ASE法提取饲料中三聚氰胺的研究进展

论文编号:SW054  论文字数:10289,页数:27

摘要：三聚氰胺是一种三嗪类含氮杂环有机化合物。 由于其较高的含氮量而被添加于食品和饲料中充当蛋白质含量，对动物和人体造成了一定的危害。本文阐诉了使用ASE快速萃取技术来提取饲料中的三聚氰胺，并与超声波提取法做比较，最后使用气相色谱-质谱联用（GC-MS）检测法检测比较结果。本方法从浓度1.25µg/ml到20.0µg/ml范围内线性关系良好，线性方程为y=490514x+19766，相关系数R=0.9994，检测限为0.05 mg/kg，通过空白样品饲料外标法加标，回收率为96%。采用本方法对含有三聚氰胺的阳性样品进行4次平行检测，测定结果为19.50 mg/kg，RSD为2.68 %，采用超声波法-GC/MS法进行同一样品的4次平行检测，平均值为14.65mg/kg，RSD为2.79 %。ASE法萃取效率明显优于超声萃取法。
关键词：三聚氰胺；快速溶剂萃取（ASE）；饲料；气相色谱质谱

The research progress of determination the melamine in feed by ASE method
Abstract：Melamine is a nitrogen-containing heterocyclic triazine compounds. .Due to its rich in nitrogen, it has been added to give a false impression of high protein content. Melamine added to food and animal feeds could possibly cause fatal kidney stones. Determination of melamine is therefore of large importance to ensure food safety. This article reviewed a new method of ASE v. rapid extraction technology to extract the melamine in feed and sediments of different conditions and with the conventional method of extraction methods for comparison, the last use of GC-MS assay test results of the comparison. A standard curve was obtained and the regression equation was y=490514x+19766,correlation coefficient R=0.9994,the detection limit was 0.05 mg/kg,the recoveries of feed blank sample were 96% by external standard calibration.Using this method to detect melamine-positive samples for four times in parallel,measurement results were 19.50 mg/kg, RSD was 2.68 %.Using the method of Ultrasonic extraction-GC/MS to detect the same melamine-positive samples for four times in parallel,measurement results were 14.65 mg/kg, RSD was 2.79 %.The extraction efficiency of ASE method obtained was better than Ultrasonic extraction.
Keywords: melamine; accelerated solvent extraction; feed; GC/MS

目  录
中文摘要 I
英文摘要 II
目录 III
1. 绪论 1
 1.1  引言 1
 1.2  三聚氰胺的性质与毒性 1
 1.3  饲料中三聚氰胺的来源 2
 1.4  三聚氰胺的前处理 3
 1.5  饲料中三聚氰胺的分析方法 3
 2. 实验部分 6
 2.1 试剂与仪器 6
 2.2 材料 7
 2.3 方法 7
 2.4 ASE的提取条件确定 8
 2.5 色谱条件 8
 2.6 标准曲线的绘制 8
 2.7 加标回收 9
 2.8 ASE法与超声波法比较 9
 2.9 结果计算 9
 2.10 本章小结 9
3. 结果与讨论 10
 3.1 ASE的提取条件 10
 3.2 色谱条件的优化 13
 3.3 方法线性 14
 3.4 ASE萃取法优于超声波法的原因分析 17
 3.5 本章小结 17
4．总结与展望 19
 4.1 ASE法提取饲料中三聚氰胺的建立 19
 4.2 ASE法提取饲料中三聚氰胺的操作要点 19
 4.3 饲料中三聚氰胺的含量测定及意义 19
 4.4 问题及展望 19
致谢 21
参考文献 22