色谱

色谱 ›› 2013, Vol. 31 ›› Issue (8): 747-752.DOI: 10.3724/SP.J.1123.2013.01033

• 研究论文 • 上一篇    下一篇

多重吸附同步净化-气相色谱-质谱法测定干性样品中丁烯氟虫腈的残留量

丁立平, 郭菁, 郑铃, 陈春添, 陈志涛   

  1. 福清出入境检验检疫局, 福建 福清 350300
  • 收稿日期:2013-01-17 修回日期:2013-02-21 出版日期:2013-08-28 发布日期:2013-09-29
  • 通讯作者: 丁立平
  • 基金资助:

    福建出入境检验检疫局项目(FK2011-61).

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

DING Liping, GUO Jing, ZHENG Ling, CHEN Chuntian, CHEN Zhitao   

  1. Fuqing Entry-Exit Inspection and Quarantine Bureau, Fuqing 350300, China
  • Received:2013-01-17 Revised:2013-02-21 Online:2013-08-28 Published:2013-09-29
  • Contact: O658

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221

被引次数

6

摘要：

建立了干性样品中丁烯氟虫腈残留量的多重吸附同步净化(MASP)-气相色谱-质谱检测方法。前处理以1%乙酸-乙腈提取样品,应用MASP法对样品同时进行提取、盐析和净化,并利用气相色谱-质谱仪在选择离子扫描(SIM)模式下进行检测,以基质匹配标准溶液外标法定量。结果表明:丁烯氟虫腈在2~100 μg/L范围内线性关系良好,相关系数(r2)不小于0.999;在2~10 μg/kg添加水平范围内,丁烯氟虫腈的平均回收率为92.2%~97.5%,相对标准偏差(RSD, n=6)为2.69%~5.21%;方法检出限(S/N=3)为2 μg/kg;定量限(S/N=10)为6 μg/kg。本方法操作简便、快速、准确,可用于干性样品中丁烯氟虫腈的日常检测。同时,对丁烯氟虫腈的裂解机理进行了探讨。

关键词: 残留量, 丁烯氟虫腈, 多重吸附同步净化(MASP), 干性样品, 气相色谱-质谱

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

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