RESUMEN
In this work, ultrasound-assisted rapidly synergistic cloud point extraction (UARS-CPE) and inductively coupled plasma optical emission spectrometry (ICP-OES) were combined to determine trace Pb in Gentiana rigescens Franch. ex Hemsl. (G. rigescens) samples. Under the optimal conditions, the enhancement factor (EF), limit of detection (LOD), limit of quantitation (LOQ) and precision were 33, 0.11 µg L-1, 0.37 µg L-1 and 1.3%, respectively. This method was applied to the analysis of G. rigescens samples, and the outcomes were in good agreement with the results determined by inductively coupled plasma mass spectrometry (ICP-MS). A mice model of immune liver injury induced by concanavalin A (ConA) was established, and the liver protection of G. rigescens and gentiopicroside (GPS) on it and the effects of various dosages of Pb exposure on its liver protection were studied. Pb at a dosage of 5 mg kg-1 had little effect on the liver protection of G. rigescens and GPS, while 25, 125 mg kg-1 dosages of Pb could significantly attenuate the liver protection of both. In addition, it aggravated the necrosis of hepatocytes and inflammatory cell infiltration, and these effects were dose-dependent.
Asunto(s)
Gentiana , Animales , Ratones , Gentiana/química , Plomo/toxicidad , Glucósidos Iridoides/química , HígadoRESUMEN
In this paper, the modified multi-walled carbon nanotubes were prepared by ß-cyclodextrin denoted as ß-CD-MWNTs. The structure and morphology of ß-CD-MWNTs was characterized by TEM and the dynamic adsorption of p-nitrophenol on ß-CD-MWNTs was studied by the Thomas model. Some affecting factors of dynamic adsorption and the adsorbent regeneration process such as the sewage concentration, the amount of absorbent in column, including the type of reagent, solid-liquid ratio, regeneration time, and regeneration times were investigated and optimized. The results indicated that the p-nitrophenol removal rate could reach 84% under stuffing 2 g ß-CD-MWNTs. The curves of p-nitrophenol's dynamic adsorption conformed to the Thomas model. Moreover, the adsorption capacity of regenerated ß-CD-MWNTs was similar to the fresh ß-CD-MWNT column. The optimal conditions of regenerations of ß-CD-MWNTs were shown as follows: the type of reagent is anhydrous ethanol, the solid-liquid ratio is 200:40 (mg/mL) and the regeneration time is 120 min.
Asunto(s)
Ciclodextrinas/química , Modelos Químicos , Nanotubos de Carbono/química , Nitrofenoles/química , Adsorción , beta-CiclodextrinasRESUMEN
A new molecularly imprinted polymer (MIP), selective for major metabolites of quinoxaline-1,4-dioxides, was prepared through bulk polymerisation using quinoxaline-2-carboxylic acid (QCA) as template, diethylaminoethylmethacrylate as functional monomer and ethylene glycol dimethacrylate as cross-linker in tetrahydrofuran. The synthesised MIP was characterised by Fourier transform infrared and adsorption experiments. MIP exhibited high affinity, fast kinetics for QCA and good selectivity for QCA and methyl-3-quinoxaline-2-carboxylic acid (MQCA). MIP obtained was used as a selective sorbent for molecularly imprinted solid phase extraction (MISPE) coupled with HPLC to detect QCA and MQCA. Under the optimal conditions, the limits of detection (S/N=3) of porcine, chicken and fish muscles were 0.1, 0.3, 0.1 µg/kg for QCA and 0.2, 0.3, 0.1 µg/kg for MQCA, respectively and good recoveries were obtained in the range from 60.0 to 119.4%. These results indicated the MISPE-HPLC procedure could be successfully used for the determination QCA and MQCA in animal muscles.
Asunto(s)
Sustancias de Crecimiento/aislamiento & purificación , Carne/análisis , Músculo Esquelético/química , Quinoxalinas/aislamiento & purificación , Extracción en Fase Sólida/métodos , Animales , Pollos , Cromatografía Líquida de Alta Presión/métodos , Peces , Contaminación de Alimentos/análisis , Sustancias de Crecimiento/química , Impresión Molecular , Estructura Molecular , Quinoxalinas/química , Extracción en Fase Sólida/instrumentación , PorcinosRESUMEN
This study describes the development of a sensor with molecularly imprinted polymer (MIP) sensitized with MWCNTs and Salen-Co(III) as recognition element for methimazole (MMI) determination. This is the first report of MWCNTs and Salen-Co(III) in MIP being used to enhance its conductivity and catalytic activity in the electrochemical oxidation process. The electrocatalytic mechanism of MMI was explained in detail by evaluating the obtained voltammograms at various potential sweep rates and pH of buffer solutions. A stable, sensitive analytical method of differential pulse voltammetry (DPV) was developed using the prepared MWCNTs-Salen-Co(III)-MIP electrode for the determination of amounts of MMI, resulting in a linear range of 0.5-6.0 mg L(-1) with detection limit of 0.048 mg L(-1). It was also successfully applied for MMI determination in tablets and spiked urine sample. At three concentration levels, the recoveries for two samples were achieved to 94.0-100.1% and 87.8-101.8%, respectively. Analytical reproducibility and stability of the developed method were also evaluated by RSD, which were calculated as 4.6-6.6% and 2.0-6.1% (n=3), respectively.
