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1.
Zhonghua Lao Dong Wei Sheng Zhi Ye Bing Za Zhi ; 36(10): 776-778, 2018 Oct 20.
Artigo em Zh | MEDLINE | ID: mdl-30541204

RESUMO

Objective: To establish a method to detect the concentrations of ethylenediamine in the air of workplace by Ion chromatography. Methods: Ethylenediamine in the air of workplace adsorpted by Silicone tube, then ultrasonic desorped by Sulfuric acid solution (0.1 mol/L) , the desorption solution qualitative and quantitative determination by Ion chromatography. Results: For ethylenediamine, the calibration curves were liner in the range of 0.1-100.0 µg/ml, the method detection limit is 0.1 µg/ml, the minimum detectable concentration is 0.13 mg/m(3) (in terms of sampling 7.5 L) . The desorption efficiency is more than 90% on spiked levels of 2.0, 4.0 and 8.0 µg/ml, the average desorption efficiency of the method was 96.1%, the precision was 1.8%-2.1%. The recovery rate of the added standard is 98.5%-104.2%. Conclusion: The method simplifies the preprocessing steps and improves the sensitivity. All the indexes are in conformity with the requirements of the method formulation guide. It is suitable for the determination of ethylenediamine in the air of the workplace.


Assuntos
Poluentes Ocupacionais do Ar/análise , Etilenodiaminas/análise , Cromatografia por Troca Iônica , Humanos , Limite de Detecção , Local de Trabalho
2.
J Dairy Sci ; 96(4): 2349-2355, 2013 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-23415519

RESUMO

The objective was to conduct a study to investigate if violative meat residues are detected in very young bob veal calves that are fed first-milking colostrum harvested from cows that were dry treated, on-label, with cephapirin benzathine. First-milking colostrum was collected from cows that were given intramammary treatment at dry off, on-label, with cephapirin benzathine (ToMORROW, Boehringer Ingelheim Vetmedica Inc., St. Joseph, MO). Newborn bull calves meeting study inclusion criteria were removed from their dams shortly after birth and before suckling, and assigned to 1 of 2 trials. For the first trial, 6 treated calves were fed 3.8L of fresh maternal colostrum and 1 control calf was fed 1.5 doses of a plasma-derived colostrum replacer (Secure Calf Colostrum Replacer, VitaPlus Inc., Madison, WI) within 1h after birth. For the second trial, 5 treated calves were fed 3.8L of fresh maternal colostrum and 1 control calf was fed 1.5 doses of Secure Calf Colostrum Replacer within 1h after birth. All calves were humanely euthanized at 24h (trial 1) or 48h (trial 2) of age, and tissues were harvested for antimicrobial residue testing. Samples of maternal colostrum and colostrum replacer were also submitted for antimicrobial residue testing. Kidneys collected from all study calves tested negative for cephapirin benzathine residues when using both the KIS assay (Charm Sciences, Lawrence, MA) and liquid chromatography-tandem mass spectrometry analysis. The potential transfer of cephapirin from cows treated on-label at dry off to calves via colostrum may not be a significant source of cephapirin residues in veal tissues.


Assuntos
Antibacterianos/análise , Cefapirina/análise , Colostro/química , Dieta/veterinária , Contaminação de Alimentos/análise , Carne/análise , Animais , Animais Recém-Nascidos , Antibacterianos/administração & dosagem , Bovinos , Cefapirina/administração & dosagem , Resíduos de Drogas/análise , Etilenodiaminas/análise , Feminino , Rim/química , Glândulas Mamárias Animais/efeitos dos fármacos
3.
Appl Opt ; 51(16): 3445-52, 2012 Jun 01.
Artigo em Inglês | MEDLINE | ID: mdl-22695582

RESUMO

The core-mode cutoff plays a major role in evanescent field absorption based sensors. A method has been proposed to calculate the core-mode cutoff by solving the eigenvalue equations of a weakly guiding three layer optical waveguide graphically. The variation of normalized waveguide parameter (V) is also calculated with different wavelengths at core-mode cutoff. At the first step, theoretical analysis of tapered fiber parameters has been performed for core-mode cutoff. The taper angle of an adiabatic tapered fiber is also analyzed using the length-scale criterion. Secondly, single-mode tapered fiber has been developed to make a precision sensor element suitable for chemical detection. Finally, the sensor element has been used to detect absorption peak of ethylenediamine. Results are presented in which an absorption peak at 1540 nm is observed.


