Four nitrofuran metabolites, including semicarbazide ( SEM), 1-amino-hydantoin ( AHD) , 3-amino-2-oxazolidinone (AOZ) and 5-methylmorphoIino-3-amino-2-oxazolidinone (AMOZ) in Uiopenaem vannamei, were determined by ultra performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS). SEM-I3C-I5N2, AHD-13C3, A0Z-D4 and AMOZ-D5 were selected as internal standard substances; the samples were derived by 2-nitrobenzaldehyde, extracted with ethyl acetate and cleaned up with n-hexane. Four targeted compounds were completely separated within 8 minutes by gradient elution of methanol and 0. 5 mmol·L-1 ammonium acetate including 0. 1% fomic acid, and they have good linear relation within 0. 4 -20.0 ng·mL-1 (R >0. 999) , the limit of detection being 0.03 -0. 15 μg·kg-1. The recovery is 92.0% ~ 107.3% (n =6) and the relative standard deviation is 3. 1% ~ 8.7% at 0.5 μg·kg-1, 1. 0 μg·kg-1 and 2. 0 μg·kg-1. The method achieved satisfactory result in the FAPAS(Food Analysis Performance. Assessment Scheme) International Proficiency Testing.%采用超高效液相色谱-串联质谱(UPLC-MS/MS)法,测定了凡纳滨对虾(Litopenaeus vannamei)中氨基脲(SEM)、1-氨基-2-内酰脲(AHD)、3-氨基-2-唑烷基酮(AOZ)和5-甲基吗啉-3-氨基-2-唑烷基酮(AMOZ)4种硝基呋喃类代谢物.采用2-硝基苯甲醛作为衍生化试剂,氘、碳-13、氮-15同位素标记的SEM-13 C-15 N2、AHD-13C3、AOZ-D4和AMOZ-D5为内标物,样品经衍生、乙酸乙酯提取、正己烷净化,以甲醇0.5 mmol·L-1乙酸铵水溶液(含0.1％甲酸)为流动相进行梯度洗脱,8 min可将4种目标化合物完全分离并测定.结果表明,4种待测物在0.4 ～20.0 ng·mL-1范围内线性关系良好(R＞0.999),检出限为0.03 ～0.15 μg·kg-1.在0.5μg·kg-1、1.0 μg·kg-1和2.0 μg·kg-13个水平上进行加标回收试验,平均回收率为92.0％～107.3％,RSD为3.1％ ～8.7％.采用该法参加FAPAS国际水平测试,获得了满意的结果.
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