (ii) characterization of the imprintingmaterial using Fourier transform infrared spectroscopy, thermogravimetric analysis, nitrogen adsorption at 77 K, and scanning electron microscopy; (iii) their molecular recognition for the template molecule using high-performance liquid chromatography, and (iv) optimization of a solid-phase extraction procedure using as sorbent the synthesized molecularly imprinted polymer for the selective extraction and clean-up of terbuthylazine from spiked organic olive oil and further quantification of the pesticide levels by high-performance liquid chromatography. The suitability of the implemented analytical methodology was demonstrated, as concentrations of terbuthylazine below the tolerated maximum residue limits in the spiked organic olive oil samples could be satisfactorily analyzed with good precision/ accuracy with high recovery rates (96%). Overall...

Sodium dodecyl sulfate coated γ-alumina support modified by a new Schiff base for solid phase extraction and flame-AAS determination of lead and copper ions

Shokrollahi,Ardeshir; Montazerozohori,Morteza; Mehrpour,Tahere; Tavallali,Hossein; Khafri,Batool Zare; Montaseri,Zohreh
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/01/2013 EN
Relevância na Pesquisa
96.12%
A simple and fast approach for solid phase extraction is herein described, and used to determine trace amounts of Pb2+ and Cu2+ metal ions. The solid phase support is sodium dodecyl sulfate (SDS)-coated γ-alumina modified with bis(2-hydroxy acetophenone)-1,6-hexanediimine (BHAH) ligand. The adsorbed ions were stripped from the solid phase by 6 mL of 4 M nitric acid as eluent. The eluting solution was analyzed by flame atomic absorption spectrometry (FAAS). The sorption recovery of metal ions was investigated with regard to the effects of pH, amount of ligand, γ-alumina and surfactant and the amount and type of eluent. Complexation of BHAH with Pb2+ or Cu2+ ions was examined via spectrophotometry using the HypSpec program. The detection limit for Cu2+ was 7.9 µg L-1 with a relative standard deviation of 1.67%, while that for Pb2+ was 6.4 µg L-1 with a relative standard deviation of 1.64%. A preconcentration factor of 100 was achieved for these ions. The method was successfully applied to determine analyte concentrations in samples of liver, parsley, cabbage, and water.

Spectrophotometric Determination of Aluminium in Iron Ores Using Solid-Phase Extraction

Ferreira,Sérgio Luis Costa; Lemos,Valfredo Azevedo; Costa,Antônio Celso Spinola; Jesus,Djane Santiago de; Carvalho,Marcelo Souza de
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/04/1998 EN
Relevância na Pesquisa
96.13%
In the present paper, a procedure for separation and determination of aluminium in iron matrices is proposed. It is based on the solid-phase extraction of the iron, in the form of thiocyanate complexes, by a polyurethane(PU) foam. The followings parameters were studied: effect of pH and of the thiocyanate concentration on the iron extraction, shaking time required for quantitative extraction, amount of PU foam necessary for complete extraction of iron, aluminium separation from other cations, influence of anions on the iron sorption by PU foam and analytical characteristics of the procedure for aluminium determination using methylthymol blue as chromogenic reagent. The results show that, in the pH range from 1.5 to 4.7, with a thiocyanate concentration of 0.80 mol L-1, by extraction using 1 g of polyurethane foam and a shaking time of 1 min, aluminium (40 mug) can be separated from large amounts of iron (10 mg), 800 mug of copper(II), cobalt(II), zinc(II), mercury(II), tin(IV), manganese(II) and tungsten(V); 100 mug of titanium(IV) and lead(II); and 50 mug of vanadium(V). Calcium(II), barium(II), strontium(II) and magnesium(II) can not be separated by this process, but do not react with MTB under the conditions used for aluminium determination. The anions nitrate...