Assuntos
Tecnologia de Fibra Óptica/instrumentação , Miniaturização/instrumentação , Fibras Ópticas , Espectrofotometria/instrumentação , Algoritmos , Desenho de Equipamento , Etilenodiaminas/análise , Tecnologia de Fibra Óptica/métodos , Modelos Teóricos
4.
Se Pu ; 40(10): 929-936, 2022 Oct.
Artigo em Zh | MEDLINE | ID: mdl-36222256

RESUMO

Pesticides are used in the agricultural production process to ensure the yield and quality of agricultural products. However, in recent years, environmental pollution issues caused by pesticide residues have sparked widespread concern in society. It is important to develop convenient and efficient approaches to detect and monitor pesticide residues. In this study, targeting benzoylurea insecticides (BUs), polyamidoamine dendrimer-functionalized silica nanocomposite with polydopamine coating (SiO2-PAMAM-PDA) was designed and successfully synthesized. First, monodisperse silica nanoparticles were prepared by the hydrolysis of tetraethyl orthosilicate (TEOS) in mixed solution of ethanol, water and ammonia. The silane coupling agent (3-aminopropyl)triethoxysilane was then employed to introduce amino groups into the silica. Silica with the zeroth generation of polyamidoamine (PAMAM) modification (SiO2-PAMAM-G0) was obtained through Michael addition reaction of methyl acrylate. Ethylenediamine was added to polymerize with methyl acrylate using an amidation reaction to form the first-generation PAMAM (SiO2-PAMAM-G1). Finally, by polymerizing dopamine under alkaline conditions (pH=8.5), the SiO2-PAMAM-G1 was coated with PDA. Thus, the final product named SiO2-PAMAM-PDA was obtained. The composite was characterized using a transmission electron microscope (TEM) and an increase in surface roughness indicated the successful grafting of PDA coating. Dopamine structure contains abundant benzene rings and amino and hydroxyl groups. It could bind with BUs through multiple secondary interactions, such as hydrogen bond and π-π stacking interaction. Therefore, the introduction of PDA could effectively enhance the affinity of the material toward benzoylurea insecticides. The prepared nanocomposites were used as sorbents in a dispersive micro solid-phase extraction approach (D-µ-SPE). The established approach was employed to extract and enrich the BUs in water samples before high-performance liquid chromatography (HPLC) analysis. Diflubenzuron, triflumuron, hexaflumuron, and teflubenzuron were chosen as target analytes. The following was a typical D-µ-SPE procedure. The prepared adsorbents measuring 40 mg were first dispersed in an 8-mL sample solution containing 150 g/L NaCl. The dispersion was assisted by 120-s vortexing to ensure full contact between the SiO2-PAMAM-PDA and the targets. Next, the adsorbents were separated from the liquid phase by 4-min centrifugation (5000 r/min). Thereafter, the adsorbed benzoylureas were eluted using 1 mL acetonitrile as desorption solvent by 120-s vortexing. Separated by centrifugation, the eluate was dried under a mild nitrogen stream. The solid remains were redissolved in 0.1 mL of acetonitrile, filtered by filter membrane (0.22 µm), and then analyzed by HPLC. The experimental conditions in the D-µ-SPE process could have a great impact on the extraction efficiency. Experimental conditions were optimized using a single factor optimization approach to further enhance the extraction recoveries. The optimized conditions included adsorbent amount, extraction time, desorption solvent type, desorption solvent volume, desorption time, and NaCl addition amount. Under the optimal conditions, a linearity range of 10-500 µg/L and limits of detection (LODs, S/N=3) of 1.1-2.1 µg/L were obtained. The extraction recoveries and relative standard deviations (RSDs) of the four BUs were 82.8%-94.1% and 2.1%-8.0%, respectively. The established approach was compared with reported approaches targeting benzoylurea insecticides. It was discovered that this approach consumed less sample, material, organic solvent, and pretreatment time. It provided a more rapid and green choice for the determination of benzoylurea pesticides. To determine the applicability, the proposed approach was applied to analyze the four benzoylurea insecticides in three river water samples. The real water samples were pretreated using the developed approach ahead of instrumental analysis, and no benzoylurea pesticides residue was detected. Next, standard addition experiments were performed under three spiking levels, including 15, 50, and 200 µg/L. The established approach had good accuracy and feasibility with satisfactory recoveries (69.5%-99.4%) and RSDs (0.2%-9.5%).


