【摘要】 本文旨在建立同位素内标法定量测定饲料中三聚氰胺的方法。饲料用三氯乙酸和乙酸铅溶液提取,再经PCX固相萃取柱净化、BSTFA衍生化,定容后用气相色谱-质谱(GC-MS)测定,并以同位素内标定量。饲料中三聚氰胺的检出限为50μg/kg,三聚氰胺的测定在125～5000ng/mL范围内具有良好的线性关系,配合饲料、浓缩饲料、预混饲料中的平均回收率分别为95.0%、95.6%、94.9%,平均变异系数为2.8%、3.3%、3.7%。通过与外标法比较,该方法定量准确可靠,更加适合用作饲料中三聚氰胺的定量测定。更多还原

【Abstract】 Isotopic internal standard and gas chromatography-mass spectrometric(GC-MS)method has been established for the detection of melamine in animal feed. Extracted with the solution of trichloroacetic acid and lead acetate,the samples were cleaned by PCX SPE columns, derived with BSTFA and dissolved,before detected by GC-MS and isotopic internal standard method. The limit of detection(LOD)of melamine in feed was 50 μg/kg,and the linearity of melamine was within the range of 125~5 000 ng/mL. The mean recovery of melamine in formula feed,concentrated feed and premix was 95.0%,95.6% and 94.9%,and the mean RSD was 2.8%,3.3% and 3.7%,respectively. Compared with the external standard method,this method was accurate and reliable in quantification,and it was more propitious to be used for the quantitative determination of melamine in feed.更多还原