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1.
Artículo en Inglés | MEDLINE | ID: mdl-33059159

RESUMEN

In this research study, a method of dispersive-micro-solid phase extraction (D-µ-SPE) combined with molecularly imprinted polymer nanoparticles (MIP-NPs) with HPLC-UV was developed for the fast and selective detection of the trace amount of albendazole sulfoxide (ABZSO) in the biological samples. To investigate the effective factors on ABZSO microextraction by the method, central composite design (CCD) was utilized, and the optimum conditions for ABZSO microextraction were sample pH of 8.0, MIP-mass of 15 mg, sonication time of 12 min, and eluent (methanol) volume of 0.25 mL. Under the obtained optimal extraction conditions, the value for the limit of detection (LOD) and limit of quantification (LOQ) was respectively showed to be 0.074 and 0.246 ng mL-1. In addition, the calculated peak areas exhibited a linear relationship with the ABZSO concentration ranging from 0.4 to 4200 ng mL-1. The analyses of the samples including human plasma and urine, and water were successfully performed by the usage of the D-µ-SPE method, which was a simple and sensitive technique and a suitable alternative for the analysis of ABZSO. In the analysis of ABZSO in various samples, the recoveries at various levels of ABZSO concentrations (50, 300, and 500 ng mL-1) were in the range of 95.7-103.0 %, and the relative standard deviations (RSDs; n = 3) varied from 2.2 to 4.4%.


Asunto(s)
Albendazol/análogos & derivados , Cromatografía Líquida de Alta Presión/métodos , Impresión Molecular/métodos , Microextracción en Fase Sólida/métodos , Albendazol/análisis , Albendazol/química , Albendazol/aislamiento & purificación , Humanos , Límite de Detección , Modelos Lineales , Polímeros Impresos Molecularmente/química , Nanopartículas/química , Reproducibilidad de los Resultados , Agua/química
2.
Food Chem ; 269: 442-449, 2018 Dec 15.
Artículo en Inglés | MEDLINE | ID: mdl-30100458

RESUMEN

A liquid chromatography-tandem mass spectrometry quantitative method was developed for determining mebendazole and its metabolites, albendazole and its metabolites, and levamisole in muscles of bluntnose black bream, shrimp, eel and turtle based on modified QuEChERS methodology. The method included 2 g of the muscle matrix with 10 mL acetonitrile, and 0.8 g of magnesium sulphate and 0.2 g of sodium chloride for liquid-liquid partitioning. After vortex and centrifugation, the resulting liquid (5.5 mL) was purified by C18 (50 mg) and Al-N (50 mg). The limits of detection were lower than 0.3 µg kg-1 and the limits of quantitation were no more than 1 µg kg-1 for all analytes. The recoveries of the analytes ranged from 80.0% to 113.7% with the relative standard derivation less than 10.0%. The preparation procedure provided efficient extraction and purification that enabled a sensitive and rugged determination of target compounds.


Asunto(s)
Albendazol/aislamiento & purificación , Levamisol/aislamiento & purificación , Mebendazol/aislamiento & purificación , Alimentos Marinos/análisis , Espectrometría de Masas en Tándem/métodos , Animales , Cromatografía Líquida de Alta Presión , Cromatografía Liquida/métodos , Límite de Detección , Residuos de Plaguicidas/análisis , Residuos de Plaguicidas/aislamiento & purificación , Extracción en Fase Sólida
3.
Anal Chim Acta ; 932: 22-8, 2016 Aug 17.
Artículo en Inglés | MEDLINE | ID: mdl-27286766

RESUMEN

A syringe to syringe dispersive liquid phase microextraction-solidified floating organic drop was introduced and used for the simultaneous extraction of trace amounts of albendazole and triclabendazole from different matrices. The extracted analytes were determined by high performance liquid chromatography along with fluorescence detection. The analytical parameters affecting the microextraction efficiency including the nature and volume of the extraction solvent, sample volume, sample pH, ionic strength and the cycles of extraction were optimized. The calibration curves were linear in the range of 0.1-30.0 µg L(-1) and 0.2-30.0 µg L(-1) with determination coefficients of 0.9999 and 0.9998 for albendazole and triclabendazole respectively. The detection limits defined as three folds of the signal to noise ratio were found to be 0.02 µg L(-1) for albendazole and 0.06 µg L(-1) for triclabendazole. The inter-day and intra-day precision (RSD%) for both analytes at three concentration levels (0.5, 2.0 and 10.0 µg L(-1)) were in the range of 6.3-10.1% and 5.0-7.5% respectively. The developed method was successfully applied to determine albendazole and triclabendazole in water, cow milk, honey, and urine samples.