Assuntos
Dendrímeros , Diflubenzuron , Inseticidas , Nanocompostos , Resíduos de Praguicidas , Acetonitrilas/análise , Acrilatos , Amônia/análise , Benzeno/análise , Cromatografia Líquida de Alta Pressão , Dendrímeros/análise , Diflubenzuron/análise , Dopamina/análise , Etanol/análise , Etilenodiaminas/análise , Indóis , Inseticidas/análise , Nanocompostos/análise , Nitrogênio/análise , Resíduos de Praguicidas/análise , Poliaminas , Polímeros , Silanos/análise , Dióxido de Silício/análise , Cloreto de Sódio/análise , Extração em Fase Sólida , Solventes/análise , Água/análise
5.
Food Chem ; 316: 126396, 2020 Jun 30.
Artigo em Inglês | MEDLINE | ID: mdl-32066068

RESUMO

This study employed the use of a microfluidic paper-based analytical device (µPAD) to determine the concentration of nitrite in pork and enhanced the limit of detection by analyzing the coffee-ring effect. The µPAD was fabricated by designing and embedding wax channels onto the cellulose-based filter paper through printing and subjecting the paper to heat treatment to allow wax penetration. Nitrite concentration was determined by monitoring the colorimetric reaction that occurred between nitrite and the added Griess reagent. The limit of detection of this device for nitrite in pork was determined to be 19.2 mg kg-1 by analyzing the inner-chamber reaction, while it could be as low as 1.1 mg kg-1 if the coffee-ring region was analyzed. The overall analysis could be completed within 15 min. This µPAD-based method has potential applications to routinely screen the nitrite concentration of meat products and ensure food safety and consumer health.


Assuntos
Nitritos/análise , Carne Vermelha/análise , Animais , Colorimetria , Etilenodiaminas/análise , Filtração , Dispositivos Lab-On-A-Chip , Técnicas Analíticas Microfluídicas/instrumentação , Papel , Sulfanilamidas/análise , Suínos
6.
Anal Chem ; 81(14): 5827-32, 2009 Jul 15.
Artigo em Inglês | MEDLINE | ID: mdl-19522515

RESUMO

The selective determination of the diamine ethylenediamine (EDA) in the presence of a higher amount of residual dimethylamine in cationic polymers has been developed. The strategy uses both a solution derivatization with a selective agent of primary amines such as o-phthaldialdehyde-N-acetyl-L-cysteine (OPA-NAC) and an in-tube solid-phase microextraction (IT-SPME) coupled to liquid chromatography (LC). A 70 cm long, 0.32 mm internal diameter, and 3 microm thick commercially available capillary column coated with 95% polydimethylsiloxane and 5% polydiphenylsiloxane was employed to replace the injection loop of a Rheodyne injection valve. A volume of 1 mL of derivatized sample was passed through the capillary, and 100 microL of water was later used for cleaning and filling the capillary. After, the injection was effected and the desorption of the derivative from the capillary was carried out in the dynamic mode using the mobile phase. Chromatographic separation was performed in less than 2 min using a monolithic silica column Onyx (100 mm x 3.0 mm i.d.) under isocratic conditions. The effect of several parameters affecting derivatization and IT-SPME was investigated. The quantification of EDA was realized over the range of 0.07-2 microg/mL with adequate linearity, accuracy, and reproducibility, and the limit of detection was 20 ng/mL. The method is rapid and low in cost, and sample handling and organic solvent consumption have been minimized. Its application to polymeric cationic surfactants used in water treatment allowed the selective quantification of residual EDA at low microgram per milliliter levels of concentration without off-line preconcentration.


Assuntos
Indústria Química , Cromatografia Líquida/métodos , Etilenodiaminas/análise , Etilenodiaminas/isolamento & purificação , Polímeros/química , Microextração em Fase Sólida/métodos , Etilenodiaminas/química , Indicadores e Reagentes/química
7.
J Trace Elem Med Biol ; 55: 44-49, 2019 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-31345364

RESUMO

While the underlying mechanisms of Parkinson's disease (PD) are still insufficiently studied, a complex interaction between genetic and environmental factors is emphasized. Nevertheless, the role of the essential trace element zinc (Zn) in this regard remains controversial. In this study we altered Zn balance within PD models of the versatile model organism Caenorhabditis elegans (C. elegans) in order to examine whether a genetic predisposition in selected genes with relevance for PD affects Zn homeostasis. Protein-bound and labile Zn species act in various areas, such as enzymatic catalysis, protein stabilization pathways and cell signaling. Therefore, total Zn and labile Zn were quantitatively determined in living nematodes as individual biomarkers of Zn uptake and bioavailability with inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) or a multi-well method using the fluorescent probe ZinPyr-1. Young and middle-aged deletion mutants of catp-6 and pdr-1, which are orthologues of mammalian ATP13A2 (PARK9) and parkin (PARK2), showed altered Zn homeostasis following Zn exposure compared to wildtype worms. Furthermore, age-specific differences in Zn uptake were observed in wildtype worms for total as well as labile Zn species. These data emphasize the importance of differentiation between Zn species as meaningful biomarkers of Zn uptake as well as the need for further studies investigating the role of dysregulated Zn homeostasis in the etiology of PD.


