›› 2009, Vol. 21 ›› Issue (4): 0-384.

• 论文 •    

GC/MS法研究鸡体内三聚氰胺的残留及代谢规律

余晓华 1,2,孙泽祥 2,吕 燕 3,杨挺 3,方维焕 1   

  1. 1 浙江大学动物科学学院,浙江杭州310029;2 宁波市畜牧兽医局,浙江宁波315012;3 宁波市农业科学研究院,浙江宁波315040
  • 收稿日期:1900-01-01 修回日期:1900-01-01 出版日期:2009-07-25 发布日期:2009-07-25

Determination of residues and metabolism of melamine in chicken using GC/MS

YU Xiao—hua;SUN Ze—xiang;LU Yan;YANG Ting;FANG Wei-huan   

  1. 1 College of Animal Science,Zhejiang University,Hangzhou 310029,China; 2 Ningbo Bureau of Animal Husbandry and Veterinary Medicine,Ningbo 315012,China;3 Ningbo Academy of Agricultural Sciences,Ningbo 315040,China
  • Received:1900-01-01 Revised:1900-01-01 Online:2009-07-25 Published:2009-07-25

摘要: 研究建立了气相色谱一质谱法(GC/MS)测定鸡体内三聚氰胺残留的方法。样品以10 L三氯乙酸
溶液提取,Cleanert PCX固相萃取柱净化,50℃水浴中氮气吹干后衍生化。以G(1/Ms选择99,171,327,342 4个碎片离子进行定性定量分析。三聚氰胺在0.05~2.50 mg/L呈线性(R 为0.999),鸡蛋中3种不同添加浓度0.05,0.10和0.50 ms/ks下三聚氰胺平均回收率分别为84.71% ,88.12%,92.62%;相对标准偏差分别为10.57% ,7.12% ,6.92%;样品中最低检测限(S/N=3)为0.005 ms/kg。采用该方法研究三聚氰胺在鸡体内的代谢机理,结果表明:在较高饲喂浓度(1 000 ms/kg)时,用药后,鸡体内三聚氰胺蓄积量逐渐增加,最高蓄积浓度为16.465 ms/kg,但停药后代谢又非常快。

关键词: 鸡蛋, 三聚氰胺, 残留, 气相色谱一质谱法(GC/MS)

Abstract: A method for determination of melamine residues in chicken by gas chromatography-mass spectrometry(GC/MS) was developed.The melamine Was extracted from chicken samples by employing 10 S/L trichioroaeetic acid solution,the cleaning procedure was performed by Cleanert PCX solid phase extraction cartridge.Th e extracts were warmed with water at 50 ℃ and blowed with nitrogen until it got near to dryness and then it was derivated .Retention time and specific ions were used to identify melamine.The selective fragments were m/z 99,171,327,342,respectively.The calibration curve of melamine was linear(correlation coeficient:0.999)in the range of O.05—2.5 ms/L.The average recovery rates(at 0.05,0.10 and 0.50 mg/kg)were 84.71% ,88.12% ,92 .62% ,respectively;while the relative standard deviations (RSD)of the method were 10.57% ,7.12% ,6.92 % ,respectively;and the limit of detection(LOD),defined in terms of 3 times baseline nosie Was 0.005 ms/kg.The developing method Was applied to study the metabolic behaviour and mechanism of melamine in chicken.Th e results indicated that the residual contents of melamine was increased gradually in chicken fed with higher dosage(1 000 mg/kg),and the highest content ofmelamine Was 16.465 ms/kg.However,the content of melamine in chicken was reduced immediately after feeding withdrawal.

Key words: chicken, melamine, residual, gas chromatography—mass spectrome try(GC/MS)