液相色谱-串联质谱法测定甲壳类水产品中氨基脲的含量

利用液相色谱-串联质谱技术测定了甲壳类水产品中氨基脲的含量。样品用HCl水解、2-硝基苯甲醛衍生、乙酸乙酯萃取,液相色谱分离,串联质谱检测,内标法定量。方法检出限为0.25μg/kg(S/N>3);定量限为0.5μg/kg(S/N>10)。甲壳类水产品的品种涉及青虾、斑节对虾、罗氏沼虾、南美白对虾、小龙虾、青蟹、珍宝蟹、三疣梭子蟹、中华绒螯蟹和鲎等。虾类样品中氨基脲的含量在未检出～370.4μg/kg之间,蟹类样品中氨基脲的含量在未检出～87.5μg/kg之间。氨基脲在甲壳中含量最高,在肌肉中含量最低。结果表明:氨基脲作为内源性物质普遍存在于甲壳类水产品中。

Determination of Semicarbazide Content in Crustaceans by Liquid Chromatography Tandem Mass Spectrometry

The content of semicarbazide in crustaceans had been determined by LC/MS/MS.Samples were hydrolyzed by hydrochloric acid and derivatized with 2-nitrobenzaidehyde.After extraction with ethyl acetate,chromatographic separation was achieved by HPLC and the target compound was detected by tandem mass spectrometry using internal standard as quantification method.The qualitative limit was 0.25 μg/kg(S/N>3)and the quantitative limit was 0.5 μg/kg(S/N>10).Crustacean species were from natural water and free market of agricultural products including oriental river prawn,giant tiger prawn,giant freshwater prawn,white-leg shrimp,red swamp crayfish,mud crab,dungeness crab,swimming crab,mitten crab and horse shoe crab.Concentrations of semicarbazide in shrimp and in crab were from not detected to 370.4 μg/kg and not detected to 87.5 μg/kg and concentrations of semicarbazide varied from tissues with highest in carapace and lowest in muscle.In the present study,the results revealed that semicarbazide was an endogenous substance existing in crustaceans.