Assuntos
Caenorhabditis elegans/genética , Caenorhabditis elegans/metabolismo , Homeostase , Modelos Genéticos , Doença de Parkinson/genética , Doença de Parkinson/metabolismo , Sulfato de Zinco/farmacocinética , Animais , Disponibilidade Biológica , Biomarcadores/análise , Etilenodiaminas/análise , Etilenodiaminas/metabolismo , Etilenodiaminas/farmacocinética , Sulfato de Zinco/análise , Sulfato de Zinco/metabolismo
8.
J Vis Exp ; (152)2019 10 11.
Artigo em Inglês | MEDLINE | ID: mdl-31657793

RESUMO

Primaquine (PMQ), an important anti-malarial drug, has been recommended by the World Health Organization (WHO) for the treatment of life-threatening infections caused by P. vivax and ovale. However, PMQ has unwanted adverse effects that lead to acute hemolysis in patients with glucose-6-phosphate dehydrogenase (G6PD) deficiency. There is a need to develop simple and reliable methods for PMQ determination with the purpose of dosage monitoring. In early 2019, we have reported an UV-Vis and naked-eye based approach for PMQ colorimetric quantification. The detection was based on a Griess-like reaction between PMQ and anilines, which can generate colored azo products. The detection limit for direct measurement of PMQ in synthetic urine is in the nanomolar range. Moreover, this method has shown great potential for PMQ quantification from human serum samples at clinically relevant concentrations. In this protocol, we will describe the technical details regarding the syntheses and characterization of colored azo products, the reagent preparation, and the procedures for PMQ determination.


Assuntos
Antimaláricos/análise , Técnicas de Química Analítica/métodos , Etilenodiaminas/análise , Primaquina/análise , Sulfanilamidas/análise , Antimaláricos/sangue , Antimaláricos/urina , Líquidos Corporais/química , Líquidos Corporais/metabolismo , Técnicas de Química Analítica/instrumentação , Colorimetria/instrumentação , Colorimetria/métodos , Humanos , Limite de Detecção , Microscopia Ultravioleta/instrumentação , Microscopia Ultravioleta/métodos , Primaquina/sangue , Primaquina/urina
9.
Talanta ; 204: 592-601, 2019 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-31357339

RESUMO

Development of conjugated polymers with fluorescence sensing characteristics has received close attention from researchers in fields of environmental protection, biosensing and toxins detection on food. In this paper, novel polyaniline derivatives of poly(9-methyl-9H-carbazol-3-amine) and poly(9,9-dihexyl-9H-fluoren-2-amine) are prepared by facile chemical polymerization. Then they are characterized with NMR (Nuclear Magnetic Resonance), GPC (Gel Permeation Chromatography), XRD (X-Ray Diffraction), FT-IR (Fourier Transform Infrared spectroscopy), FL (Fluorescence spectrometry) and UV-vis (Ultraviolet-visible spectroscopy) characterizations and further applied to the fluorescence detection of different acids and amines. Moreover, the obtained poly(9-methyl-9H-carbazol-3-amine) displays excellent fluorescence properties in the detection for both acids and amines. Besides, this poly(9-methyl-9H-carbazol-3-amine) can not only be used for fluorescence detection in solution, but also can be prepared into solid state and applied in the gas phase fluorescence detection. This work has greatly expanded the scope of application to these polyaniline derivatives materials, opening a new path for the researches on multi-functional chemosensor.


Assuntos
Compostos de Anilina/química , Carbazóis/química , Fluorenos/química , Corantes Fluorescentes/química , Compostos de Anilina/síntese química , Carbazóis/síntese química , Etilenodiaminas/análise , Etilenodiaminas/química , Fluorenos/síntese química , Fluorescência , Corantes Fluorescentes/síntese química , Ácido Clorídrico/análise , Ácido Clorídrico/química , Ligação de Hidrogênio , Limite de Detecção , Metilaminas/análise , Metilaminas/química , Ácido Nítrico/análise , Ácido Nítrico/química , Reprodutibilidade dos Testes , Espectrometria de Fluorescência/métodos
10.
Cell Chem Biol ; 26(2): 213-222.e6, 2019 02 21.
Artigo em Inglês | MEDLINE | ID: mdl-30527998

RESUMO

Diabetes is a hyperglycemic condition characterized by pancreatic ß-cell dysfunction and depletion. Whereas methods for monitoring ß-cell function in vivo exist, methods to deliver therapeutics to ß cells are lacking. We leveraged the rare ability of ß cells to concentrate zinc to preferentially trap zinc-binding molecules within ß cells, resulting in ß-cell-targeted compound delivery. We determined that zinc-rich ß cells and islets preferentially accumulated TSQ (6-methoxy-8-p-toluenesulfonamido-quinoline) in a zinc-dependent manner compared with exocrine pancreas. Next, we asked whether appending a zinc-chelating moiety onto a ß-cell replication-inducing compound was sufficient to confer preferential ß-cell accumulation and activity. Indeed, the hybrid compound preferentially accumulated within rodent and human islets in a zinc-dependent manner and increased the selectivity of replication-promoting activity toward ß cells. These data resolve the fundamental question of whether intracellular accumulation of zinc-chelating compounds is influenced by zinc content. Furthermore, application of this principle yielded a proof-of-concept method for ß-cell-targeted drug delivery and bioactivity.


