高效液相色谱-串联质谱法测定禽肉中氟吡菌酰胺残留量的研究

Determination of fluopyram residues in poultry meat by high performance liquid chromatography-tandem mass spectrometry

建立了检测禽肉中氟吡菌酰胺的高效液相色谱-串联质谱法。试样通过20 mL 1%甲酸乙腈提取、5 g无水硫酸钠除水,分散固相萃取(QuEChERS)净化,以乙腈和0.1%甲酸水溶液作为流动相梯度洗脱,多反应监测模式(MRM)测定,基质曲线外标法定量。结果表明:氟吡菌酰胺在0.5μg/L~50μg/L浓度范围内线性良好(r>0.99),检出限:0.5μg/kg,回收率在87.5%~96.4%之间,相对标准偏差2.5%~7.7%。该方法快速、准确、适用于禽肉中氟吡菌酰胺的定性与定量检测。

A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for the determination of fluopyram in poultry meat was established.The sample was extracted with 20 mL of acetonitrile containing 1%formic acid,dehydrated with 5 g anhydrous sodium sulfate,purified by dispersed solid phase extraction(QuEChERS),gradient eluted with acetonitrile and 0.1%formic acid aqueous solution as mobile phase,determined by multi-reaction monitoring mode(MRM),and quantified by matrix curve external standard method.Results revealed that the linearity was good in the range of 0.5μg/L~50μg/L(r>0.99),and the limit of quantification of fluopyram was 0.5μg/kg,the recovery of fluopyram was 87.5%~96.4%,and the relative standard deviation was in range of 2.5%~7.7%.This method was rapid,accurate and suitable for the qualitative and quantitative determination of fluopyram in poultry meat.