HPLC–MS/MS法测定南美白对虾苗中硝基呋喃类代谢物残留

研究了南美白对虾苗中4种硝基呋喃代谢物呋喃唑酮代谢物(AOZ)、呋喃它酮代谢物(AMOZ)、呋喃妥因代谢物(AHD)、呋喃西林代谢物(SEM)的高效液相色谱–串联质谱(HPLC–MS/MS)测定方法。以水解衍生并添加4种同位素内标的方法对样品进行处理,补偿了衍生化效率,提高了定量的准确性。实验结果表明,AOZ,AMOZ的检出限为0.10μg/kg,SEM,AHD的检出限为0.25μg/kg;AOZ,AMOZ的定量下限为0.40μg/kg,SEM,AHD的定量下限为0.50μg/kg。方法加标回收率在88.2%~97.6%之间,相对标准偏差在4.6%~8.1%(n=6)之间。该法检测灵敏度高,测量结果的精密度和准确度满足药物残留检测要求。

Determination of Metabolites of Nitrofuran Antibiotics Residual in Penaeus Vannamei Seeds

High performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） method was developed for simultaneously analyzing the metabolites of four nitrofuran antibiotics such as furazolidone,furaltadone, nitrofurazone and nitrofurantoin in Penaeus vannamei seed. Four isotope internal standards were utilized to improve the quantitative precision. The detection limits （LODs） were 0.10μg/kg for the metabolite of furazolidone and furaltadone, and 0.25μg/kg for the metabolite of nitrofurazone and nitrofurantoin. The quantitative limits were 0.40μg/kg for the metabolite of furazolidone and furaltadone, and 0.50μg/kg for the metabolite of nitrofurazone and nitrofurantoin. The recoveries calibrated by internal standard ranged from 88.2%to 97.6%with the relative standard deviations of 4.6%-8.1%（n=6）. The method has high detection sensitivity and the detection result can meet the requirements of drug residue detection.