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目的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。
Objective To establish a gas chromatography-tandem mass spectrometry (GC-MS / MS) method for the determination of fipronil and chlorfenapyr in food. Methods The samples were extracted with acetonitrile and purified with N-propyl ethylenediamine (PSA) solid phase extraction column (SPE). The samples were qualitatively and quantitatively determined by GC-MS / MS with positive ion mode MRM. Chlorfenapyr. Results The method was linear in the concentration range of 5 ~ 50μg / L, the correlation coefficient r was greater than 0.998. The recoveries of fipronil and chlorfenapyc were 78.2% -102.5% and 77.0% -104.1%, respectively, with RSDs of 6.8% -15.2% and 6.9% -17.1%, respectively. The detection limits (LODs) 5μg / kg, the limit of quantification (LOQ) were 10μg / kg. Conclusion Gas chromatography-tandem mass spectrometry positive ion mode is a simple, rapid and accurate method for the determination of fipronil and chlorfenapyr residues in food.