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1.
Anal Chim Acta ; 1044: 1-11, 2018 Dec 31.
Artículo en Inglés | MEDLINE | ID: mdl-30442389

RESUMEN

Structural identification is challenging in mass spectrometric imaging because of inadequate sample quantities and limited sampling time in each pixel for tandem mass spectrometry (MS/MS) experiments, which are usually used for the generation of fragment ions. We report herein the observation of a cascade of highly specific chemical bond cleavages via a low-energy photoelectron activated radical relays and a competed hole oxidization on surfaces of (Bi2O3)0.07(CoO)0.03(ZnO)0.9 semiconductor nanoparticles irradiated with the 3rd harmonic (355 nm) of the Nd3+: YAG laser. Distinguished from high energy electron impact (EI), this approach generates gaseous radical anions through the exothermic capture of low-energy tunneling electrons that are not able to cause extensive vibrational excitations. It was found not only original radical center but also secondary or even tertiary radical centers cause specific bond cleavages exclusively on α positions. The original radical center directly activates the cleavages of α-positioned chemical bonds that cause the formation of secondary radical centers. Ion fragmentations proceed along the newly formed radical centers that further activate the cleavages of their α-positioned chemical bonds. Using 8 compounds, we have demonstrated various radical reactions involved in desulfonation, cyclization, and ring contraction reactions as well as competed hole oxidization-generated hydroxyl radical substitution reactions. The interpretable fragment ions provide unambiguous experimental evidences for structural elucidation of drug residues and metabolites in mass spectrometric imaging of tissue slices without tandem mass spectrometry (MS/MS).


Asunto(s)
Electrones , Espectrometría de Masas , Nanopartículas/química , Semiconductores , Sulfaquinoxalina/análisis , Animales , Radicales Libres/química , Hígado/química , Hígado/metabolismo , Masculino , Oxidación-Reducción , Tamaño de la Partícula , Procesos Fotoquímicos , Porosidad , Ratas , Sulfaquinoxalina/metabolismo , Propiedades de Superficie
2.
Anal Chim Acta ; 982: 185-192, 2017 Aug 22.
Artículo en Inglés | MEDLINE | ID: mdl-28734358

RESUMEN

In this study, two novel fluorescence quenching immune chromatographic strips (FQICS) were developed to detect sulfaquinoxaline (SQX) in foods of animal origin. These proposed FQICSs were based on fluorescence resonance energy transfer (FRET) from fluorescence donors (quantum dots or upconversion nanoparticles) to fluorescence acceptors (colloidal gold nanoparticles). Compared with traditional colloidal gold-based immune chromatographic strips (ICS), these FQICSs showed positive correlation between the fluorescent signals and the targets, and allowed user to get test results from weak fluorescent signals. The visual detection limits of these two FQICSs were both 1 ng mL-1 in standard solution and 8 µg kg-1 in samples, while the visual detection limit of the colloidal gold-based ICS was 10 ng mL-1 in standard solution and 80 µg kg-1 in samples. Besides, the results we obtained by the use of FQICS showed high agreement with those obtained by the use of commercial ELISA kits, indicating the good accuracy of these strips. As a conclusion, these proposed FQICS based on quantum dots and upconversion nanoparticles can be applied in sensitive, rapid and on-site detection of SQX in foods of animal origin.


Asunto(s)
Cromatografía de Afinidad , Análisis de los Alimentos/instrumentación , Nanopartículas del Metal , Puntos Cuánticos , Sulfaquinoxalina/análisis , Animales , Transferencia Resonante de Energía de Fluorescencia , Límite de Detección
3.
Environ Sci Pollut Res Int ; 24(24): 19535-19545, 2017 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-28681293

RESUMEN

Sulfaquinoxaline (SQX) is a coccidiostatic drug widely used in poultry and swine production and has been frequently detected in various environmental compartments such as surface water, groundwater, soils, and sediments. In the present study, degradation of SQX by ferrous ion-activated peroxymonosulfate oxidation process (Fe(II)/PMS), a promising in situ chemical oxidation (ISCO) technique, was systematically investigated. Experimental results showed that Fe(II)/PMS process appeared to be more efficient for SQX removal relative to Fe(II)/persulfate process (Fe(II)/PS). An optimal Fe(II):PMS molar ratio of 1:1 was found to be necessary for efficient removal of SQX. Increasing the solution pH hampered the degradation of SQX, and no enhancement in SQX degradation was observed when chelating agents S,S'-ethylenediamine-N,N'-disuccinic acid (EDDS) and citrate were present. The presence of Suwannee River fulvic acid (SRFA), as a representative of aquatic natural organic matter (NOM), could inhibit the degradation of SQX. SQX was more susceptible to Fe(II)/PMS oxidation in comparison to its substructural analog 2-amino-quinoxaline (2-AQ) and other sulfonamides, i.e., sulfapyridine (SPD) and sulfadiazine (SDZ). Transformation products of SQX were enriched by solid-phase extraction (SPE) and identified by liquid chromatography-electrospray ionization-triple quadrupole mass spectrometry (LC-ESI-MS/MS). On the basis of the TPs identified, detailed reaction pathways for SQX degradation including sulfonamide bond cleavage, SO2 extrusion, and aniline moiety oxidation were proposed. Our contribution may provide some useful information for better understanding the kinetics and mechanisms of SQX degradation by sulfate radical-based advanced oxidation processes (SR-AOPs).


