气相色谱质谱-同位素内标法定量分析动物源性食品中的三聚氰胺.pdf

分析检测 气相色谱/质谱-同位素内标法定量分析动物源性食品 中的三聚氰胺 1* 1 2 1 1 巢强国 ，葛宇 ，王守法 ，周耀斌 ，雷涛 1.上海市质量监督检验技术研究院 (上海 200233)，2.华东理工大学生物工程学院 (上海 200237) 摘 要 采用同位素内标物定量法，建立了一种适合检测动物源性食品中三聚氰胺残留的气相色谱-质 谱(GC-MS)方法。使用1%的三氯乙酸溶液提取动物源性食品中三聚氰胺残留，经阳离子交换固相萃取 柱净化后，氮气吹干、硅烷化衍生，再由气相色谱-质谱联用仪检测和确证。选用同位素标记三聚氰胺 13 15 ( C N N H )内标法定量。该方法在五种具有代表性的动物食品中三聚氰胺加标回收率78.28%~110.84%， 3 3 3 6 相对标准偏差(RSD)不大于6.80%，在(0.02~1.00) mg/kg浓度范围内呈现良好的线性关系；灵敏度高，最低 检测限达到0.023 mg/kg；选择性好，能有效消除复杂基体的干扰。适合于动物源性食品中三聚氰胺的确 证和定量分析。 关键词 同位素内标；气相色谱-质谱(GC/MS)；三聚氰胺；同位素标记三聚氰胺；动物源性食品 Isotope Internal Standard Method for Quantitative Analysis of Melamine in Animal Derived Food by Gas Chromatography/Mass Spectrometry 1* 1 2 1 1 Chao Qiang-Guo ，Ge Yu ，Wang Shou-Fa ，Zhou Yao-Bin ，Lei Tao 1.Shanghai Institute of Quality Inspection and Technical Research (Shanghai 200233) 2.College of Bioengineering, East China University of Science and Technology (Shanghai 200237) Abstract A suitable gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of melamine with isotope internal standard in animal-derived food. The melamine residue in animal- derived food was extracted by 1% solution of trichloroacetic, purifi ed by cation exchange solid phase extraction column, blow-dried by nitrogen, derivatized by silane derivatives, and then detected and confirmed by gas 13 15 chromatography-mass spectrometry, and quantifi ed by isotope labeled melamine( C N N H ) internal stan