title: Assessment of dispersive liquid-liquid microextraction conditions for gas chromatography time-of-flight mass spectrometry identification of organic compounds in honey.
abstract: The suitability of the dispersive liquid-liquid microextraction (DLLME) technique for gas chromatography (GC) characterization of minor organic compounds in honey samples is evaluated. Under optimized conditions, samples were pre-treated by liquid-liquid extraction with acetonitrile followed by DLLME using carbon tetrachloride (CCl4, 0.075 mL) as extractant. The yielded settled phase was analyzed by GC using high resolution time-of-flight (TOF) mass spectrometry (MS). The whole sample preparation process is completed in approximately 10 min, with a total consumption of organic solvents below 4 mL, relative standard deviations lower than 12% and with more than 70 organic compounds, displaying linear retention index in the range from 990 to 2900, identified in the obtained extracts. In comparison with HS SPME extraction, higher peak intensities were attained for most volatile and semi-volatile compounds amenable to both extraction techniques. Furthermore, other species such as highly polar and water soluble benzene acids, long chain fatty acids, esters and flavonoids, which are difficult to concentrate by HS SPME, could be identified in DLLME extracts. Some of the compounds identified in DLLME extracts have been proposed as useful for samples classification and/or they are recognized as markers of honeys from certain geographic areas.
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain; Department of Pharmacology, School of Medical Sciences, Universiti Sains Malaysia, Kubang Kerian, Kelantan, 16150 Malaysia.
authors.forename: M
authors.initials: M
authors.lastname: Moniruzzaman
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain. Electronic address: isaac.rodriguez@usc.es.
authors.forename: I
authors.initials: I
authors.lastname: Rodríguez
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
authors.forename: T
authors.initials: T
authors.lastname: Rodríguez-Cabo
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
authors.forename: R
authors.initials: R
authors.lastname: Cela
authors.affiliation: Department of Pharmacology, School of Medical Sciences, Universiti Sains Malaysia, Kubang Kerian, Kelantan, 16150 Malaysia.
authors.forename: S A
authors.initials: SA
authors.lastname: Sulaiman
authors.affiliation: Human Genome Centre, School of Medical Sciences, Universiti Sains Malaysia, Kubang Kerian, Kelantan, 16150 Malaysia.
authors.forename: S H
authors.initials: SH
authors.lastname: Gan
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006722:Honey / Q000032:analysis*; D006863:Hydrogen-Ion Concentration; D059627:Liquid Phase Microextraction / Q000379:methods*; D009930:Organic Chemicals / Q000032:analysis*; D052617:Solid Phase Microextraction; D012997:Solvents / Q000737:chemistry
chemical_list: D009930:Organic Chemicals; D012997:Solvents
keywords: Dispersive liquid–liquid microextraction; Gas chromatography time-of-flight mass spectrometry; Honey organic compounds identification