Asunto(s)
Antiinfecciosos/análisis , Compuestos Ferrosos/química , Peróxidos/química , Sulfaquinoxalina/análisis , Contaminantes Químicos del Agua/análisis , Purificación del Agua/métodos , Animales , Antiinfecciosos/química , Cinética , Modelos Teóricos , Oxidación-Reducción , Soluciones , Sulfaquinoxalina/química , Contaminantes Químicos del Agua/química
4.
J Agric Food Chem ; 64(19): 3908-15, 2016 May 18.
Artículo en Inglés | MEDLINE | ID: mdl-27134048

RESUMEN

A novel fluorescence immunoassay for detecting sulfaquinoxaline (SQX) in animal-derived foods was developed using NaYF4:Yb/Tm upconversion nanoparticles (UCNPs) conjugated with antibodies as fluorescence signal probes, and monodisperse magnetic polystyrene microspheres (MMPMs) modified with coating antigen as immune-sensing capture probes for trapping and separating the signal probes. Based on a competitive immunoassay format, the detection limit of the proposed method for detecting SQX was 0.1 µg L(-1) in buffer and 0.5 µg kg(-1) in food samples. The recoveries of SQX in spiked samples ranged from 69.80 to 133.00%, with coefficients of variation of 0.24-25.06%. The extraction procedure was fast, simple, and environmentally friendly, requiring no organic solvents. In particular, milk samples can be analyzed directly after simple dilution. This method has appealing properties, such as sensitive fluorescence response, a simple and fast extraction procedure, and environmental friendliness, and could be applied to detecting SQX in animal-derived foods.


Asunto(s)
Antiinfecciosos/análisis , Técnica del Anticuerpo Fluorescente/métodos , Magnetismo , Productos de la Carne/análisis , Microesferas , Nanopartículas , Poliestirenos/química , Sulfaquinoxalina/análisis , Animales , Límite de Detección , Microscopía Electrónica de Transmisión , Reproducibilidad de los Resultados , Espectroscopía Infrarroja por Transformada de Fourier
5.
Mater Sci Eng C Mater Biol Appl ; 58: 504-9, 2016 Jan 01.
Artículo en Inglés | MEDLINE | ID: mdl-26478338

RESUMEN

A potentiometric carbon paste sensor was fabricated for determination of sulfaquinoxaline (SQX) based on the use of ion-association complex of sulfaquinoxaline sodium with 2,3,5-triphenyltetrazolium chloride. The proposed sensor exhibited Nernstian slope of 58.4 ± 0.3 mV per decade for sulfaquinoxaline over a wide concentration range of 5.0 × 10(-6) to 1.0 × 10(-2)M, with a low detection limit of 3.0 × 10(-6)M. The sensor manifested advantages of fast response time, satisfactory reproducibility, long life time, high thermal stability and, most importantly, excellent selectivities for sulfaquinoxaline relative to a wide variety of common foreign inorganic cations, anions, sugars and amino acids. The sensor was successfully used for determination of sulfaquinoxaline in pharmaceutical solution, blood serum, urine and milk samples. The isothermal coefficient of the electrode was calculated by the investigation of temperature effects on the electrode potential response.


