基于疏水性低共熔溶剂的分散液液微萃取结合气相色谱-串联质谱法测定肉及肉制品中拟除虫菊酯农药残留

Determination of pyrethroid pesticide residues in meat and meat products by gas chromatography-tandem mass spectrometry with hydrophobic deep eutectic solvent-dispersive liquid-liquid microextraction

中文关键词:  疏水性低共熔溶剂  分散液液微萃取  拟除虫菊酯农药  肉及肉制品

英文关键词:hydrophobic deep eutectic solvent  dispersive liquid-liquid microextraction  pyrethroid pesticides  meat and meat products

中文摘要:

      目的 建立疏水性低共熔溶剂-分散液液微萃取结合气相色谱-串联质谱法(gas chromatography- tandem mass spectrometry, GC-MS/MS)测定肉及肉制品中9种拟除虫菊酯农药残留的分析方法。方法 样品先经乙腈进行提取, 提取液加入微量由DL-薄荷醇与正辛醇(物质的量比为1:3)合成的疏水性低共熔溶剂进行分散液液微萃取。对影响萃取效率的因素, 如样品提取条件、萃取剂种类及体积、氯化钠浓度等进行了考察。结果 所有目标物在0.002~0.500 μg/mL范围内线性良好, 相关系数(r2)为0.9964~0.9990, 检出限为0.5~ 2.0 μg/kg, 定量限为2.0~6.0 μg/kg, 目标物回收率为72.5%~101.6%, 相对标准偏差(relative standard deviations, RSDs)为1.2%~6.0%。结论 该方法环保、准确、灵敏, 适用于肉及肉制品中拟除虫菊酯农药的测定。

英文摘要:

      Objective To establish a method for the determination of 9 kinds of pyrethroid pesticide residues in meat and meat products by hydrophobic deep eutectic solvent-dispersive liquid-liquid microextraction coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The sample was extracted with acetonitrile, the extraction solution was added with trace hydrophobic deep eutectic solvent that prepared with menthol-1-octanol (1:3, substance ratio) for dispersive liquid-liquid microextraction. The factors affecting extraction efficiency, such as sample extraction conditions, types and volumes of extractants, and concentration of sodium chloride, were investigated. Results The linearities were good within the range of 0.002?0.500 μg/mL, with the correlation coefficient (r2) were 0.9964?0.9990, the limits of detection were 0.5?2.0 μg/kg, the limits of quantitation were 2.0?6.0 μg/kg, the recoveries of the target were 72.5%?101.6%, and the relative standard deviations (RSDs) were 1.2%?6.0%. Conclusion The developed method is environmental, accurate and sensitive, it is applicable for the determination of pyrethroid pesticide residues in meat and meat products.