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中国精品科技期刊2020
李敏青, 徐娟, 王岚, 安文佳, 庄嘉, 孙灵慧. 高效液相色谱-电喷雾电离串联质谱法测定植物性食品中氟虫腈及其代谢物的残留[J]. 食品工业科技, 2019, 40(2): 245-250,256. DOI: 10.13386/j.issn1002-0306.2019.02.042
引用本文: 李敏青, 徐娟, 王岚, 安文佳, 庄嘉, 孙灵慧. 高效液相色谱-电喷雾电离串联质谱法测定植物性食品中氟虫腈及其代谢物的残留[J]. 食品工业科技, 2019, 40(2): 245-250,256. DOI: 10.13386/j.issn1002-0306.2019.02.042
LI Min-qing, XU Juan, WANG Lan, AN Wen-jia, ZHUANG Jia, SUN Ling-hui. Determination of Fipronil and Its Metabolites Residues in Vegetative Foods by High Performance Liquid Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2019, 40(2): 245-250,256. DOI: 10.13386/j.issn1002-0306.2019.02.042
Citation: LI Min-qing, XU Juan, WANG Lan, AN Wen-jia, ZHUANG Jia, SUN Ling-hui. Determination of Fipronil and Its Metabolites Residues in Vegetative Foods by High Performance Liquid Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2019, 40(2): 245-250,256. DOI: 10.13386/j.issn1002-0306.2019.02.042

高效液相色谱-电喷雾电离串联质谱法测定植物性食品中氟虫腈及其代谢物的残留

Determination of Fipronil and Its Metabolites Residues in Vegetative Foods by High Performance Liquid Chromatography-tandem Mass Spectrometry

  • 摘要: 建立了高效液相色谱-串联质谱测定植物源食品(菠菜、苹果、香蕉、大米、大豆、茶叶)中的氟虫腈及其代谢物(氟虫腈砜,氟虫腈硫醚,氟甲腈)残留量的检测方法。以QuEChERS(Quick、Easy、Cheap、Effective、Rugged、Safe)提取盐包(CEN EN-15662)提取目标化合物,借助分散固相萃取或固相萃取(GCB/PSA)作为净化手段,经Thermo Accucore aQ(2.6 μm,2.1×150 mm)进行高效液相色谱分离,以电喷雾电离串联质谱多反应监测负离子模式进行检测,外标法定量。结果表明:4种分析物在0.1~5.0 μg/L范围内线性关系良好,相关系数(R2)均大于0.999。6种样品基质在3个添加水平(1、2、4 μg/kg)下的回收率为91.5%~101.5%,相对标准偏差为0.47%~3.88%;定量限(LOQ)均为0.1 μg/kg。该方法步骤简便、可靠、稳定,能满足于目前我国主要贸易国和地区的限量要求。

     

    Abstract: A methods was developed for the simultaneous determination of fipronil and its metabolites residues in various vegetative foods (such as spinach, apple, banana, rice, soybean and tea) by HPLC-MS/MS. The sample was extracted with acetronitrile by QuEChERS extraction tube (CEN EN-15662), cleaned-up with an dSPE or GCB/PSA solid phase extraction cartridge prior to separate on a Thermo Accucore aQ (2.6 μm, 2.1×150 mm), detected by HPLC-MS/MS with multiple reaction monitoring mode. The analyte was quantified by matrix-matched external standard method for fipronil and its metabolites. The results showed that good linearity was obtained when the concentration of the method was within 0.1~5 μg/L. The correlation coefficients (R2) were greater than 0.999. The average recoveries ranged from 91.5%~101.5% with the relative standard deviations of 0.47%~3.88% at the spiked levels of 1, 2, 4 μg/kg for fipronil and its metabolites. The limites of quantitation (LOQ) were 0.1 μg/kg. The methods were simple, sensitive and reliable, and had been applied successfully for the residue determination of fipronil in the real samples.

     

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