Asunto(s)
Carbono/química , Preparaciones Farmacéuticas/análisis , Sulfaquinoxalina/análisis , Calibración , Electrodos , Concentración de Iones de Hidrógeno , Preparaciones Farmacéuticas/química , Potenciometría , Estándares de Referencia , Soluciones , Sulfaquinoxalina/química , Temperatura
6.
Talanta ; 123: 63-70, 2014 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-24725865

RESUMEN

A novel porous molecularly imprinted monolithic capillary column (MIMCC) based on ternary porogen was synthesized by in situ technique with sulfaquinoxaline as the template molecule. The characteristics of the MIMCC were investigated by scanning electron microscopy, infrared spectrum, thermogravimetric analysis and solvent resistance test. The saturated adsorption amount of sulfaquinoxaline on MIMCC was 2.7 times over that on the non-imprinted monolithic capillary column (NIMCC). The MIMCC also exhibited good enrichment ability to its analogs and the enrichment factors were 46-211 for five antimicrobials. High permeability and imprinting factors as well as good stability, reproducibility and long lifetime were obtained. An on-line method based on MIMCC solid-phase microextraction coupled with high-performance liquid chromatography was developed for the determination of trace antimicrobials in complex samples. The good linearity for sulfametoxydiazine, sulamethoxazole and sulfaquinoxaline was 0.05-10 µg/L, the limits of detection (LODs) were 10.0-14.0 ng/L. The linear range for mequindox and quinocetone were 0.10-10.0 µg/L, the LODs were 20.0-27.0 ng/L respectively. The recoveries were 71.0-108.2% with relative standard deviation of 1.6-8.5%, correspondingly. The results showed that MIMCC could effectively enrich antimicrobials from complex matrices. The on-line method based on MIMCC and HPLC was selective, sensitive and convenient for trace determination of antimicrobials in complex samples.


Asunto(s)
Antiinfecciosos/análisis , Cromatografía Líquida de Alta Presión/métodos , Análisis de los Alimentos/métodos , Extracción en Fase Sólida/métodos , Animales , Antiinfecciosos/química , Antiinfecciosos/aislamiento & purificación , Pollos , Cromatografía Líquida de Alta Presión/instrumentación , Huevos/análisis , Carne/análisis , Metacrilatos/química , Microscopía Electrónica de Rastreo , Impresión Molecular , Estructura Molecular , Porosidad , Quinoxalinas/análisis , Quinoxalinas/química , Quinoxalinas/aislamiento & purificación , Reproducibilidad de los Resultados , Dióxido de Silicio/química , Solventes/química , Espectrofotometría Infrarroja , Sulfameter/análisis , Sulfameter/química , Sulfameter/aislamiento & purificación , Sulfaquinoxalina/análisis , Sulfaquinoxalina/química , Sulfaquinoxalina/aislamiento & purificación , Porcinos , Termogravimetría
7.
J Agric Food Chem ; 62(17): 3690-6, 2014 Apr 30.
Artículo en Inglés | MEDLINE | ID: mdl-24437928

RESUMEN

In 2007 chicken jerky dog treats were implicated in causing illnesses and death in dogs in several countries. Affected dogs were diagnosed with acquired Fanconi syndrome, which is characterized by kidney malfunction. Known causes of this condition include a chemical assault by various contaminants including certain drugs. For this reason investigations into possible causes of the illnesses included antibiotics that may be used in animal husbandry. Targeted analyte screens of individual imported chicken jerky dog treats using LC-MS/MS detected six illegal antibiotics in imported products of several brands. Trimethoprim, tilmicosin, enrofloxacin, sulfaclozine, and sulfamethoxazole are not allowed in chicken at any level and were found as high as 2800 ng/g (ppb). Sulfaquinoxaline was found in chicken jerky treats as high as 800 ng/g, which is well above the U.S. FDA tolerance of 100 ng/g. Although there is no evidence these contaminants were responsible for the dog illnesses, their misuse could contribute to antibiotic-resistant strains of bacteria.


Asunto(s)
Alimentación Animal/análisis , Antibacterianos/análisis , Enfermedades de los Perros/etiología , Síndrome de Fanconi/veterinaria , Contaminación de Alimentos/análisis , Productos de la Carne/análisis , Alimentación Animal/toxicidad , Animales , Antibacterianos/toxicidad , Pollos , Perros , Enrofloxacina , Síndrome de Fanconi/etiología , Fluoroquinolonas/análisis , Fluoroquinolonas/toxicidad , Contaminación de Alimentos/legislación & jurisprudencia , Productos de la Carne/toxicidad , Sulfametoxazol/análisis , Sulfametoxazol/toxicidad , Sulfaquinoxalina/análisis , Sulfaquinoxalina/toxicidad , Drogas Veterinarias/análisis , Drogas Veterinarias/toxicidad
8.
Artículo en Inglés | MEDLINE | ID: mdl-23782396