Assuntos
Quelantes/química , Células Secretoras de Insulina/metabolismo , Zinco/química , Aminoquinolinas/análise , Aminoquinolinas/química , Aminoquinolinas/metabolismo , Animais , Quelantes/metabolismo , Cromatografia Líquida de Alta Pressão , Ditizona/química , Ditizona/metabolismo , Etilenodiaminas/análise , Etilenodiaminas/química , Etilenodiaminas/metabolismo , Humanos , Células Secretoras de Insulina/citologia , Masculino , Camundongos , Camundongos Endogâmicos C57BL , Inibidores de Proteínas Quinases/síntese química , Inibidores de Proteínas Quinases/química , Inibidores de Proteínas Quinases/metabolismo , Proteínas Serina-Treonina Quinases/antagonistas & inibidores , Proteínas Serina-Treonina Quinases/metabolismo , Proteínas Tirosina Quinases/antagonistas & inibidores , Proteínas Tirosina Quinases/metabolismo , Espectrometria de Massas em Tandem , Compostos de Tosil/análise , Compostos de Tosil/química , Compostos de Tosil/metabolismo , Quinases Dyrk
11.
Se Pu ; 37(10): 1118-1123, 2019 Oct 08.
Artigo em Zh | MEDLINE | ID: mdl-31642292

RESUMO

A method was developed for the determination of N,N'-ethylenediamine disuccinic acid (EDDS) in bioconversion samples by high performance liquid chromatography (HPLC). An InertSustain AQ-C18 column (250 mm×4.6 mm, 5 µm) was used in the analysis. The mobile phase was 25% (v/v) methanol with 1.0 g/L Cu(CO2CH3)2·H2O, 2.0 g/L tetrabutylammonium hydroxide, and the pH was adjusted to 2.80 with phosphoric acid. The flow rate of the mobile phase was 1.0 mL/min, and the column temperature was set at 30℃. The detection wavelength was 254 nm. EDDS, fumaric acid, citric acid, malic acid and ethylenediaminetetraacetic acid (EDTA) were separated from one another within 8 min. EDDS showed good linearity in the range of 0.06-0.6 g/L. About 0.25 g/L EDDS was detected in the biosynthesis reaction solution catalyzed by recombinant EDDS-lyase, while 36.56 g/L malic acid was formed as the by-product from fumaric acid. The catalytic activity of the enzyme was confirmed in the hydrolysis of 10 g/L EDDS, which produced 3.05 g/L malic acid in 3 h. This analytical method is simple, rapid, sensitive, reliable, and suitable for the analysis in the research of EDDS bioconversion process.


Assuntos
Cromatografia Líquida de Alta Pressão , Etilenodiaminas/análise , Succinatos/análise
12.
Acta Pol Pharm ; 65(5): 507-13, 2008.
Artigo em Inglês | MEDLINE | ID: mdl-19051595

RESUMO

Ethylenediamine-N,N,N',N'-tetrakismethylene phosphonate (EDTMP) and ascorbic acid (AA) were determined in two batches of lyophilized experimental radiopharmaceutical kits by using ion chromatography with UV detection. The separation of EDTM and AA was carried out on PRP-X 800 weak cation exchange column and as an eluant 0.0025 mol L(-1) sodium sulfate was used. Validation parameters of both analytical procedures: limit of detection (LOD), limit of quantitation (LOQ), linearity, precision, accuracy and system suitability test (SST) parameters are presented.


