气相色谱-串联质谱正离子模式测定食品中氟虫腈和溴虫腈残留
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薄海波 女 副教授 研究方向为食品安全与质量分析研究E-mail:bohb1212@163.com

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Determination of fipronil and chlorfenapyr residues in foodstuffs by gas chromatography-tandem mass spectrometry in positive ion mode
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    摘要:

    建立食品中氟虫腈和溴虫腈残留的气相色谱-串联质谱(GC-MS/MS)分析方法。方法 试样经乙腈提取, N-丙基乙二胺(PSA)固相萃取柱(SPE)净化,采用GC-MS/MS以正离子模式多反应监测(MRM)定性、定量测定氟虫腈和溴虫腈。结果 该方法在5~50μg/L浓度范围内呈线性,相关系数r均大于0.998。氟虫腈和溴虫腈的添加回收率分别为78.2%~102.5%和77.0%~104.1%,RSD分别为6.8%~15.2%和6.9%~17.1%,二者的检出限(LOD)均为5μg/kg,定量限(LOQ)均为10μg/kg。结论 气相色谱-串联质谱法正离子模式是简便、快速、准确测定食品中氟虫腈和溴虫腈残留分析方法。

    Abstract:

    To develop an analytical method for determination of fipronil and chlorfenapyr residues in foodstuffs by gas chromatography-tandem mass spectrometry (GC-MS/MS).MethodsFipronil and chlorfenapyr were extracted with acetonitrile and cleaned-up by a PSA solid phase extract (SPE) column for GC-MS/MS determination. Fipronil and chlorfenapyr were separated by a THERMO TR-Pesticide II column and detected by multiple reaction monitoring (MRM) with electrospray ionization operating in the positive ion mode.Results The calibration curves were linear between the range of 5-50μg/L with r≥0.998. The recoveries of fipronil spiked sample ranged 78.2%-102.5% with RSD 6.8%-15.2%, and the recoveries of chlorfenapyr ranged 77.0%-104.1% with RSD 6.9%-17.1%. The limits of detection (LODs) and limits of quantification (LOQs) of fipronil and chlorfenapyr were both 5and 10μg/kg, respectively.Conclusion GC-MS/MS in positive ion mode is an simple, rapid, accurate analytical method for determination of fipronil and chlorfenapyr residues in foodstuffs

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薄海波.气相色谱-串联质谱正离子模式测定食品中氟虫腈和溴虫腈残留[J].中国食品卫生杂志,2013,25(5):431-434.

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  • 收稿日期:2013-07-02
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  • 在线发布日期: 2013-10-25
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