Asunto(s)
Albendazol/análisis , Albendazol/aislamiento & purificación , Bencimidazoles/análisis , Bencimidazoles/aislamiento & purificación , Microextracción en Fase Líquida/instrumentación , Jeringas , Cromatografía Líquida de Alta Presión , Concentración de Iones de Hidrógeno , Límite de Detección , Concentración Osmolar , Solventes/química , Factores de Tiempo , Triclabendazol
4.
PLoS One ; 9(9): e105637, 2014.
Artículo en Inglés | MEDLINE | ID: mdl-25255321

RESUMEN

Albendazole is a broad-spectrum parasiticide with high effectiveness and low host toxicity. No method is currently available for measuring albendazole and its metabolites in silkworm hemolymph. This study describes a rapid, selective, sensitive, synchronous and reliable detection method for albendazole and its metabolites in silkworm hemolymph using ultrafast liquid chromatography tandem triple quadrupole mass spectrometry (UFLC-MS/MS). The method is liquid-liquid extraction followed by UFLC separation and quantification in an MS/MS system with positive electrospray ionization in multiple reaction monitoring mode. Precursor-to-product ion transitions were monitored at 266.100 to 234.100 for albendazole (ABZ), 282.200 to 208.100 for albendazole sulfoxide (ABZSO), 298.200 to 159.100 for albendazole sulfone (ABZSO2) and 240.200 to 133.100 for albendazole amino sulfone (ABZSO2-NH2). Calibration curves had good linearities with R2 of 0.9905-0.9972. Limits of quantitation (LOQs) were 1.32 ng/mL for ABZ, 16.67 ng/mL for ABZSO, 0.76 ng/mL for ABZSO2 and 5.94 ng/mL for ABZSO2-NH2. Recoveries were 93.12%-103.83% for ABZ, 66.51%-108.51% for ABZSO, 96.85%-105.6% for ABZSO2 and 96.46%-106.14% for ABZSO2-NH2, (RSDs <8%). Accuracy, precision and stability tests showed acceptable variation in quality control (QC) samples. This analytical method successfully determined albendazole and its metabolites in silkworm hemolymph in a pharmacokinetic study. The results of single-dose treatment suggested that the concentrations of ABZ, ABZSO and ABZSO2 increased and then fell, while ABZSO2-NH2 level was low without obvious change. Different trends were observed for multi-dose treatment, with concentrations of ABZSO and ABZSO2 rising over time.


Asunto(s)
Albendazol/metabolismo , Antiparasitarios/metabolismo , Bombyx/metabolismo , Cromatografía Líquida de Alta Presión/métodos , Hemolinfa/metabolismo , Espectrometría de Masas en Tándem/métodos , Albendazol/análogos & derivados , Albendazol/aislamiento & purificación , Albendazol/farmacocinética , Métodos Analíticos de la Preparación de la Muestra , Animales , Antiparasitarios/aislamiento & purificación , Antiparasitarios/farmacocinética , Estabilidad de Medicamentos , Estudios de Factibilidad , Congelación , Límite de Detección , Modelos Lineales , Extracción Líquido-Líquido , Factores de Tiempo
5.
J Chromatogr A ; 1230: 61-5, 2012 Mar 23.
Artículo en Inglés | MEDLINE | ID: mdl-22341660

RESUMEN

The enantiomeric separation of albendazole sulfoxide was carried out by simulated moving bed chromatography with variable zones (VARICOL). An overall recovery of 97% was achieved and enantiomeric ratios of 99.5% for raffinate and 99.0% for extract were attained. A total of 880 mg of (+)-albendazol sulfoxide and 930 mg of its antipode were collected after 55 cycles or 11 h of process, resulting in a mass rate of 2 g/day. Furthermore the absolute configuration of the enantiopure compounds was determined for the first time by vibrational circular dichroism (VCD) with the aid of theoretical calculations as (-)-(S) and (+)-(R)-albendazole sulfoxide.


Asunto(s)
Albendazol/análogos & derivados , Cromatografía/métodos , Albendazol/química , Albendazol/aislamiento & purificación , Dicroismo Circular , Conformación Molecular , Estereoisomerismo
6.
Talanta ; 76(1): 146-53, 2008 Jun 30.
Artículo en Inglés | MEDLINE | ID: mdl-18585256

RESUMEN

The development and validation of a fully automated achiral-chiral high performance liquid chromatography (HPLC) method for the simultaneous determination of albendazole metabolites: enantiomers of albendazole sulphoxide (ABZ-SO), albendazole sulphone (ABZ-SO(2)) and albendazole 2-aminosulphone (ABZ-SO(2)NH(2)) in bovine plasma are described. This method involves an octyl restricted access media bovine serum albumin column (C(8)-RAM-BSA) (50 mm x 4.6 mm I.D.) for sample clean-up, followed by enantioselective analysis on a column containing an amylose tris(3,5-dimethylphenylcarbamate) stationary phase (150 mm x 4.6 mm I.D.). The chromatographic separations of all target compounds were performed at 30 degrees C using a mobile phase composed of phosphate buffer (10 mmol L(-1); pH 7.5):acetonitrile (60:40, v/v), flow rate of 0.5 mL min(-1) and fluorescence detection at 290 nm and 320 nm, excitation and emission, respectively. The influence of different organic modifiers and chiral selector of the stationary phase on enantioseparation of ABZ-SO was investigated. The method developed was fully validated. The calibration curves were linear in the concentration range of 40.00-1280 ng mL(-1) for each albendazole sulphoxide enantiomer, 10.0-320 ng mL(-1) for albendazole sulphone and 20.0-320 ng mL(-1) for albendazole 2-aminosulphone. The inter- and intra-day precision ranged from 0.760% to 7.79% relative standard deviation (R.S.D.), and the accuracy ranged 101% from 114% of the nominal values while the transfer efficiency was in the range of 84.4-103%. The method showed good linearity, precision, accuracy, sensitivity and selectivity allowing it to be appropriate for further pharmacokinetics and metabolism studies of albendazole.


