动物源性食品中硝基呋喃代谢物的超高效液相色谱-串联质谱测定法

目的建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定8种基质(鸡肉、鸭肉、牛肉、猪肉、鱼肉、虾肉、海参、鸡肝)中呋喃它酮、呋喃西林、呋喃妥因和呋喃唑酮4种硝基呋喃代谢物的检测方法。方法试样经2-硝基苯甲醛衍生化,调节pH值至7.2~7.6,经Oasis HLB固相萃取柱净化,由乙酸乙酯洗脱,流动相定容,采用选择反应监测(SRM)模式检测,电喷雾正离子(ESI+)模式电离,同位素内标法定量。结果硝基呋喃代谢物在0.5~30.0μg/L范围内线性关系良好(r>0.99)。方法的最低检出限为0.5μg/kg,在0.5、1.0、2.0μg/kg的3个添加水平的回收率为60.9%~103.5%,相对标准偏差(RSD,n=6)在2.1%~11.1%之间。结论超高效液相色谱-串联质谱测定法快速、灵敏、准确,适合动物源性食品中硝基呋喃代谢物的测定。

Determination of nitrofuran metabolites in animal derived food by ultra performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for the determination of nitrofuran metabolites (furantazone,furacilin,furantoin and furazolidone) in eight animal derived matrices (including chicken muscle,duck muscle,beef muscle,pork muscle,fish muscle, prawn muscle,sea cucumber,chicken liver) by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/ MS). Methods Samples were derivatized with 2-nitrobenzaldehyde and adjusted the pH value to 7.2-7.6. The derivatized solutions were cleaned up by Oasis HLB solid extraction column (SPE)and the target compounds were eluted with ethylacetate. The analysis were carried out on electrospray ion (ESI+) source in the positive mode and monitored by selective reaction monitoring(SRM) mode. The internal standard isotope dilution method was used for quantification. Results The calibration curve showed a good linearity in the range of 0.5-30.0 μg/L and the correlation coefficient (r) was higher than 0.99. The limit of determinations was 0.5 μg/kg. At the spiked levels of 0.5,1.0 and 2.0 μg/kg,the recoveries of nitrofuran metabolites ranged from 60.9% to 103.5% and the relative standard deviation (RSD,n=6) ranged from 2.1% to 11.1%. Conclusion The method of UPLC-MS/MS is simple,rapid,sensitive and suitable for the qualitative and quantitative analysis of nitrofuran metabolites in animal derived food.