RESUMEN

A dual-label time-resolved fluoroimmunoassay (TRFIA) was introduced for the simultaneous quantification of sulfamethazine (SM2) and sulfaquinoxaline (SQX). Lanthanide (Eu(3+) and Sm(3+))-labelled antibodies were used because lanthanides have higher stabilities and narrower emission spectra than most fluorescent dyes. The sensitivity of the TRFIA for SM2 was 0.02 ng ml(-1), and the average recoveries and the intra- and inter-assay CVs were 77.2-107.6%, 5.4-10.5%, and 6.0-11.2%, respectively. The sensitivity of the TRFIA for SQX was 0.04 ng ml(-1); and the average recoveries and the intra- and inter-assay CVs were 74.1-102.8%, 4.6-10.9%, and 8.7-11.2%, respectively. The method was used to analyse chicken tissue and egg samples, and the results agreed well with the results of HPLC and enzyme-linked immunosorbent assay (ELISA) analyses, with correlation coefficients (R(2)) of 0.9415-0.9724. The TRFIA developed is a simple, fast and sensitive method for the high-throughput simultaneous screening of SM2 and SQX in edible animal tissues.


Asunto(s)
Antiinfecciosos/análisis , Técnica del Anticuerpo Fluorescente/métodos , Sulfametazina/análisis , Sulfaquinoxalina/análisis , Cromatografía Líquida de Alta Presión , Ensayo de Inmunoadsorción Enzimática , Límite de Detección , Reproducibilidad de los Resultados
9.
Rapid Commun Mass Spectrom ; 27(6): 722-30, 2013 Mar 30.
Artículo en Inglés | MEDLINE | ID: mdl-23418152

RESUMEN

RATIONALE: Sulfonamides such as sulfaquinoxaline (SQX) are among the most important antibiotic families due to their extensive use in veterinary medicine. The prediction of their fate under solar irradiation through the identification of the generated metabolites is required. However, unambiguous structural characterizations often remain a challenge particularly when several isomers could match with the same MS(2) data. METHODS: Liquid chromatography/electrospray ionization quadrupole time-of-flight mass spectrometry (LC/ESI-Q-TOFMS) in the positive ion mode, leading to the formation of the protonated forms of the studied compounds, [M + H(+)] ions, was employed. Collision-induced dissociation tandem mass spectrometry (CID-MS/MS) of the protonated molecules was carried out, and the effect of the collision energy as well as the elemental compositions of the product ions were used to propose chemical structures. Validation of the hypothesized structures was performed by the calculation of key fragmentation pathway energies using density functional theory (DFT) calculations (B3LYP/6-31 G (d,p)). RESULTS: The photoproducts were identified as 2-aminoquinoxaline, SQX isomers, 2-(N-parabenzoquinoneimine)quinoxaline and isomers resulting from SO(2) extrusion. The direct fragmentations of [SQX + H](+) and its protonated isomers mostly occurred through the loss of 2-aminoquinoxaline and/or the 4-sulfoaniline radical ion, while their rearrangements involved the migration of H and/or O atoms. For the desulfonated byproducts in their protonated forms, the main neutral losses were of the quinoxaline radical, aminoquinoxaline and NH(3). The fragmentation of the protonated 2-aminoquinoxaline mainly involved the elimination of NH(3) and HCN. CONCLUSIONS: LC/ESI-Q-TOFMS and DFT calculations have been shown to be useful and complementary methods for the identification of unknown isomeric compounds and the elucidation of fragmentation patterns, in the case of the sulfaquinoxaline veterinary antibiotic.


Asunto(s)
Cromatografía Liquida/métodos , Espectrometría de Masa por Ionización de Electrospray/métodos , Sulfaquinoxalina/análogos & derivados , Sulfaquinoxalina/química , Luz Solar , Agua/química , Isomerismo , Procesos Fotoquímicos , Quinoxalinas/química , Sulfaquinoxalina/análisis , Sulfaquinoxalina/efectos de la radiación , Espectrometría de Masas en Tándem
10.
J Agric Food Chem ; 60(7): 1613-8, 2012 Feb 22.
Artículo en Inglés | MEDLINE | ID: mdl-22277081

RESUMEN

A new, rapid, and sensitive method was proposed for the determination of sulfonamide residues in milk and chicken muscle samples by microchip electrophoresis with laser-induced fluorescence detection. Separation of fluorescamine-labeled sulfonamides was accomplished by using a buffer containing 5 mmol/L boric acid and 1% (w/v) polyvinyl alcohol (PVA). The pH, amount of PVA, and concentration of boric acid in the running buffer were found to have great influence on the separation. By optimizing these conditions, the separation of four sulfonamides, sulfamethazine, sulfamethoxazole, sulfaquinoxaline, and sulfanilamide, was achieved within 1 min with limits of detection (S/N = 3) of 0.2-2.3 µg/L, which are well below the maximum residue limit. The proposed method also exhibited very good repeatability; the relative standard deviations for both within-day and between-day measurements were ≤3.0%. With a simplified sample pretreatment protocol, fast determination of sulfonamides in real samples was successfully performed with standard addition recoveries of 93.3-100.8 and 82.9-92.3%, respectively.


