超高效液相色谱-串联质谱法测定水产品中硝基呋喃类代谢物

Determination of nitrofuran metabolites in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

[目的]建立超高效液相色谱-串联质谱法(LC-MS/MS)测定鱼肉中呋喃它酮(AMOZ)、呋喃西林(SEM)、呋喃妥因(AHD)和呋喃唑酮(AOZ)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7.0~7.5,经乙酸乙酯提取,5%甲醇水溶液定容,采用多反应监测(MRM)模式,电喷雾正离子(ESI+)模式电离,内标法定量。[结果]硝基呋喃代谢物在0.5~50.0 ng/mL范围内线性关系良好,相关系数R>0.996。方法检出限为0.5μg/kg,3个添加水平(0.5、1.5、5.0μg/kg)下的回收率在70%~120%范围内,相对标准偏差RSD均小于10%。[结论]该方法具有较好的准确性和稳定性,能够用于鱼肉中硝基呋喃代谢物的检测。

[Objectives]To establish a method for the determination of furaltadone(AMOZ),nitrofura-zone(SEM),nitrofurantoin(AHD)and furazolidone(AOZ),four nitrofuran metabolites in aquatic prod-ucts by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).[Methods]The samples were derivatized by 2-nitrobenzaldehyde,and the pH value was adjusted to 7.0-7.5.The samples were extracted by ethyl acetate,and 5%methanol in aqueous solution was fixed volume.The samples were detected by selective multiple reaction monitoring(MRM)mode,ionized by electrospray positive ion(ESI+)mode,and quantified by internal standard method.[Results]The nitrofuran metabolite had a good linear relationship in the range of 0.5-50.0 ng/mL,and the correlation coefficients()better than 0.996,and the detection limit of this method was 0.5μg/kg.The recoveries rates were in the range of 70%-120%at the three supplemental levels(0.5,1.5 and 5.0μg/kg),and the relative standard deviation(RSD)was less than 10%.[Conclusions]The results show that this method has good accuracy and stability,and can be used for the determination of nitrofuran metabolites in fish.