食品中某些有害物质的GCMS和高效毛细管电泳检测新方式.pdfVIP

摘 要 摘 要 随着色谱技术的不断发展，色谱在食品分析中的应用越来越广泛。本文首先对色谱 在食品分析中的应用进行了介绍，主要包括GC/MS和高效毛细管电色谱在食品安全分析 中的应用。 第二章建立了高效毛细管电泳(HPCE)浊度法检测牛奶和奶粉中三聚氰胺的方法。样 品中加入三氯乙酸水溶液，加热样品至沸腾后自然冷却，使蛋白质充分凝聚、沉降，并 提取三聚氰胺。添加回收率在83% - 98%之间，相对标准偏差为1.8% - 3.4%(n=5) 。定量 限为1 mg/kg 。样品的前处理步骤简单、过程易于控制，浊度法特异性强、重现性好， 灵敏度与高效液相色谱法相近。方法经济环保，可用于大量牛奶和奶粉样品中三聚氰胺 的快速检测。 第三章建立了气相色谱- 串联质谱法(GC-MS/MS)测定果蔬中苯醚甲环唑残留量分 析方法。试样中残留的苯醚甲环唑用乙腈提取，提取液经固相萃取柱净化后，以 GC-MS/MS在多反应监测模式测定。方法回收率在78.82% - 94.64%之间，测定低限为:10 µg/kg ，苯醚甲环唑在0.01 mg/L - 2.5 mg/L(10 µg/kg - 250 µg/kg)范围内符合线性关系，相 关系数大于0.99 。 第四章采用气相色谱- 串联质谱法(GC-MS/MS) 同时测定蜂蜜中的杀虫脒和双甲脒 的含量。用丙酮和正己烷的混合液提取样品中的杀虫脒和双甲脒，净化后检测，在0.010 mg/L - 0.2 mg/L(10µg/kg - 200 µg/kg)范围内，杀虫脒、双甲脒及其代谢物2 ，4-二甲基苯 胺均符合线性关系，线性相关系数R0.99，平均回收率在76.83%-91.35%之间。 关键词 气相色谱- 串联质谱 高效毛细管电泳 三聚氰胺 苯醚甲环唑 杀虫脒 双 甲脒 2 ，4-二甲基苯胺 I Abstract Abstract In recent years the chromatography develops rapidly, and it has been used widely. In the paper, the application of chromatography in food safety analysis has been reviewed, including application of GC/MS and HPCE in food analysis. In chapter 2, a novel method of high performance capillary electrophoresis (HPCE) has been established for the separation of melamine in milk and milk powder. Trichloroacetic acid solution was used to precipitate proteins and to dissociate the melamine from the sample matrix. In order to dissociate the proteins clean and simply, the sample was heated to boil, then cooled naturally. The average recoveries ranged from 83.2% to 97.5% in the spiked range of the determination of melamine in milk and milk powder. The limit of quantification (LOQs) of milk and milk powder was 1.0 mg/kg, and the relative standard deviations were between 2.1% and 3.9% (