Asunto(s)
Pollos , Electroforesis por Microchip , Leche/química , Músculo Esquelético/química , Sulfonamidas/análisis , Animales , Antibacterianos/análisis , Concentración de Iones de Hidrógeno , Reproducibilidad de los Resultados , Sulfametazina/análisis , Sulfametoxazol/análisis , Sulfanilamida , Sulfanilamidas/análisis , Sulfaquinoxalina/análisis
11.
Br Poult Sci ; 52(3): 376-80, 2011 Jun 01.
Artículo en Inglés | MEDLINE | ID: mdl-21732884

RESUMEN

1. A physiologically-based pharmacokinetic model was developed for the purpose of describing the relationship between plasma concentration of drugs and their deposition into eggs. 2. By incorporating the physiology of egg formation into the model, the transfer of drugs into the egg albumen and yolk could be described using rate constants. 3. The model was used to describe concentrations in albumen and yolk of sulphanilamide, sulphaquinoxaline and pyrimethamine as a function of time using datasets from the literature. 4. The model could be used as a tool to obtain an insight into those properties of a drug which are responsible for the amount of residue in eggs, and could help in the design of critical studies for determining withdrawal periods for eggs.


Asunto(s)
Aves de Corral/metabolismo , Pirimetamina/farmacocinética , Sulfanilamidas/farmacocinética , Sulfaquinoxalina/farmacocinética , Animales , Clara de Huevo/química , Yema de Huevo/química , Huevos , Cinética , Modelos Biológicos , Pirimetamina/análisis , Sulfanilamida , Sulfanilamidas/análisis , Sulfaquinoxalina/análisis
12.
Environ Toxicol Chem ; 30(6): 1252-60, 2011 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-21351294

RESUMEN

The presence of antibiotics in the environment is of great concern because of their potential for resistance selection among pathogens. In the present study we investigated the occurrence of 19 sulfonamides, five N-acetylated sulfonamide metabolites, and trimethoprim in the Liao River basin and adjacent Liaodong Bay, China, as well as 10 human/agricultural source samples. Within the 35 river samples, 12 sulfonamides, four acetylated sulfonamides, and trimethoprim were detected, with the dominant being sulfamethoxazole (66.6 ng/L), N-acetylsulfamethoxazole (63.1 ng/L), trimethoprim (29.0 ng/L), sulfadiazine (14.0 ng/L), and sulfamonomethoxine (8.4 ng/L); within the 36 marine samples, 10 chemicals were detected, with the main contributions from sulfamethoxazole (25.2 ng/L) and N-acetylsulfamethoxazole (28.6 ng/L). Sulfamethoxazole (25.9%), N-acetylsulfamethoxazole (46.6%), trimethoprim (22.9%), and sulfapyridine (1.4%) were the main chemicals from human sources, while sulfamonomethoxine, sulfamethazine, sulfaquinoxaline, sulfaguanidine, sulfadiazine, sulfanilamide, and sulfamethoxypyridazine were dominant in the animal husbandry sources, specifically, swine and poultry farms, and sulfamethoxazole (91%) was dominant in the mariculture source. A principal component analysis with multiple linear regression was performed to evaluate the source apportionment of total sulfonamides in Liaodong Bay. It was found that animal husbandry contributed 15.2% of total sulfonamides, while human sources contributed 28.5%, and combined human and mariculture sources contributed 56.3%. In addition, the mariculture contribution was 24.1% of total sulfonamides into the sea based on mass flux estimation. The present study is the first report that the environmental levels of sulfonamide metabolites were comparable to the corresponding parents; therefore, we should pay attention to their environmental occurrence. Source apportionment showed human discharge (60.7%) significantly contributed to these antibiotics in Liaodong Bay, which provides important information for environmental management.


