超高效液相色谱-串联质谱法测定凡纳滨对虾中的硝基呋喃代谢物残留

Determination of residues of nitrofuran metabolites in Litopenaeus vannamei by UPLC-MS/MS

  • 摘要: 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-13C-15N2、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0.5 μg·kg-1、1.0 μg·kg-1和2.0 μg·kg-1 3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。

     

    Abstract: Four nitrofuran metabolites, including semicarbazide (SEM), 1-amino-hydantoin (AHD), 3-amino-2-oxazolidinone (AOZ) and 5-methylmorpholino-3-amino-2-oxazolidinone (AMOZ) in Litopenaeus vannamei, were determined by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). SEM-13C-15N2, AHD-13C3, AOZ-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.

     

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