title: Ultrasound-assisted extraction and solid-phase extraction for the simultaneous determination of five amide herbicides in fish samples by gas chromatography with electron capture detection.
abstract: An efficient sample extraction and clean-up method was developed for simultaneous determination of five amide herbicides (alachlor, acetochlor, propisochlor, metazachlor, and butachlor) in fish samples. The protocol consisted of ultrasound-assisted solvent extraction and solid-phase extraction clean-up. In detail, aliquots of homogenized fish flesh were thoroughly mixed with 20 mL of n-hexane and then extracted with ultrasonication for 40 min. Each sample was centrifuged and the supernatant was collected for the subsequent clean-up. For the sample preparation, the above supernatant was processed with a C18column with 3 mL of dichloromethane/n-hexane (1:1, v/v) as the eluant. Then the samples were analyzed by gas chromatography with electron capture detection. The correlation coefficients of the five calibration curves were 0.9976-0.9998 (n = 3). The limits of detection (S/N = 3, n = 11) and limits of quantification (S/N = 10, n = 11) were 0.19-0.42 and 0.63-1.39 μg/kg, respectively. The recoveries of this method were 71.2-92.6% with good precision (<4.7% relative standard deviations, n = 6). The developed method was successfully applied to monitor the five amide herbicides in fish samples collected from different cities.
authors.affiliation: College of Chemistry and Chemical Engineering, Central South University, Changsha, Hunan, P.R. China.
authors.forename: Zhipeng
authors.initials: Z
authors.lastname: Qu
authors.affiliation: College of Chemistry and Chemical Engineering, Central South University, Changsha, Hunan, P.R. China.
authors.forename: Xiuzhi
authors.initials: X
authors.lastname: Bai
authors.affiliation: College of Chemistry and Chemical Engineering, Central South University, Changsha, Hunan, P.R. China.
authors.forename: Ting
authors.initials: T
authors.lastname: Zhang
authors.affiliation: College of Chemistry and Chemical Engineering, Central South University, Changsha, Hunan, P.R. China.|Center for Environment and Water Resources, Central South University, Changsha, Hunan, P.R. China.
authors.forename: Zhaoguang
authors.initials: Z
authors.lastname: Yang
mesh_terms: D000818:Animals; D002849:Chromatography, Gas; D004583:Electrons; D005399:Fishes; D005506:Food Contamination / Q000032:analysis*; D006540:Herbicides / Q000302:isolation & purification*; D017747:Seafood / Q000032:analysis*; D052616:Solid Phase Extraction
chemical_list: D006540:Herbicides
keywords: amide herbicides; fish sample; gas chromatography; solid-phase extraction; ultrasound-assisted extraction