Asunto(s)
Antibacterianos/análisis , Ríos/química , Sulfonamidas/análisis , Contaminantes Químicos del Agua/análisis , Agricultura , Acuicultura , China , Monitoreo del Ambiente , Humanos , Modelos Lineales , Análisis de Componente Principal , Agua de Mar/química , Espectrometría de Masa por Ionización de Electrospray , Sulfametazina/análisis , Sulfametoxazol/análisis , Sulfametoxipiridazina/análisis , Sulfamonometoxina/análisis , Sulfapiridina/análisis , Sulfaquinoxalina/análisis , Espectrometría de Masas en Tándem , Trimetoprim/análisis , Contaminación Química del Agua/estadística & datos numéricos
13.
Anal Chem ; 82(18): 7550-5, 2010 Sep 15.
Artículo en Inglés | MEDLINE | ID: mdl-20726505

RESUMEN

A rapid and sensitive immunochromatographic assay (ICA) based on competitive format was developed and validated for simultaneous detection of sulfamethazine (SM(2)), sulfadiazine (SDZ), and sulfaquinoxaline (SQX) in chicken breast muscle and egg samples. For this purpose, three monoclonal antibodies raised against those three sulfonamides were conjugated to colloidal gold particles and applied to the conjugate pads of the test strip. The competitors of the sulfonamides (SM(2)/SDZ/SQX-bovine serum albumin conjugates) were immobilized onto a nitrocellulose membrane at three detection zones to form T(1), T(2), and T(3), respectively. With this method, the cutoff values for the three test lines were achieved at 80 µg/kg, which is lower than the maximum residue levels (MRLs) established for sulfonamides. The recoveries in negative samples spiked at concentrations of 10, 50, and 100 µg/kg ranged from 75% to 82% for egg samples and from 78% to 81% for chicken samples. The method was compared with the HPLC method by testing 180 eggs and chicken breast samples from local markets, and an agreement rate of 99.7% was obtained between the two methods.


Asunto(s)
Anticuerpos Monoclonales/inmunología , Cromatografía/métodos , Residuos de Medicamentos/análisis , Contaminación de Alimentos/análisis , Inmunoensayo/métodos , Músculos/química , Óvulo/química , Métodos Analíticos de la Preparación de la Muestra , Animales , Bovinos , Pollos , Cromatografía Líquida de Alta Presión , Oro Coloide/química , Carne/análisis , Sulfadiazina/análisis , Sulfadiazina/inmunología , Sulfametazina/análisis , Sulfametazina/inmunología , Sulfaquinoxalina/análisis , Sulfaquinoxalina/inmunología , Factores de Tiempo
14.
Se Pu ; 25(2): 238-40, 2007 Mar.
Artículo en Chino | MEDLINE | ID: mdl-17580695

RESUMEN

A method for the determination of 12 sulfonamides (SAs) (sulfanilamide, sulfamonomethoxine, sulfacetamide, sulfamethoxazole, sulfadiazine, sulfisoxazole, sulfathiazole, sulfadi-methoxine, sulfamerazine, sulfaquinoxaline, sulfamethazine, sulfanitran) in cosmetics was developed by ultra performance liquid chromatography with photodiode array detector (UPLC-PDA). The chromatographic column used was Acquity UPLC BEHC C18 (50 mm x 2. 1 mm, 1. 7 microm) and the mobile phase was acetonitrile-0. 1% formic acid aqueous solution. A gradient elution program was utilized for the separation and determination. After liquid-liquid extraction, SAs were separated and detected by UPLC-PDA. The qualification analysis was done by using retention time and spectrum, and the quantification was based on the detection wavelength of 268 nm. The limits of qualification (S/N = 3) and quantification (S/N = 10) for 12 SAs were 1 microg/g and 2 -3 microg/g, respectively. The correlation coefficient of linear calibration curve was over 0. 999 7 within the SAs concentration range of 1 - 25 mg/L (except sulfanitran 0. 5 - 12. 5 mg/L). At the spiked levels of 40 and 8 microg (except sulfanitran 20 and 4 microg), the average recoveries for 12 SAs were 86. 8% - 98. 1% and 80. 1% - 96. 9%, respectively. Relative standard deviations were less than 10%. Routine tests show that the method is simple, fast, and has a good separation efficiency. It can be routinely used for the determination of these SAs in cosmetics.


Asunto(s)
Cromatografía Liquida/métodos , Sulfonamidas/análisis , Cosméticos/análisis , Reproducibilidad de los Resultados , Sulfacetamida/análisis , Sulfadiazina/análisis , Sulfamerazina/análisis , Sulfametazina/análisis , Sulfametoxazol/análisis , Sulfamonometoxina/análisis , Sulfanilamida , Sulfanilamidas/análisis , Sulfaquinoxalina/análisis , Sulfatiazol , Sulfatiazoles/análisis , Sulfisoxazol/análisis
15.
Se Pu ; 23(4): 397-400, 2005 Jul.
Artículo en Chino | MEDLINE | ID: mdl-16250451