Pre-concentration and determination of trace uranium (VI) in environments using ion-imprinted chitosan resin via solid phase extraction

Liu,Yunhai; Cao,Xiaohong; Le,Zhanggao; Luo,Mingbiao; Xu,Wenyuan; Huang,Guolin
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/01/2010 EN
Relevância na Pesquisa
96.14%
The uranyl-ion-imprinted and non-imprinted cross-linked chitosan resins possessing quinoline-8-ol moiety have been prepared. In all the cases, a significant imprinting effect was noticed on comparing percent extraction of uranium (VI). The resulting ion-imprinted resin was used for solid phase extractive preconcentration of uranium (VI) prior to its determination by spectrophotometry. Experimental variables that influence the quantitative extraction of uranium (VI) were optimized by both static and column methods. The retention capacity found for uranium (VI) was 218 mg g-1 of resin which is higher than the corresponding non-imprinted resins and other solid phase extraction sorbents possessing quinoline-8-ol moiety. The optimum pH range was 4.5-7.0. Uranium adsorbed was easily and quantitatively eluted with 1 mol L-1 HCl (10 mL) at a flow rate of 2 mL min-1. Interference studies showed a high tolerance of diverse ions and electrolyte species. The limit of detection was 2 µg L-1 and the dynamic linear range was 5-100 µg L-1. The accuracy of the developed method was tested with one uranium ore standard reference material. Furthermore, the proposed method was successfully applied for the determination of uranium in contaminated soil and sediment samples.

Determination of the hydrophobic fraction of Ca, Fe, Mg and Zn in dark color honeys using solid phase extraction and flame atomic absorption spectrometry

Pohl,Pawel; Stecka,Helena; Greda,Krzysztof; Jamroz,Piotr
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/06/2012 EN
Relevância na Pesquisa
96.12%
In this study, the hydrophobic fraction of Ca, Fe, Mg and Zn in dark honeys was assessed by means of solid phase extraction using silica gel based material with monomerically bonded phenyl active groups (Discovery® DSC-Ph tubes). It was found that Fe is associated with this fraction, likely polyphenolic compounds, to the highest degree. The contribution of the hydrophobic fraction to the total content of this element in analyzed honeys accounted for 7-43%. The reliability of these results was verified using for solid phase extraction silica gel based material with polymerically bonded octadecyl active groups (SupercleanÔ ENVI DSC-18). Additionally, a strong positive correlation was established between the concentration of Fe in the hydrophobic fraction assessed and the optical density of dark honeys, indicating a possible contribution of blue complexes of this metal with phenolic substances to the overall color of honey.

Preconcentration and determination of cadmium in water and food samples by in situ surfactant-based solid-phase extraction and flame atomic absorption spectrometry

Jamali,Mohammad Reza; Boromandi,Afsaneh
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/06/2014 EN
Relevância na Pesquisa
96.11%
In situ surfactant-based solid-phase extraction (ISS-SPE) is proposed as a preconcentration procedure for the determination of cadmium in water and food samples by flame atomic absorption spectrometry. In the present work, cetyltrimethylammonium bromide was used as a cationic surfactant, hexafluorophosphate ion as an ion-pairing agent and 4-benzylpiperidinedithiocarbamate potassium salt (K-4-BPDC) as a chelating agent. Several variables that affect the extraction efficiencies such as pH, type and amount of surfactant, concentration of ion-pairing agent, concentration of chelating agent, ionic strength and extraction time were investigated and optimized. After optimization of the complexation and extraction conditions, an enrichment factor of 40 was obtained. The calibration curve was linear in the range of 1-50 µg L-1 and the limit of detection was 0.3 µg L-1. The relative standard deviation for 20 µg L-1 of cadmium was lower than 2.2%. Validation of the methodology was performed by standard addition method and analysis of certified reference materials. The method was successfully applied to the determination of cadmium in various food and water samples.

Ligand-Less in situ Surfactant-Based Solid Phase Extraction for Preconcentration of Cobalt, Nickel and Zinc from Water Samples Prior to their FAAS Determination

