[关键词]
[摘要]
以改进的QuEChERS(quick,easy,cheap,effective,rugged and safe)前处理方法结合气相色谱-三重四极杆质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)技术,建立了鸡蛋中七种手性拟除虫菊酯类有机污染物的检测和分析方法,为鸡蛋中拟除虫菊酯残留限量的制定提供依据。将鸡蛋样品经80%乙酸乙酯-丙酮提取,乙二胺-N-丙基甲硅烷(PSA)净化,无水硫酸镁脱水,以HP-5MS毛细管柱进行分离,在电子轰击源(EI)和多反应监测模式下进行测定,基质曲线外标法定量。结果表明,该方法能有效的分离7种手性拟除虫菊酯,峰形良好,待测物质在1~200 μg/L范围内线性良好,相关系数大于0.99,检出限为0.46~1.59 μg/kg,定量限为1.52~5.29 μg/kg,加标回收率范围为72.1%~117.5%,相对标准偏差(RSD)为1.6%~15.1%(n=6)。该方法前处理简单易行,便于操作,方法精密度高,适用于鸡蛋中拟除虫菊酯类有机污染物的快速筛查和定量检测。
[Key word]
[Abstract]
The modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, as a pre-treatment method, combined with gas chromatography-tandem mass spectrometry (GC-MS/MS), was established for the determination of seven chiral pyrethroid organic pollutants in eggs, so as to provide a basis for the establishment of the pyrethroid residue limit in eggs. The egg samples were extracted with 80% ethyl acetate-acetone, purified by ethylenediamine-N-propylsilane (PSA), and dehydrated by anhydrous magnesium sulfate. The obtained extracts were further separated using a HP-5MS capillary column. The seven compounds were determined using an electron impact (EI) ion source and multi-reaction monitoring (MRM) mode and quantified using the matrix-matched calibration curve external standard method. The results showed that this method could effectively separate the seven chiral pyrethroids. The seven compounds showed good peak shapes, displayed good linearity over the range of 1~200 μg/L, and the correlation coefficients were greater than 0.99. The limits of detection (LODs) were 0.46~1.59 μg/kg, the limits of quantitation (LOQs) were 1.52~5.29 μg/kg, and the recovery rates were in the range of 72.1%~117.5% with relative standard deviations (RSDs) between 1.6% and 15.1% (n = 6). This pre-treatment method was proven to be simple, accurate, efficient, and suitable for rapid screening and quantitative analysis of chiral pyrethroid organic pollutants in eggs.
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[基金项目]
国家重点研发计划项目重点专项(2018YFC1602304);湖北省自然科学基金青年项目(2019CFB380);湖北省食品药品监督管理局科研项目(201801011)