Assuntos
Ácido Ascórbico/análise , Etilenodiaminas/análise , Organofosfonatos/análise , Compostos Radiofarmacêuticos/análise , Cromatografia Líquida de Alta Pressão , Kit de Reagentes para Diagnóstico , Espectrofotometria Ultravioleta
13.
Huan Jing Ke Xue ; 39(9): 4122-4131, 2018 Sep 08.
Artigo em Zh | MEDLINE | ID: mdl-30188053

RESUMO

The absorption characteristics, composition, spatial variability, and relative contribution of optically active constituents over the range of photosynthetically active radiation (PAR, 400-700 nm) were analyzed from samples collected in the Yiluo and Huntai Rivers in May 2017 and 2013, respectively. Results demonstrated that the absorption curves of total suspended particulates[ap(λ)] were similar to those of non-algae particles[ad(λ)]. Significant correlations between ap(λ) and ad(λ) were obtained, especially at 440 nm, with r=0.968 in the Yiluo River and r=0.899 in the Huntai River. Meanwhile, positive correlations between ap(λ) and the absorption of phytoplankton[aph(λ)] were observed at 675 nm. ap(λ) in the two basins was dominated by ad(λ). Moreover, the composition of auxiliary pigments and chloropyhll a concentration[Chla] showed more significant spatial variations based on aph(440)/aph(675) in the Yiluo River than in the Huntai River. In addition, CDOM absorption slopes (SCDOM) indicated that CDOM composition in the Yiluo River was dominated by exogenous substances; in comparison, the Huntai River had more endogenous substances. SCDOM in the Yiluo River was lower than in the Huntai River, indicating that the CDOM composition of the Yiluo River was inclined towards high molecular weights. Furthermore, Mr[aCDOM(250)/aCDOM(365)] showed greater ranges and lower mean values in the Yiluo River than in the Huntai River, confirming that CDOM molecular weight varied greatly in the former. CDOM molecular weight in the Huntai River was also lower than in the Yiluo River, in accordance with SCDOM results.


Assuntos
Monitoramento Ambiental , Rios , Estações do Ano , Qualidade da Água , China , Etilenodiaminas/análise , Fitoplâncton , Pigmentos Biológicos/análise
14.
J Am Soc Mass Spectrom ; 18(1): 37-47, 2007 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-17010641

RESUMO

A high-performance liquid chromatography-electrospray ionization/mass spectrometry (time of flight) method has been developed for the simultaneous determination of synthetic Fe(III)-chelates used as fertilizers. Analytes included the seven major Fe(III)-chelates used in agriculture, Fe(III)-EDTA, Fe(III)-DTPA, Fe(III)-HEDTA, Fe(III)-CDTA, Fe(III)-o,oEDDHA, Fe(III)-o,pEDDHA, and Fe(III)-EDDHMA, and the method was validated using isotope labeled (57)Fe(III)-chelates as internal standards. Calibration curves had R values in the range 0.9962-0.9997. Limits of detection and quantification were in the ranges 3-164 and 14-945 pmol, respectively. Analyte concentrations could be determined between the limits of quantification and 25 muM (racemic and meso Fe(III)-o,oEDDHA and Fe(III)-EDDHMA) or 50 muM (Fe(III)-EDTA, Fe(III)-HEDTA, Fe(III)-DTPA, Fe(III)-CDTA and Fe(III)-o,pEDDHA). The average intraday repeatability values were approximately 0.5 and 5% for retention time and peak area, respectively, whereas the interday repeatability values were approximately 0.7 and 8% for retention time and peak area, respectively. The method was validated using four different agricultural matrices, including nutrient solution, irrigation water, soil solution, and plant xylem exudates, spiked with Fe(III)-chelate standards and their stable isotope-labeled corresponding chelates. Analyte recoveries found were in the ranges 92-101% (nutrient solution), 89-102% (irrigation water), 82-100% (soil solution), and 70-111% (plant xylem exudates). Recoveries depended on the analyte, with Fe(III)-EDTA and Fe(III)-DTPA showing the lowest recoveries (average values of 87 and 88%, respectively, for all agricultural matrices used), whereas for other analytes recoveries were between 91 and 101%. The method was also used to determine the real concentrations of Fe(III)-chelates in commercial fertilizers. Furthermore, the method is also capable of resolving two more synthetic Fe(III)-chelates, Fe(III)-EDDHSA and Fe(III)-EDDCHA, whose exact quantification is not currently possible because of lack of commercial standards.


Assuntos
Cromatografia Líquida de Alta Pressão , Ácido Edético/análise , Compostos Férricos/análise , Fertilizantes/análise , Quelantes de Ferro/análise , Espectrometria de Massas por Ionização por Electrospray/métodos , Agricultura , Ácido Edético/análogos & derivados , Ácido Edético/química , Etilenodiaminas/análise , Etilenodiaminas/química , Compostos Férricos/química , Ácido Pentético/análogos & derivados , Ácido Pentético/análise , Ácido Pentético/química , Espectrometria de Massas por Ionização por Electrospray/instrumentação
15.
J Chromatogr A ; 1167(1): 27-34, 2007 Oct 05.
Artigo em Inglês | MEDLINE | ID: mdl-17765251