Asunto(s)
Técnicas Biosensibles/instrumentación , Conductometría/instrumentación , Metimazol/orina , Técnicas de Sonda Molecular/instrumentación , Nanotubos de Carbono/química , Urinálisis/instrumentación , Cobalto/química , Diseño de Equipo , Análisis de Falla de Equipo , Etilenodiaminas/química , Nanotecnología/instrumentación , Nanotubos de Carbono/ultraestructura , Polímeros/químicaRESUMEN
A new molecularly imprinted polymer (MIP), selective for major metabolites of quinoxaline-1,4-dioxides was firstly prepared by combining surface molecular imprinting technique with the sol-gel process. Methyl-3-quinoxaline-2-carboxylic acid (MQCA) was used as template, 3-aminopropyltriethoxysilane as functional monomer, and tetraethoxysilicane as cross-linker. The MIP was characterized by Fourier transform infrared and evaluated through static adsorption experiments. The results indicated that MIP had high adsorption capacity, fast binding kinetics for MQCA, and the polymer showed a high degree of cross-reactivity for quinoxaline-2-carboxylic acid (QCA). The MIP was then applied as a selective sorbent in an online solid phase extraction (SPE) coupled with high-performance liquid chromatography (HPLC). For a 50-mL sample solution, enrichment factors of 1,349 and 1,046 for QCA and MQCA, respectively, and limits of detection (S/N=3) of 0.8 and 2 ng L(-1) for QCA and MQCA, respectively, were obtained (corresponding to 0.02 and 0.04 ng g(-1) in solid samples for final 100 mL of sample solutions of 5 g of pork). The sample preparation protocol was simplified and only included one step extraction with acetonitrile (MeCN) after the release of target analytes through acidic hydrolysis without further sample cleanup. The new MIP-SPE-HPLC method was successfully applied to the quantification of trace QCA and MQCA in pork muscle with good recoveries ranging from 67% to 80% and RSD below 8%.
Asunto(s)
Carne/análisis , Impresión Molecular , Músculos/química , Polímeros/química , Quinoxalinas/aislamiento & purificación , Gel de Sílice/química , Adsorción , Animales , Cromatografía Líquida de Alta Presión , Polímeros/metabolismo , Extracción en Fase Sólida , PorcinosRESUMEN
A sensitive biotin-streptavidin amplified enzyme-linked immunosorbent assay (BA-ELISA) method was developed for the determination of chloramphenicol residues in milk. The biotin-streptavidin system was applied to enhance the sensitivity. After optimization, the detection limit of the method was found to be 0.042 +/- 0.006 ng mL(-1), which is 8-fold more sensitive than the traditional competitive ELISA using the same antibody and coating antigen. The amplification mechanism of the biotin-streptavidin system and the major factors affecting the sensitivity of detection are discussed. This method was successfully applied to determine the chloramphenicol residues in milk samples with a simple and rapid extraction procedure, and good recoveries (85.66-109.67%) were obtained. The result indicated that the biotin-streptavidin system may be a valuable tool to improve the specific detection of trace veterinary drug residues and could be widely used for routine monitoring of food samples.
Asunto(s)
Cloranfenicol/análisis , Residuos de Medicamentos/análisis , Ensayo de Inmunoadsorción Enzimática/métodos , Leche/química , Animales , Antibacterianos , Biotina/análisis , Límite de Detección , Estreptavidina/análisisRESUMEN
In the present paper, a hapten of methamidophos was synthesized and conjugated with KLH by active ester method, thus the first artificial antigen was obtained. By diazotization method methamidophos conjugated with BSA, and the second artificial antigen was obtained. The synthesized haptens were characterized by MS, IR and 1H NMR, and the two artificial antigens were determined by the method of IR spectrum. The result implied that both the artificial antigens have absorbance peaks of hapten and protein, indicating that they were prepared successfully. This could provide evidence that the method of IR spectrum can be used to determine whether the artificial antigens are synthesized successfully.
