Li Jige, Fang Lanyun, Wang Yufei, Lu Yanyan, Zhao Yonggang, Jin Micong
Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China.
Wei Sheng Yan Jiu. 2021 Sep;50(5):792-798. doi: 10.19813/j.cnki.weishengyanjiu.2021.05.015.
To develop a method for determination of fipronil and its metabolites in eggs by gas chromatography-tandem mass spectrometry(GC-MS/MS)cleaned with dispersive-solid phase extraction(D-SPE).
Orthogonal array design with OA16(4~4) matrices was used to optimize the efficiency of D-SPE. The targets were extracted from samples with acetonitrile, and followed by D-SPE cleanup. The extracts were analyzed by GC-MS/MS, and quantified by internal standard method with matrix correction.
The calibration curves showed good linearity in the range of 1.0-250.0 μg/L. The correlation coefficients were larger than 0.99.The average recoveries spiked in eggs at the levels of 2 μg/kg, 4 μg/kg and 20 μg/kg were between 87.1% and 125.0%(n=6), and the relative standard deviations were less than 10%. The limits of determination were between 0.1 and 0.4 μg/kg, and the limits of quantitation were between 0.3 and 1.2 μg/kg.
The method possesses low background, high sensitivity. It can be applied to determine the residues of fipronil and its metabolites in eggs.
建立一种采用分散固相萃取（D-SPE）净化、气相色谱-串联质谱（GC-MS/MS）测定鸡蛋中氟虫腈及其代谢物的方法。
采用OA16(4~4)矩阵的正交试验设计优化D-SPE的净化效率。目标物用乙腈从样品中提取，然后进行D-SPE净化。提取物采用GC-MS/MS分析，采用基质校正内标法进行定量。
校准曲线在1.0250.0 μg/L范围内呈良好线性，相关系数大于0.99。在鸡蛋中添加2 μg/kg、4 μg/kg和20 μg/kg水平的平均回收率为87.1%125.0%（n=6），相对标准偏差小于10%。测定限为0.10.4 μg/kg，定量限为0.31.2 μg/kg。
该方法背景低、灵敏度高，可用于测定鸡蛋中氟虫腈及其代谢物的残留量。
