Determination of fluoroquinolones in cattle manure-based biogas residue by ultrasonic-enhanced microwave-assisted extraction followed by online solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry.
J Chromatogr B Analyt Technol Biomed Life Sci
; 1086: 166-175, 2018 Jun 01.
Article
em En
| MEDLINE
| ID: mdl-29680661
ABSTRACT
The present work describes the development and application of an ultrasonic-enhanced microwave-assisted extraction (UEMAE) followed by online solid phase extraction (SPE)-ultra-high performance liquid chromatography-tandem mass spectrometry method for the analysis of 14 fluoroquinolones in cattle manure-based biogas residue (CMBBR). The UEMAE was performed using the mixed solution of sodium dihydrogen phosphate and disodium ethylenediamine tetraacetic acid, avoiding use of any organic solvent. The online SPE system employed two solid phase extraction columns in a parallel manner, and the extraction was performed by passing 1â¯mL of the extract through the column. Quantification was performed using standard spiked samples and structural analogue internal standard, which were indispensable to reduce the matrix effects. Validation parameters were performed and good linearity (R2â¯>â¯0.99 in all cases) and precision (inter- and intra-day relative standard deviations were lower than 12.8%) were obtained. Limits of detection were as low as 0.021â¯ngâ¯ââ¯g-1 and lower limits of quantification were 0.5â¯ngâ¯ââ¯g-1 for all fluoroquinolones. The overall extraction recovery, which was the product of the UEMAE recovery and the online SPE recovery, was assessed for three concentration levels (0.8, 40 and 400â¯ngâ¯ââ¯g-1) and acceptable values (74.3-99.3%) were found. As a part of the method validation, the developed method has been used to analyze real CMBBR samples. Nine fluoroquinolones were found in the concentration range of 0.9-74.6â¯ngâ¯ââ¯g-1, while five were not detected in the samples. The results showed the method could be adapted for screening the presence or the final fate of fluoroquinolones during fermentation of animal waste.
Palavras-chave
Texto completo:
1
Bases de dados:
MEDLINE
Assunto principal:
Sonicação
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Cromatografia Líquida de Alta Pressão
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Fluoroquinolonas
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Biocombustíveis
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Esterco
Tipo de estudo:
Prognostic_studies
Limite:
Animals
Idioma:
En
Revista:
J Chromatogr B Analyt Technol Biomed Life Sci
Assunto da revista:
ENGENHARIA BIOMEDICA
Ano de publicação:
2018
Tipo de documento:
Article