title: Determination and surveillance of nine acaricides and one metabolite in honey by liquid chromatography-tandem mass spectrometry.
abstract: A simple and accurate analytical method for the determination of acaricides in honey was developed and validated in accordance with Japanese validation guidelines. Analytes - amitraz, N-2,4-dimethylphenyl-N-methylformamidine (DMPF), etoxazole, fenpyroximate, fipronil, hexythiazox, propargite, pyridaben and spirodiclofen - were extracted with ethyl acetate under basic conditions and subsequently cleaned up using an InertSep(®) MA-1 polymer-based anion-exchange column. The method was validated by fortified recovery tests at three different concentrations (1, 5 and 10 µg kg(-1)) performed with three samples daily on five different days. The method exhibited recoveries of 77-116% and precision (relative standard deviations - RSDs) of repeatability and within-laboratory reproducibility ranged from 2% to 22% and from 3% to 23%, respectively. The sample solution was successfully cleaned up to enable quantification using external solvent calibration curves. The limits of quantification (LOQs) were estimated to be 1 µg kg(-1) for all analytes. The method was applied to honey samples commercially available in Tokyo, Japan. Analysis of 250 honey samples indicated that amitraz was present in 127 samples, and that its residual concentration was less than 20 µg kg(-1). Propargite was detected in 23 samples at concentrations less than 1 µg kg(-1).
authors.affiliation: a Tokyo Metropolitan Institute of Public Health , Shinjuku-ku, Tokyo 169-0073 , Japan.
authors.forename: Takayuki
authors.initials: T
authors.lastname: Nakajima
authors.forename: Yumi
authors.initials: Y
authors.lastname: Tsuruoka
authors.forename: Maki
authors.initials: M
authors.lastname: Kanda
authors.forename: Hiroshi
authors.initials: H
authors.lastname: Hayashi
authors.forename: Tsuneo
authors.initials: T
authors.lastname: Hashimoto
authors.forename: Youko
authors.initials: Y
authors.lastname: Matsushima
authors.forename: Souichi
authors.initials: S
authors.lastname: Yoshikawa
authors.forename: Chieko
authors.initials: C
authors.lastname: Nagano
authors.forename: Yuki
authors.initials: Y
authors.lastname: Okutomi
authors.forename: Ichiro
authors.initials: I
authors.lastname: Takano
mesh_terms: D056810:Acaricides / Q000737:chemistry* / Q000378:metabolism; D002853:Chromatography, Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods; D006722:Honey / Q000032:analysis*; D010573:Pesticide Residues / Q000737:chemistry* / Q000378:metabolism; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D056810:Acaricides; D010573:Pesticide Residues
keywords: acaricide; honey; liquid chromatography-tandem mass spectrometry; surveillance