Simultaneous derivatization and extraction of chlorophenols in water samples with up-and-down shaker-assisted dispersive liquid-liquid microextraction coupled with gas chromatography/mass spectrometric detection.
Anal Bioanal Chem
; 406(8): 2123-31, 2014 Mar.
Article
en En
| MEDLINE
| ID: mdl-23727731
ABSTRACT
A new up-and-down shaker-assisted dispersive liquid-liquid microextraction (UDSA-DLLME) for extraction and derivatization of five chlorophenols (4-chlorophenol, 4-chloro-2-methylphenol, 2,4-dichlorophenol, 2,4,6-trichloro-phenol, and pentachlorophenol) has been developed. The method requires minimal solvent usage. The relatively polar, water-soluble, and low-toxicity solvent 1-heptanol (12 µL) was selected as the extraction solvent and acetic anhydride (50 µL) as the derivatization reagent. With the use of an up-and-down shaker, the emulsification of aqueous samples was formed homogeneously and quickly. The derivatization and extraction of chlorophenols were completed simultaneously in 1 min. The common requirement of disperser solvent in DLLME could be avoided. After optimization, the linear range covered over two orders of magnitude, and the coefficient of determination (r (2)) was greater than 0.9981. The detection limit was from 0.05 to 0.2 µg L(-1), and the relative standard deviation was from 4.6 to 10.8 %. Real samples of river water and lake water had relative recoveries from 90.3 to 117.3 %. Other emulsification methods such as vortex-assisted, ultrasound-assisted, and manual shaking-enhanced ultrasound-assisted methods were also compared with the proposed UDSA-DLLME. The results revealed that UDSA-DLLME performed with higher extraction efficiency and precision compared with the other methods.
Texto completo:
1
Colección:
01-internacional
Banco de datos:
MEDLINE
Asunto principal:
Contaminantes Químicos del Agua
/
Clorofenoles
/
Microextracción en Fase Líquida
/
Cromatografía de Gases y Espectrometría de Masas
Tipo de estudio:
Diagnostic_studies
/
Evaluation_studies
Idioma:
En
Revista:
Anal Bioanal Chem
Año:
2014
Tipo del documento:
Article
País de afiliación:
Taiwán