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1.
Biomed Chromatogr ; 21(9): 925-30, 2007 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-17428019

RESUMO

This paper reports a rapid and sensitive method for determination of the anti-inflammatory compound vicenin-2 in L. ericoides Mart. using liquid chromatography-tandem mass spectrometry. Separation of the compound of interest was performed on a VP-ODS(18) (150 x 2 mm, Shimadzu, Japan) column and a pre-column packed with GPV-ODS C(18) (5 x 2 mm, Sigma-Aldrich, USA) with acetonitrile-water (15:85) mobile phase containing 2% acetic acid using isocratic flow at 0.5 mL/min for 2 min. Multiple-reaction monitoring of vicenin-2 was performed using electrospray positive ionization. The linear calibration curves were generated using a concentration range of 5-2500 ng/mL with correlation coefficients >0.99. The values of limit of detection and limit of quantitation were found to be 1 and 5 ng/mL, respectively. The method developed based on LC-ESIMS/MS is advantageous because it permits the rapid and selective detection of vicenin-2. Furthermore, the method can be easily applied to the routine analysis of vicenin-2 in plant extracts using a minimal amount of sample.


Assuntos
Anti-Inflamatórios/análise , Apigenina/análise , Asteraceae/química , Cromatografia Líquida/métodos , Glucosídeos/análise , Folhas de Planta/química , Espectrometria de Massas em Tandem/métodos , Extratos Vegetais/química , Sensibilidade e Especificidade , Espectrometria de Massas por Ionização por Electrospray/métodos
2.
J Environ Sci Health B ; 38(5): 605-15, 2003 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-12929719

RESUMO

The possibility of applying thin layer chromatography (TLC) detection for the analysis of pesticide residues in tomatoes was investigated. Samples of tomatoes that have never been treated with pesticide were fortified with atrazine, carbaryl, carbofuran, chloroxuron, diuron, dimethoate, imazalil, oxamyl and methamidophos. The samples were extracted, cleaned-up by gel permeation chromatography and then applied on silica gel plates. The pesticides were eluted with ethyl acetate and dichloromethane. Two eluting solvent systems were tested, one using the reagents o-toluidine + potassium iodite (o-TKI) and the other p- nitrobenzene fluoroborate (NBFB). After the development of the plates, the diameter of the spots was measured. The lowest minimum detection quantity (MDQ) for o-TKI system for atrazine was 12 ng. The highest was 125 ng for carbofuran. Using NBFB system, the lowest MDQ was 60 ng for carbaryl and the highest was 70 ng obtained for carbofuran. Considering the concentration of these pesticides in the spiked tomato samples, the minimum concentration was 1.1 ng/microL and 32.3 ng/microL for atrazine and carbofuran, respectively, by using o-TKI system. For NBFB system the minimum concentration reached was 3.5 ng/microL and 4.3 ng/microL for carbaryl and carbofuran, respectively. This study showed that TLC can be used for semi-quantitative analysis.


Assuntos
Cromatografia em Camada Fina/métodos , Contaminação de Alimentos/análise , Resíduos de Praguicidas/análise , Solanum lycopersicum/química , Calibragem , Cromatografia em Gel/métodos , Sensibilidade e Especificidade , Solventes
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