Mohammadi,Sayed Z.; Afzali,Daryoush; Fallahi,Zahra; Mehrabi,Asieh; Moslemi,Shima
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/01/2015 EN
Relevância na Pesquisa
96.12%
A new simple and rapid ligand-less in situ surfactant-based solid phase extraction (LL-ISSPE) was developed for preconcentration of cobalt, nickel and zinc in water samples. In this method, a cationic surfactant containing a proper alkyl group (n-dodecyltrimethylammonium bromide) is dissolved in the aqueous sample and then a proper ion-pairing agent (ClO4−) is added. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed and precipitate of the analytes was adsorbed on surface of sorbent. After centrifugation, the sediment is dissolved in 3.0 mL HNO3 in ethanol and then aspirated directly into the flame atomic absorption spectrometer. Variables affecting the extraction efficiencies such as pH, concentrations of surfactant and ion pair, CO32− amount, extraction time, time and rate of centrifuge were optimized. Detection limits for Co(II), Ni(II) and Zn(II) based on 3Sb/m were 1.0, 1.5 and 0.3 ng mL−1, respectively. The proposed method has been successfully applied for the determination of cobalt...

Electric Field-Assisted Solid Phase Extraction: Study of Electrochromatographic Parameters with an Anionic Model Compound

Orlando,Ricardo M.; Rohwedder,Jarbas J. R.; Rath,Susanne
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/02/2015 EN
Relevância na Pesquisa
96.14%
Electric field-assisted solid phase extraction using syringe type cartridges (E-SPE) is a recent approach with a high capacity to obtain differential selectivity and/or recovery in comparison with conventional solid phase extraction (SPE). In this work, E-SPE was employed for the extraction of the anionic dye sunset yellow. During the washing step the electric field was evaluated with the top electrode negatively (E-SPE(–/+)) or positively charged (E-SPE(+/–)) and the results were compared with conventional SPE to understand how the electrochromatographic parameters can influence the recovery of the dye. Using the E-SPE(–/+) the electric field can increase the elution of the dye from the cartridge by over 57-fold. This notable result can be attributed to the electrophoretic velocity of the dye in the direction of the flow rate of the eluent. These results demonstrated that E-SPE is an interesting approach to elute ionic compounds with reduced volumes of eluent or less amount of organic solvent.

Preparation of an Immunosorbent and its use in the Solid Phase Extraction of Benzodiazepines

Quintana, Jorge E
Fonte: FIU Digital Commons Publicador: FIU Digital Commons
Tipo: Artigo de Revista Científica Formato: application/pdf
Relevância na Pesquisa
96.17%
The use of capillary electrophoresis (CE) has been restricted to applications having high sample concentrations because of its low sensitivity caused by small injection volumes and, when ultraviolet (UV) detection is used, the short optical path length. Sensitivity in CE can be improved by using more sensitive detection systems, or by preconcentration techniques which are based on chromatographic and/or electrophoretic principles. One of the promising strategies to improve sensitivity is solid phase extraction (SPE). Solid Phase Extraction utilizes high sample volumes and a variety of complex matrixes to facilitate trace detection. To increase the specificity of the SPE a selective solid phase must be chosen. Immunosorbents, which are a combination of an antibody and a solid support, have proven to be an excellent option because of high selectivity of the antibody. This thesis is an exploratory study of the application of immunosorbent-SPE combined with CE for trace concentration of benzodiazepines. This research describes the immobilization and performance evaluation of an immunosorbent prepared by immobilizing a benzodiazepine-specific antibody on aminopropyl silica. The binding capacity of the immunosorbent, measured as µg of benzodiazepine/ gram of immunosorbent...

A simple method for the small scale synthesis and solid-phase extraction purification of steroid sulfates

Waller, Christopher C.; McLeod, Malcolm D.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica Formato: 7 pages
Relevância na Pesquisa
96.12%
Steroid sulfates are a major class of steroid metabolite that are of growing importance in fields such as anti-doping analysis, the detection of residues in agricultural produce or medicine. Despite this, many steroid sulfate reference materials may have limited or no availability hampering the development of analytical methods. We report simple protocols for the rapid synthesis and purification of steroid sulfates that are suitable for adoption by analytical laboratories. Central to this approach is the use of solid-phase extraction (SPE) for purification, a technique routinely used for sample preparation in analytical laboratories around the world. The sulfate conjugates of sixteen steroid compounds encompassing a wide range of steroid substitution patterns and configurations are prepared, including the previously unreported sulfate conjugates of the designer steroids furazadrol (17β-hydroxyandrostan[2,3-d]isoxazole), isofurazadrol (17β-hydroxyandrostan[3,2-c]isoxazole) and trenazone (17β-hydroxyestra-4,9-dien-3-one). Structural characterization data, together with NMR and mass spectra are reported for all steroid sulfates, often for the first time. The scope of this approach for small scale synthesis is highlighted by the sulfation of 1μg of testosterone (17β-hydroxyandrost-4-en-3-one) as monitored by liquid chromatography-mass spectrometry (LCMS).; We thank the Australian Research Council (LP120200444) for financial support.