RESUMO

A new method for N,N'-ethylenebisstearamide (EBS) analysis was developed and validated in normal phase-HP liquid chromatography (NP-HPLC) with diol column at 50 degrees C with 100% CHCl(3) at 1 mL min(-1) and evaporative light scattering detection with elution time at 3.0 min. EBS solubility was the best at 0.80 gL(-1) in CHCl(3)/methanol 90:10. The molecular structure of commercial samples of EBS was determined by GC-MS which ascertained that the main structure is C18/C18 at approximately 45%. The remaining part was constituted by molecules with different alkyl chain length. The HPLC quantification method was proved linear (r=0.9983), accurate (99.6%) and precise (1.95%). Limit of quantification (LOQ) and limit of detection (LOD) were equal to 2.0 and 0.8 microg mL(-1), respectively. The suitability of this method was assessed with a dissolution/precipitation extraction procedure of EBS from ethylene vinyl acetate (EVA) polymer which showed that other additives and polymer do not interfere with EBS analysis. The intra-day and day-to-day precisions of extraction method were equal to 9.1% and 9.9%, respectively.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Etilenodiaminas/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Polivinil/análise , Espalhamento de Radiação , Succinatos/análise , Cromatografia Líquida de Alta Pressão/instrumentação , Cromatografia Gasosa-Espectrometria de Massas/instrumentação , Polímeros/análise , Sensibilidade e Especificidade , Volatilização
16.
J Chromatogr A ; 1169(1-2): 151-7, 2007 Oct 26.
Artigo em Inglês | MEDLINE | ID: mdl-17897656

RESUMO

A simple, selective and sensitive method for the determination of aminopolycarboxylic acids [diethylenetriaminepentaacetic acid (DTPA), S,S-ethylenediamine N,N'-disuccinic acid (EDDS), ethylenediaminetetraacetate (EDTA) and nitrilotriacetate (NTA)] has been developed using high-performance liquid chromatography with chemiluminescence detection. The aminopolycarboxylic acids were separated on a C18 reversed-phase column with an aqueous sulfuric acid mobile phase at a pH lower than 1.5. The eluate was mixed with tris(2,2'-bipyridyl)ruthenium(III), which was on-line generated by photooxidation of the ruthenium(II) complex in the presence of peroxydisulfate, and the generated chemiluminescence was detected. Calibration graphs, based on standard solutions, were linear over the range 8x10(-9) to 4x10(-5) M. The detection limits at a signal-to-noise ratio of 3 ranged from 9x10(-10) to 8x10(-8) M. The relative standard deviations of intra- and inter-day precision were below 1.3% and 2.1%, respectively. This HPLC system was successfully applied to the determination of aminopolycarboxylic acids in three different types of water samples. The low pH of the mobile phase limits interference from metal ions in natural waters. When such interference occurs, a cation-exchange column can be used to suppress it. The lowest amounts measurable were: 75 pg for NTA, 0.7 ng for EDDS, 0.8 ng for DTPA and 12ng for EDTA. The method was also applied for the EDTA assay in canned foods.


Assuntos
Ácidos Carboxílicos/análise , Cromatografia Líquida de Alta Pressão/métodos , Medições Luminescentes/métodos , Poluentes Químicos da Água/análise , Ácido Edético/análise , Ácido Edético/química , Etilenodiaminas/análise , Etilenodiaminas/química , Concentração de Íons de Hidrogênio , Indicadores e Reagentes , Metais/química , Ácido Nitrilotriacético/análise , Ácido Nitrilotriacético/química , Compostos Organometálicos/química , Ácido Pentético/análise , Ácido Pentético/química , Fotoquímica/métodos , Rutênio , Sensibilidade e Especificidade , Manejo de Espécimes , Succinatos/análise , Succinatos/química , Trometamina
17.
Sci Total Environ ; 377(1): 45-51, 2007 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-17346781

RESUMO

The biodegradability of four novel diethanolamine derivative complexing agents was examined by using two biodegradation tests standardised by OECD (301B and 301F). Ethylenediaminetetraacetic acid (EDTA) and diethylenetriaminepentaacetic acid (DTPA) were employed as reference substances. Biodegradation of the new complexing agents was studied both with unacclimated and acclimated inocula as well as by simulating wastewater treatment in sequencing batch reactors (SBRs). These new complexing agents were of technical grade, and therefore, the results are only indicative but these new compounds hold promise for use as complexing agents in the pulp and paper industry. The novel complexing agents were not readily biodegradable but they showed slight biodegradation. Around 10-30% degradation was found in the SBR where degradation was followed by measurement of concentration. Moreover the novel complexing agents did not have any negative impact on reactor performance as measured by chemical oxygen demand reduction. In the standardised biodegradation tests at best around 50% degradation was observed with the acclimated inoculum and in the prolonged test whereas EDTA and DTPA exhibited no biodegradation. The elevated degradation in acclimated sludge indicates that the water treatment plant microbes are capable of decomposing these molecules under favourable conditions. The total concentration of novel complexing agents decreased slightly during biodegradation tests, while the EDTA and DTPA concentrations remained stable.


