摘要
对115个水产品及鱼苗样品进行呋喃妥因(AHD)、呋喃它酮(AMOZ)、呋喃唑酮(AOZ)和呋喃西林(SEM)4种硝基呋喃代谢物残留量分析。样品水解、衍生和净化后,采用液相色谱-电喷雾三重四级杆串联质谱仪检测,多反应监测扫描模式和同位素内标法定量。各类硝基呋喃代谢物线性范围为0.5～20ng/mL、检出限0.25μg/kg,在0.25～5μg/kg范围内样品添加回收率为89.0%～117.2%,相对标准偏差小于10%。结果表明,水产鱼苗中的硝基呋喃代谢物残留量远远高于成鱼,其中大黄鱼苗中AOZ的检出率为62%,最大残留量3890μg/kg,而大黄鱼成鱼AOZ的检出率17%,最大残留量2.81μg/kg,同时淡水鱼的硝基呋喃类药物残留小于海产鱼。
In this study,we presented a high performance liquid chromatography-tandem mass spectrometric（HPLC-MS/MS） method for determining 4 nitrofuran metabolites in 115 fish or fry products,namely 1-aminohydantoin hydrochloride（AHD）,3-amino-5-morpholinomethyl-2-oxazolidineone（AMOZ）,3-amino-2-oxazolidinone（AOZ） and semicarbazide（SEM）.Samples were subjected to hydrolysis,derivation and clean-up prior to HPLC-MS/MS analysis.The analysis was carried out in the multi reaction monitoring（MRM） mode and internal standard isotope dilution method was used for quantification.Calibration curves for the analytes exhibited good linearity over the concentration range from 0.5 to 20 ng/mL and their limits of detection were all 0.25μg/kg.Average recoveries for them spiked at 3 levels ranged from 89.0% to 117.2%,with a RSD of less than 10%.Nitrofuran metabolites residues in fry were found much higher than those in adult fish.The detection rate of AOZ in large yellow croaker fry was 62%,with a maximum residue of 3890μg/kg;however,for large yellow croaker,the detection rate and the maximum residue were both comparatively lower,17% and 2.81 μg/kg,respectively.Less nitrofuran metabolites residues were detected in fresh water fish than in their sea counterpart.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2010年第12期206-211,共6页
Food Science
关键词
硝基呋喃代谢物
高效液相色谱-串联质谱
水产品
nitrofuran metabolites
high performance liquid chromatography-tandem mass spectrometry
fish and fry products