Asunto(s)
Antígenos/análisis , Espectroscopía de Resonancia Magnética/métodos , Compuestos Organofosforados/análisis , Compuestos Organotiofosforados/química , Plaguicidas/análisis , Espectrometría de Masa por Ionización de Electrospray/métodos , Espectrofotometría Infrarroja/métodos , Animales , Antígenos/química , Bovinos , Estructura Molecular , Compuestos Organofosforados/química , Plaguicidas/química , Albúmina Sérica Bovina/químicaRESUMEN
A highly selective imprinted polymer was synthesized by a surface molecular imprinting technique in combination with a sol-gel process. The imprinted polymer was evaluated by FT-IR and static and kinetic adsorption experiments. The results showed that the imprinted sorbent exhibited good recognition and selective ability, offered a faster kinetics for the adsorption and desorption of Sudan I than the non-imprinted sorbent, a saturated binding capacity (Qmax) that reached 33.47 mg g-1. The prepared sorbent was applied for the determination of trace Sudan I through on-line solid-phase coupled with high-performance liquid chromatography (SPE-HPLC). With a loading flow rate of 1.5 mL min-1 for sampling 50 mL, an enrichment factor of 1266 was achieved. The detection limit (S/N = 3) was 1.2 ng L-1, and the peak area precision (RSD) for five replicate detections of 0.01 microg L-1 Sudan I was 3.66%. The Sudan I in the chilli powder from the local market was determined at three levels (0.25, 0.5, and 1.0 ng g-1) with recoveries ranging from 80.31 to 94.02%.
Asunto(s)
Capsicum/química , Cromatografía Líquida de Alta Presión/métodos , Colorantes/análisis , Naftoles/análisis , Adsorción , Conservación de Alimentos , Gel de Sílice , Dióxido de SilicioRESUMEN
This paper reports the synthesis of five sulfonamide derivatives, the production of broad-specificity polyclonal antibodies for immunoassay of sulfonamides, and the analysis of milk samples by developed assay. The three-step synthesis procedure reported in most of the literature was adopted and modified in this study. In the procedure, the purification of the intermediate was avoided and the time of synthesis was shortened from >20 to 6-9 h with improved yields. This method is generally applicable to the synthesis of haptens containing the common structure of sulfonamides. Three haptens were coupled to keyhole limpet hemocyanin, and polyclonal antibodies were obtained from rabbits immunized with these conjugates. Using the antibodies obtained, from one of these was developed an enzyme-linked immunosorbent assay (ELISA) based on the competition between free sulfonamides and the hapten-horseradish peroxidase (HRP) conjugates. The hapten-HRP conjugate giving the best competitive results and 11 structurally different sulfonamides showed 50% inhibition at concentrations of <100 ng mL(-1). After removal of the protein with acetone, milk samples were analyzed by ELISA directly; a matrix effect could be avoided when a 1:20 dilution with phosphate-buffered saline was used, and 104-131% recoveries of spiked samples were obtained. The developed immunoassay is suitable to determine sulfisozole, sulfathiazole, sulfameter, sulfamethoxypyridazine, sulfapyridine, and sulfamethizole below the maximum residue limit in milk (100 ng mL(-1) of total sulfonamides) rapidly and reliably.
Asunto(s)
Anticuerpos/inmunología , Ensayo de Inmunoadsorción Enzimática/métodos , Haptenos/química , Leche/química , Sulfonamidas/análisis , Animales , Especificidad de Anticuerpos , Haptenos/inmunología , Hemocianinas/inmunología , Indicadores y Reactivos , ConejosRESUMEN
An antibody-based rapid, quantitative, and qualitative tube enzyme-linked immunosorbent assay (tube-ELISA) was developed and used to determine carbaryl (1-naphthyl methylcarbamate) residues in agricultural products (apple, Chinese cabbage, rice, and barley). The tube-ELISA is a competitive immunoassay in which the antibody is coated in the polystyrene tube, with a dynamic range between 0.7 and 46.3 microg kg(-1). Carbaryl was extracted from each agricultural sample by hand-shaking with methanol and examined for application to on-site analysis. After the liquid extraction, the sample extracts diluted with buffer were analyzed by rapid tube-ELISA directly. The overall test time was around 15-30 min, including sample preparation and assay performance. The results obtained from tube-ELISA correlated well with high-performance liquid chromatography (R2 > 0.9). The study shows that tube-ELISA is useful as a quality control tool and can be used to quantitatively detect carbaryl as well.