Journal
MICROCHEMICAL JOURNAL
Volume 159, Issue -, Pages -Publisher
ELSEVIER
DOI: 10.1016/j.microc.2020.105313
Keywords
Wine; Melatonin; Microextracion; Optimization
Categories
Funding
- Fundacao de Amparo a Pesquisa do Estado da Bahia (FAPESB)
- Conselho Nacional de Desenvolvimento Cientifico e Tecnologico (CNPq)
- Coordenacao de Aperfeicoamento de Pessoal de Pessoal de Nivel Superior (CAPES)
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In the present work, a method based on the Ultrasound-dispersive liquid-liquid microextraction (US-DLLME) for the preconcentration of melatonin in Brazilian and Argentinian wine samples prior to the determination by reverse phase high performance liquid chromatography with diode array detector HPLC-DAD was developed. Sample prep optimization was carried out in two stages. First, a full factorial design was executed to evaluate the variables significance. The second step consisted of significant variables optimization (pH, extraction volume, sonication time, centrifugation time) using a Doehlert matrix to determine the critical values. Optimal USDLLME extraction conditions were as follows: pH of 4.5, sonication time of 6.8 min, centrifugation time of 2.5 min, extractor volume of 250 mu L and 5.0 mL of sample. The organic phase was retrieved with a microsyringe to a glass tube, dried and diluted with the mobile phase prior injection. The method presented a limit of detection (LOD) of 0.23 mu g L-1 and a limit of quantification (LOQ) of 0.70 mu g L-1. The precision expressed as relative standard deviation (R.S.D.) was 0.8% and 1.9% at 10.0 and 1.0 mu g L-1, respectively. Accuracy was confirmed by comparison of the results found by the proposed methods with an alternative method, and spike tests with recuperations ranging from 92 to 103%. The analyzed samples showed concentrations varying from 2.2 to 5.0 mu g L-1.
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