Assuntos
Etilenodiaminas/análise , Poluentes Químicos da Água/análise , Purificação da Água/métodos , Biodegradação Ambiental , Indústria Química/instrumentação , Indústria Química/normas , Etilenodiaminas/química , Estrutura Molecular , Papel/normas , Poluentes Químicos da Água/química
18.
Artigo em Inglês | MEDLINE | ID: mdl-17267267

RESUMO

The interactions of yttrium with N,N'-ethylenebis[2-(o-hydroxyphenolic)glycine] (EHPG) and N,N'-di(2-hydroxybenzyl)ethylenediamine-N,N'-diacetic acid (HBED) are investigated by using UV difference and fluorescence spectra methods in 0.1M N-2-hydroxyethylpiperazine-N-2-ethanesulfonic acid (Hepes) at pH 7.4. Yttrium binding produces two UV difference peaks near 240 and 294 nm, respectively, that both are the characteristic of phenolic groups binding to yttrium. The molar extinction coefficient of Y-EHPG and Y-HBED are (15.7 +/- 0.40) x 10(3), (15.8 +/- 0.80) x 10(3)cm(-1)M(-1) at 240 nm, respectively. Using EDTA as a competitor the obtained conditional equilibrium constants of the complexes are logK(Y-EHPG) = 15.07 +/- 0.32 and logK(Y-HBED) = 15.18 +/- 0.26, respectively. However, the effects of yttrium binding on the fluorescence intensity of EHPG and HBED are quite different, the former showing a decrease but the latter an increase.


Assuntos
Acetatos/química , Etilenodiaminas/química , Glicina/análogos & derivados , Glicina/química , Íons , Fenol/química , Ítrio/química , Acetatos/análise , Ligação Competitiva , Ácido Edético/química , Etilenodiaminas/análise , Glicina/análise , HEPES/química , Cinética , Ligantes , Neodímio/química , Espectrofotometria/métodos , Espectrofotometria Ultravioleta/métodos
19.
Guang Pu Xue Yu Guang Pu Fen Xi ; 27(12): 2546-9, 2007 Dec.
Artigo em Zh | MEDLINE | ID: mdl-18330306

RESUMO

The fluorescence of terbium was sensitized after addition of terbium to the ethylene-N, N'-bis (o-hydioxyphenylglycine) (EHPG) solution. A novel and simple method used for the determination of Tb (III) was developed by means of fluorescence spectroscopy in the presence of EHPG. It was showed that the relative fluorescence intensity is proportional to the concentration of terbium ions, while the molar ratio of terbium to EHPG is less than 1.0 in the system. The maximum wavelengths of excitation and emission are 295 and 547 nm respectively. The optimal range of pH is 7-9. The linear range of detection of the concentration of terbium is from 1.0 x 10(-8) mol x L(-1) to 1.0 x 10(-5) mol x L(-1), with a detection limit of 1.18 x 10(-9) mol x L(-1). The relative standard deviation is still within +/-3% in the presence of other lanthanide ions. The method was applied to the determination of the recoveries of synthetic samples and a rare earth sample with satisfactory results.


Assuntos
Etilenodiaminas/análise , Térbio/análise , Espectrometria de Fluorescência
20.
Guang Pu Xue Yu Guang Pu Fen Xi ; 27(2): 313-6, 2007 Feb.
Artigo em Zh | MEDLINE | ID: mdl-17514964

RESUMO

Under the conditions of 0.05 mol x L(-1) Hepes buffer at room temperature and pH 7.4, the interaction of ethylene-N,N'-bis(o-hydroxyphenylglycine) (EHPG) and Mn(II) was investigated by both fluorescence and UV difference spectra. Results showed that the molar ratio of the complex is 1:1. With the addition of manganese ions, the fluorescence peak of EHPG at 310 nm decreased, while the peaks of UV absorptivity at 238 and 291 nm increased. The molar absorptivity of Mn(II) to EHPG at 238 nm is (1.31 +/- 0.02) x 10(4) cm(-1) x mol(-1) L. The disassociation constant for Mn-EHPG was determined to be (1.36 +/- 0.21) x 10(-5). It can be concluded that the binding of Mn(II) to EHPG is not a strongly binding reaction.


Assuntos
Etilenodiaminas/análise , Manganês/análise , Espectrometria de Fluorescência/métodos , Espectrofotometria Ultravioleta/métodos , Etilenodiaminas/química , Manganês/química , Estrutura Molecular
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