碳膜电位器河北大学
硕士学位论文
食品中某些有害物质的GC/MS和高效毛细管电泳检测新方法tsf过载保护
姓名：***
申请学位级别：硕士
专业：分析化学
指导教师：***
20100501
摘要
摘要
盲源分离
随着谱技术的不断发展，谱在食品分析中的应用越来越广泛。本文首先对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1mg/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:10µg/kg，苯醚甲环唑在0.01mg/L-2.5mg/L(10µg/kg-250µg/kg)范围内符合线性关系，相关系数大于0.99。玻璃加工工艺
第四章采用气相谱-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-0.2mg/L(10µg/kg-200µg/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R>0.99，平均回收率在76.83%-91.35%之间。
关键词气相谱-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
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 chapter2,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 from83.2%to97.5%in the spiked range of the determination of melamine in milk and milk powder.The limit of quantification (LOQs)of milk and milk powder was1.0mg/kg,and the relative standard deviations were between 2.1%and 3.9%(n=5).The sensitivity of the method is similar to the high-performance liquid chromatography,and the sample pre-treatment is more simple, specific,reproducible,economic,environment.So it can be used for a large number of samples of milk and milk powder’s melamine rapid detection.
热再生
In chapter3,a new method of the determination of difenoconazole in Vegetable by GC-MS/MS was d
生态砖eveloped.The difenoconazole in sample was extracted with acetonitrile. The extract was purified and concentrated with solid phase extraction column,then detected by GC-MS/MS in the multiple reaction monitoring mode.The average recoveries ranged from78.82%to94.64%,The limit of quantification(LOQs)was10µg/kg,The calibration curve was linear between0.01mg/L and0.25mg/L(10µg/kg-250µg/kg),and the correlation coefficient was more than0.99.
In chapter4,a novel method of simultaneous differmination of amitraz and chlordimeform in honey by GC-MS/MS was investigated.The amitraz and chlordimeform in sample were extracted with mixture of acetone and n-hexane,the extract was purified and concentrated, then detected by GC-MS/MS.The calibration curve was linear of amitraz,chlordimeform and 2,4-xylidine between0.01mg/L and0.2mg/L(10µg/kg-200µg/kg),and the correlation coefficient was more than0.990.The average recovery was ranged from76.83%-91.35%.
Key words GC/MS HPCE Melamine Difenoconazole Amitraz Chlordimeform 2,4-Dimethylaniline
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