DEVELOPMENT OF FLUOROUS SOLID-PHASE EXTRACTION (FSPE) ON A MICROCHIP AND ITS APPLICATION TO PROTEOMICS

XU, ZHENPO
Fonte: Quens University Publicador: Quens University
Tipo: Tese de Doutorado
EN; EN
Relevância na Pesquisa
96.11%
The origin of fluorous interaction was explored and experimentally examined based on both HPLC and CEC data in this project. It was found that the selective fluorous interaction is a kind of reduced instantaneous or induced dipole interaction compared to the hydrophobic interaction. A series of FPPM preparation parameters were optimized. The optimized FPPM column can resolve the components in a manner that was otherwise not possible with its non-fluorous (hydrocarbon) counterpart. Following, the CEC separation of fluorous analytes on FPPM stationary phase based upon fluorous-fluorous interaction was realized for the first time. It was also found that, quantitatively, hydrophobic stationary phases have better methylene selectivity (〖 α〗_(-CH_2-)), while fluorous stationary phases have better perfluoromethylene selectivity (〖 α〗_(-CF_2-)). Thermodynamically, ∆G_(-CF_2- → -CF_2-)^° : ∆G_(-CH_2- → -CH_2-)^° (Gibbs free energy change of transferring a –CF2– unit to pure fluorous stationary phase versus Gibbs free energy change of transferring a –CH2– unit to pure hydrophobic stationary phase) is approximately equal to 8:1. A new concept, hypothetical water percentage (HWP) based on the comparison of 〖 α〗_(-CH_2-) and〖 α〗_(-CF_2-) was proposed for the first time to quantitatively evaluate the hydrophobicity/fluorophilicity of a stationary phase. A stationary phase can be classified as fluorous stationary phase when the HWP is less than 0 (more negative indicates more fluorous)...

Solid phase extraction and spectrophotometric determination of mercury in tobacco and tobacco additives with 5-(p-aminobenzylidene)-thiothiorhodanine

Yang,Weizhu; Hu,Qun; Ma,Jing; Wang,Liming; Yang,Guangyu; Xie,Gang
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/10/2006 EN
Relevância na Pesquisa
96.12%
A highly sensitive, selective and rapid method for the determination of mercury based on the rapid reaction of mercury(II) with 5-(p-aminobenzylidene)-thiorhodanine (ABTR) and the solid phase extraction of the colored chelate with C18 disks has been developed. At pH 3.5 and in the presence of emulsifier-OP medium, ABTR reacts with mercury(II) to form a red chelate of a 1:2 (mercury to ABTR) molar ratio. This chelate was enriched by solid phase extraction with C18 disks and the retained chelate eluted form the disks with dimethyl formamide (DMF). An enrichment factor of 50 was achieved. In the DMF medium, the molar absorptivity of the chelate is 1.21´10(5) L mol-1 cm-1 at 545 nm, and Beer's law is obeyed in the 0.01~3 µg mL-1 range in the measured solution. The relative standard deviation for eleven sample replicate measurements at the 0.01 µg mL-1 level is 1.7%. This method was applied to the determination of mercury in tobacco and tobacco additives and good preconcentration was found between proposed and comparative methods results.

