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Determination of pesticides originating from golf courses by solid-phase extraction and liquid chromatography-tandem mass spectrometry
Authors:Miho Shinomiya
Institution:1. National Environmental Research and Training Institute , Ministry of the Environment Namiki 3-3, Tokorozawa , Saitama 359-0042 , Japan miho_shinomiya@env.go.jp
Abstract:A multi-residue method using liquid chromatography coupled to triple quadrupole tandem mass spectrometry (LC-MS/MS), associated with solid-phase extraction (SPE), was developed for the determination of 21 pesticides in water samples. The compounds investigated are used for the maintenance of golf courses and ordinarily measured by gas chromatography-mass spectrometry (GC-MS). Electrospray ionisation (ESI) was applied to all compounds, and LC and MS conditions were optimised to measure them under SRM mode. This method showed excellent linearity ranges for all pesticides, with correlation coefficients greater than 0.996. Two kinds of extraction cartridges, namely, styrene divinylbenzene polymer (Sep-Pak PS-2) and divinylbenzene-N-vinylpyrrolidone copolymer (Oasis HLB), were tested and the extraction conditions were optimised. All the pesticides were determined using acetonitrile and ethyl acetate as eluents in both cartridges, and good recoveries (>77%) and repeatability with low relative standard deviations (RSDs, <12%) were achieved from ultra-pure water. In addition, satisfactory recoveries (>76%) and low intra-day and inter-day RSDs (<15%) of all pesticides were also obtained with the Sep-Pak PS-2 cartridge when using river water. The method limits of detection (LODs) ranged between 0.068 (diazinon) and 3.9 (triclopyrbutoxyethyl)?ng?L?1. The analytical method was successfully applied for the determination of pesticides in surface river water.
Keywords:pesticide  solid-phase extraction  liquid chromatography  tandem mass spectrometry  water  golf course
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