RESUMEN

The presence of sulfonamide (SA) residues in foods is largely due to the raising of animals with sulfonamide antibiotics added or polluted feedstuff. Because of interference from the matrices, the commonly used immunoassay or chromatographic method is not suitable for the analysis of multi-SAs in feedstuff. A high performance liquid chromatographic-electrospray tandem mass spectrometric (HPLC/ESI-MS-MS) method has been established for the simultaneous determination of multi-SAs including sulfadiazine (SD), sulfapyridine (SPD), sulfamerazine (SM1), sulfameter (SM), sulfamethazine (SM2), sulfamethoxypyridazine (SMP), sulfamethoxazole (SMZ), sulfamonomethoxine (SMM), sulfadimethoxine (SDM) and sulfaquinoxaline (SQX). After solvent extraction, solid phase extraction, dilution and reversed-phase HPLC separation, SAs were detected by ESI-MS-MS under multi-reaction monitoring mode. The qualification analysis was done by using retention time and distribution of diagnostic ion pairs, and the quantification was based on the peak intensity of common fragment ion m/z 156. The limits of quantification for 10 SAs were 0.5 - 2.0 microg/kg (S/N = 10). The correlation coefficient of linear calibration curve was over 0.9995 within the SAs concentration range 2.0 - 200 microg/L except for SDM and SQX. At the spiked level of 1.0 mg/kg, the average recoveries for the 10 SAs were between 70% and 92%, the relative standard deviations were under 10% for intra-day and under 15% for inter-day. Routine tests showed the method was fast, sensitive, specific, and practical for the SAs determination in feedstuff.


Asunto(s)
Alimentación Animal/análisis , Cromatografía Líquida de Alta Presión/métodos , Sulfonamidas/análisis , Sulfonamidas/química , Espectrometría de Masas en Tándem/métodos , Animales , Espectrometría de Masa por Ionización de Electrospray , Sulfadimetoxina/análisis , Sulfadimetoxina/química , Sulfameter/análisis , Sulfameter/química , Sulfametazina/análisis , Sulfametazina/química , Sulfametoxazol/análisis , Sulfametoxazol/química , Sulfametoxipiridazina/análisis , Sulfametoxipiridazina/química , Sulfamonometoxina/análisis , Sulfamonometoxina/química , Sulfapiridina/análisis , Sulfapiridina/química , Sulfaquinoxalina/análisis , Sulfaquinoxalina/química
16.
Se Pu ; 23(6): 636-8, 2005 Nov.
Artículo en Chino | MEDLINE | ID: mdl-16498995

RESUMEN

A method was developed for determining residual sulfonamides (SAs) such as sulfamethazine (SM2), sulfamonomethoxine (SMM), sulfamethiazole (SMZ), sulfadimethoxine (SDM) and sulfaquinoxaline (SQ) in pork and chicken using solid-phase extraction (SPE) and high performance liquid chromatography (HPLC) with a photodiode array detector. The samples were extracted with ethyl acetate. An NH2 column was used for clean up. For the HPLC determination, an Intersil ODS-2 column was used with a mixture of methanol-acetonitrile-water-acetic acid (2: 2: 9: 0.2, v/v) as the mobile phase. The detection limits (S/N = 3) were 3 microg/kg for SM2, SMM and SMZ, and 7 microg/kg for SDM and SQ. The quantitation limits (S/N = 10) were 10 microg/kg for SM2, SMM and SMZ, and 25 microg/kg for SDM and SQ. The linear ranges were 30 - 5 000 microg/L for SM2, SMM and SMZ, and 60 - 5 000 microg/L for SDM and SQ. The recoveries were between 73.2% and 97.3% with the relative standard deviations between 2.5% and 11.6% originated from the spiked level of 50 microg/kg.


Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Carne/análisis , Extracción en Fase Sólida/métodos , Sulfonamidas/análisis , Animales , Pollos , Reproducibilidad de los Resultados , Sulfadimetoxina/análisis , Sulfadimetoxina/química , Sulfametazina/análisis , Sulfametazina/química , Sulfametizol/análisis , Sulfametizol/química , Sulfamonometoxina/análisis , Sulfamonometoxina/química , Sulfaquinoxalina/análisis , Sulfaquinoxalina/química , Sulfonamidas/química , Porcinos
17.
J AOAC Int ; 85(4): 848-52, 2002.
Artículo en Inglés | MEDLINE | ID: mdl-12180677

