高效液相色谱-串联质谱法快速测定食品中的抗倒胺残留量

Determination of inabenfide residue in food by high performance liquid chromatography-tandem mass spectrometry

建立了水果、蔬菜、茶叶、蜂蜜、粮谷和动物源性食品中抗倒胺残留的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品经乙腈提取,混合使用乙二胺-N-丙基硅烷和十八烷基硅烷键合相基质分散净化后,用HPLC-MS/MS检测和确证,外标法定量。质谱分析采用电喷雾电离,正离子扫描,多反应监测模式。该方法通过建立基质标准曲线消除基质效应,抗倒胺在1～100μg/kg范围内具有良好的线性关系,相关系数在0.998～0.999之间;样品中添加5、10、50μg/kg的标准品,其添加回收率在85.2%～112.4%之间,相对标准偏差均小于8.5%;检出限(LOD)在0.08～1.64μg/kg之间,定量限(LOQ)在0.30～5.48μg/kg之间。实验结果表明,该方法提取效果好,具有良好的灵敏度、回收率和重复性。

A high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/ MS） method was established for the determination of inabenfide in fruits, vegetables, tea, hon- ey, cereals and animal-derived foods. The food samples were extracted with acetonitrile, then purified by dispersion solid phase extraction using primary secondary amine （PSA） and C 18 as solid phase. The residue was determined and confirmed by HPLC-MS/MS and quantified by external standard method. The mass spectrometric detection was operated with electrospray in positive ionization mode and inabenfide was identified in multiple reaction monitoring （MRM） mode. The interference of matrix was reduced by the matrix-matched calibration standard curves. The linear range of the method was 1 - 100 μg/kg, with the correlation coefficients （r2） of 0. 998 - 0.999. The recoveries of inabenfide spiked in food samples were 85.2% - 112.4% at the spiked levels of 5, 10, 50 μg/kg. The relative standard deviations （RSDs） were less than 8.5%. The limits of detection （LODs） were 0.08 - 1.54 μg/kg, and the limits of quantification （LOQs） were 0.30 - 5.48 μg/kg. The results showed that the proposed method is sensitive and accurate for the determination of inabenfide in foodstuffs.