Determination of butene-fipronil residue in dry samples by multiple adsorption synchronous purification-gas chromatography-mass spectrometry

doi:10.3724/SP.J.1123.2013.01033

Abstract

Abstract:

A method was developed for the determination of butene-fipronil residue in dry samples by multiple adsorption synchronous purification (MASP)-gas chromatography (GC)-mass spectrometry (MS). After extracted with 1% acetic acid-acetonitrile, the samples were pretreated with MASP method including extraction, salting-out and purification procedures, and analyzed with GC-MS under the selected ion monitoring (SIM) mode, and then quantified by matrix-match standard solution with external standard method. The results showed good linearity in the range of 2-100 μg/L with the correlation coefficients (r²)not less than 0.999. The average fortified recovery of butene-fipronil in samples was found in the range of 92.2%-97.5% at three fortified levels from 2 to 10 μg/kg, with the relative standard deviations of 2.69%-5.21% (n=6). The limit of detection (S/N=3) for butane-fipronil was 2 μg/kg and the limit of quantification (S/N=10) was 6 μg/kg. The method is simple, rapid and accurate, and could be used for the routine analysis of butane-fipronil in dry samples. Meanwhile, the pyrolysis mechanism of butane-fipronil, as a new substance, is discussed.

Key words: butene-fipronil, dry samples, gas chromatography-mass spectrometry (GC-MS), multiple adsorption synchronous purification (MASP), residue

CLC Number:

O658

DING Liping, GUO Jing, ZHENG Ling, CHEN Chuntian, CHEN Zhitao. Determination of butene-fipronil residue in dry samples by multiple adsorption synchronous purification-gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2013, 31(8): 747-752.

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