Citation: 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. doi: 10.3724/SP.J.1123.2013.01033 shu

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

1.
Fuqing Entry-Exit Inspection and Quarantine Bureau, Fuqing 350300, China

Corresponding author: DING Liping,
Received Date: 17 January 2013
Available Online: 21 February 2013
Fund Project: 福建出入境检验检疫局项目(FK2011-61). (FK2011-61)

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.
- multiple adsorption synchronous purification (MASP),
- gas chromatography-mass spectrometry (GC-MS),
- butene-fipronil,
- residue,
- dry samples
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沈阳化工大学材料科学与工程学院沈阳 110142