Development and application of solid phase extraction method for polycyclic aromatic hydrocarbons in water samples in Johannesburg area, South Africa

Sibiya,P.; Potgieter,M.; Cukrowska,E.; Jönsson,J.Ǻ; Chimuka,L.
Fonte: South African Journal of Chemistry Publicador: South African Journal of Chemistry
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/01/2012 EN
Relevância na Pesquisa
96.09%
A solid phase extraction (SPE) technique has been developed for the quantitative determination of polyaromatic hydrocarbons (PAHs) in aqueous samples. The SPE technique involved extraction of PAHs from a 100 mL sample containing 10 % methanol as a modifier onto C18 cartridges. 40 % methanol in water was used as conditioning solvent, and 3 mL acetone:THF (1:1) as eluting solvent. After eluting, the extract was reduced to 1 mL under nitrogen and then analyzed by GC-MS. The extraction was optimized for the addition of organic modifier, sample load volume, conditioning solvent, washing solvent and eluting solvent. In order to evaluate the practical applicability of SPE technique, water samples were spiked with the PAHs to give final sample concentrations between 3 and 7µg L-1. Enrichment factors of 81-135 were achieved with relative standard deviations (RSDs) of less than 6 %. Recoveries obtained ranged from 81 to 135 %. Detection limits ranged from 20.0-52.0 ng L-1. The optimized method was validated by analyzing certified reference materials. The optimized method was then applied to spiked real river samples in and around the Johannesburg area, South Africa. The concentrations obtained varied from 22.0 to 1040.0 ng L-1. The RSDs were between 2.3 and 13 %. The overall order of PAHs levels was: phenanthrene > acenaphthene > naphthalene > fluoranthene > pyrene.

Determination of Triclosan and Ketoprofen in River Water and Wastewater by Solid Phase Extraction and High Performance Liquid Chromatography

Madikizela,Lawrence M.; Muthwa,Sindisiwe F.; Chimuka,Luke
Fonte: South African Journal of Chemistry Publicador: South African Journal of Chemistry
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/01/2014 EN
Relevância na Pesquisa
96.09%
This paper describes a simple, sensitive and rapid method for the determination of triclosan and ketoprofen in wastewater influent, effluent and river water. The method involves solid phase extraction (SPE) of target compounds using Oasis HLB sorbent. Several extraction parameters such as sample pH, sample volume, SPE cartridge and SPE elution solvent were optimized. The pH of the collected samples was adjusted to 5.5, and then 100 mL of the sample was loaded into an Oasis HLB cartridge. Methanol was used to elute the retained compounds. The eluted compounds were analyzed using reversed-phase high performance liquid chromatography with photo diode array detection (HPLC-PDA). The method was validated by spiking ultra-pure water and wastewater with different concentrations of both compounds ranging from 5 ju,g L-1 to 1000ju,g L-1. Recoveries were in the range of 73 % to 104 %, and % RSD ranged from 8%to15%. The method gave good detection limits of 0.01 and 0.08 ju,g L-1 for triclosan and ketoprofen, respectively. Traces of both compounds were detected in all wastewater (influent and effluent) samples at a range of 1.2 to 9.0 ju,g L-1 and in some river water samples.

Optimisation of the membrane-assisted passive sampler and its comparison with solid phase extraction technique

Nyoni,Hlengilizwe; Chimuka,Luke; Vrana,Branislav; Cukrowska,Ewa; Tutu,Hlanganani
Fonte: Water SA Publicador: Water SA
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/07/2010 EN
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A novel membrane-assisted passive sampler was further optimised in the laboratory. It was then compared to the solid phase extraction technique in terms of the extraction efficiency, enrichment factor, detection limit and selectivity in wastewater. The passive sampler was exposed to 3 wastewater samples under laboratory conditions for 3 days. Five hundred millilitres of wastewater was extracted with C18 cartridges. The extraction efficiency of the passive sampler ranged from 4 to 10% while in solid phase extraction it was 40 to 67% for the 3 chlorophenols. In both cases, extraction efficiency was highest for 2,4-dichlorophenol. The low extraction efficiency in the passive sampler supports the idea that it is not an exhaustive extraction technique and does not disturb the chemical equilibrium of the sample. It therefore measures the bioavailable fraction of the compound and can be used for equilibrium sampling and extraction. The obtained enrichment factors from the passive sampler were 89 and 295 for 2-chlorophenol and 2,4-dichlorophenol, respectively. From solid phase extraction, enrichment factors of 102, 113 and 167 were obtained for 2-chlorophenol, 4-chlorophenol and 2,4-dichlorophenol...