RESUMEN

A method was developed for determining residual sulfonamide antibacterials such as sulfamethazine (SMZ), sulfamonomethoxine (SMM), sulfadimethoxine (SDM), and sulfaquinoxaline (SQ) in eggs using liquid chromatography with a photodiode array detector. The spiked and blank samples were cleaned up by using an Ultrafree-MC/PL centrifugal ultrafiltration unit. A Mightysil RP-4 GP column and a mobile phase of 28% (v/v) ethanol-H2O with a photodiode array detector were used for the determination. Average recoveries from eggs spiked with each drug at 0.1, 0.2, 0.4, and 1.0 ppm were > or = 80.9%, with relative standard deviations between 1.3 and 4.7%. The limits of quantitation were 0.060 ppm for SMZ, 0.045 for SMM, 0.044 for SDM, and 0.093 for SQ. The analysis of one sample required < 30 min and < 5 mL ethanol as solvent.


Asunto(s)
Antiinfecciosos/análisis , Cromatografía Liquida/métodos , Huevos/análisis , Contaminación de Alimentos/análisis , Sulfonamidas/análisis , Animales , Pollos , Solventes , Sulfadimetoxina/análisis , Sulfametazina/análisis , Sulfamonometoxina/análisis , Sulfaquinoxalina/análisis
18.
J Chromatogr A ; 870(1-2): 169-77, 2000 Feb 18.
Artículo en Inglés | MEDLINE | ID: mdl-10722074

RESUMEN

A liquid chromatography method is described to determine sulfaquinoxaline (SQX), sulfamethazine (SMT), and pyrimethamine (PMT), by using a Kromasil C18 column and a 40 mM NaH2PO4 buffer solution, containing 10 mM NaClO4 (pH 3.0)-acetonitrile (65:35) as mobile phase. The mobile phase flow-rate and sample volume injected were 1.5 ml/min and 20 microl, respectively and the samples were dissolved in the mobile phase. The limits of quantification were found to be about 180 microg/l (3.6 ng) for each compound. The method was applied in veterinary commercial formulations. Analyses were made by means of the standard addition method, whose results were compared with those obtained by preparing "tests" (from the stock solutions) and with those obtained by a capillary electrophoresis method. Both methods showed similar results, and then it was proved that some commercial claimed levels were not in agreement with the obtained results by using our analytical method, as they were in other cases.


Asunto(s)
Antiinfecciosos/análisis , Cromatografía Liquida/métodos , Pirimetamina/análisis , Sulfametazina/análisis , Sulfaquinoxalina/análisis , Calibración , Reproducibilidad de los Resultados , Sensibilidad y Especificidad
19.
J Chromatogr B Biomed Sci Appl ; 715(2): 431-5, 1998 Sep 18.
Artículo en Inglés | MEDLINE | ID: mdl-9792530

RESUMEN

A supercritical fluid extraction (SFE) method is proposed for the recovery of three sulfonamides from chicken liver. Samples were extracted at 680 bar and 40 degrees C using unmodified carbon dioxide and were collected free of co-extracted artifactual material on an in-line neutral alumina sorbent bed. High recoveries of sulfamethazine (SMZ), sulfadimethoxine (SDM) and sulfaquinoxaline (SQX) were obtained from chicken liver samples fortified at levels from 1000 to 50 ppm.


Asunto(s)
Cromatografía/métodos , Hígado/química , Sulfadimetoxina/análisis , Sulfametazina/análisis , Sulfaquinoxalina/análisis , Animales , Pollos , Sensibilidad y Especificidad , Espectrofotometría Ultravioleta
20.
Zentralbl Veterinarmed A ; 45(4): 225-8, 1998 May.
Artículo en Inglés | MEDLINE | ID: mdl-9697423

RESUMEN

Sulphaquinoxaline (SQ) was fed to laying hens at the dietary levels of 25, 50, 100 and 200 ppm, respectively, for 7 successive days. The increasing amount of SQ transferred into the whole egg during SQ feeding could be well described by the following equation: [equation: see text] where y is the SQ content (ppm) in the whole egg, x is the dietary SQ level (ppm), T is days on SQ feeding (T < or = 4). After 4 days of SQ feeding, the SQ content in the homogenized eggs reached a plateau at 0.0292.x (= 0.007318.4x) ppm. This equation permits to predict SQ content in the eggs.


Asunto(s)
Antiprotozoarios/farmacocinética , Pollos/metabolismo , Residuos de Medicamentos/análisis , Huevos/análisis , Sulfaquinoxalina/farmacocinética , Administración Oral , Animales , Antiprotozoarios/administración & dosificación , Antiprotozoarios/análisis , Dieta/veterinaria , Femenino , Sulfaquinoxalina/administración & dosificación , Sulfaquinoxalina/análisis
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