Asunto(s)
Albendazol/sangre , Albendazol/metabolismo , Cromatografía Líquida de Alta Presión/métodos , Albendazol/análogos & derivados , Albendazol/síntesis química , Albendazol/química , Albendazol/aislamiento & purificación , Animales , Bovinos , Inyecciones , Polisacáridos/química , Reproducibilidad de los Resultados , Estereoisomerismo
7.
J Biochem Biophys Methods ; 62(1): 69-79, 2005 Jan 31.
Artículo en Inglés | MEDLINE | ID: mdl-15656945

RESUMEN

Broad spectrum anthelmintic agent-albendazole sulfoxide (ABZSO) have been separated and semiprepared on amylose tris (3,5-dimethylphenylcarbamate) chiral stationary phases by HPLC using mobile phases contained with n-hexane and different alcohols. For analytical separation the influence of the nature and content of alcoholic modifiers on separation were systemically studied. Then, the analytical methods were scaled up to semipreparative loading to obtain small quantities (about 1 g) of both ABZSO enantiomers. Especially, different loading amounts were investigated for their effect on various parameters of semipreparative HPLC. In addition, optical rotation and circular dichroism (CD) of both ABZSO enantiomers collected were determined and single enantiomers were found stable in configuration for 1 year.


Asunto(s)
Albendazol/análogos & derivados , Albendazol/química , Albendazol/aislamiento & purificación , Amilosa/análogos & derivados , Amilosa/química , Cromatografía Líquida de Alta Presión/métodos , Fenilcarbamatos/química , Isomerismo , Transición de Fase
8.
J Biochem Biophys Methods ; 54(1-3): 339-45, 2002 Dec 31.
Artículo en Inglés | MEDLINE | ID: mdl-12543509

RESUMEN

The enantioseparation of albendazole sulfoxide (ABZSO) by chiral supercritical-fluid chromatography (SFC) on two columns, based on the polysaccharide derivatives Chiralpak AD and Chiralcel OD, was studied. The effect of different modifiers, methanol, ethanol, 2-propanol, and acetonitrile, was examined. The results showed that ABZSO can be separated on both columns, using an alcohol-type modifier. Using the Chiralpak AD column, the best results were obtained with 2-propanol and, in the case of the Chiralcel OD, with methanol.


Asunto(s)
Albendazol/análogos & derivados , Albendazol/aislamiento & purificación , Amilosa/análogos & derivados , Celulosa/análogos & derivados , Cromatografía con Fluido Supercrítico/métodos , Fenilcarbamatos , Acetonitrilos/química , Albendazol/análisis , Albendazol/química , Albendazol/clasificación , Alcoholes/química , Carbamatos , Control de Calidad , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Soluciones/química , Estereoisomerismo
9.
J Chromatogr ; 591(1-2): 65-73, 1992 Feb 07.
Artículo en Inglés | MEDLINE | ID: mdl-1613061

RESUMEN

Three modifications of silica-bound, cross-linked bovine serum albumin (BSA) were evaluated as chiral sorbents for use in the liquid chromatographic separation of enantiomers. Glutaraldehyde, formaldehyde and di-(N-succinimidyl) carbonate were used as bifunctional reagents for the immobilization of BSA. The sorbents all contain the same loading of BSA (14.4 +/- 0.1%, w/w) and differ only with respect to the cross-linker used for immobilization. Despite their apparent similarity, the sorbents show very different chromatographic properties, not only with respect to retention of analyte enantiomers (k' and alpha), but also with respect to column efficiency (affecting Rs values). The data obtained indicate that the chemical structure of the cross-linking reagent affects to a large extent the accessibility of important chiral binding sites. Although the data obtained are difficult to interpret in any detail, certain generalizations concerning the different behaviour of the sorbents can be made.


Asunto(s)
Cromatografía Líquida de Alta Presión/instrumentación , Albúmina Sérica Bovina/química , Estereoisomerismo , Albendazol/análogos & derivados , Albendazol/aislamiento & purificación , Antihelmínticos/aislamiento & purificación , Benzodiazepinonas/aislamiento & purificación , Reactivos de Enlaces Cruzados , Espectrofotometría Ultravioleta
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