气相色谱—质谱联用技术测定食品中邻苯二甲酸酯类的研究

发布时间：2018-05-06 22:12

本文选题：邻苯二甲酸酯 + 气相色谱-质谱联用仪　；参考：《河南大学》2013年硕士论文

【摘要】：邻苯二甲酸酯类化合物是一类重要的增塑剂，被广泛用于塑料制品的生产，在其他邻域也有应用，，例如化妆品、香精等的生产。邻苯二甲酸酯也是环境激素的一种，而环境激素是一类可以对人体产生有害影响的物质。随着塑料制品的大量使用使环境中的邻苯二甲酸酯含量不断增加，而环境中的邻苯二甲酸酯也会迁移进入食物，进而进入人体，危害人体健康。虽然，邻苯二甲酸酯有降解途径，但其降解非常缓慢，因而，减少塑料制品使用的同时，建立快速、准确、安全的测定分析法是很必要和必须的。本文选定被广泛关注的16种邻苯二甲酸酯类增塑剂（邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二异丁酯（DIBP）、邻苯二甲酸二丁酯（DBP）、邻苯二甲酸（2-甲氧基）乙酯（BMEP）、邻苯二甲酸二（4-甲基-2-戊基）（BMPP）、邻苯二甲酸二（2-乙氧基）乙酯（BEEP）、邻苯二甲酸二戊酯（DPP）、邻苯二甲酸二己酯（DHXP）、邻苯二甲酸丁基苄基酯（BBP）、邻苯二甲酸己酯2-乙基己基酯（HEP）、邻苯二甲酸二（2-丁氧基）乙酯（BnBP）、邻苯二甲酸二环己酯（DCHP）、邻苯二甲酸二（2-乙基）己酯（DEHP）、邻苯二甲酸二丁正辛酯（DOP）和邻苯二甲酸二壬酯（DNP））作为研究对象，选择DB-5MS毛细管色谱柱，确定进样口温度，选择离子检测（SIM）定性，使用气相色谱-质谱联用仪（GC-MS）进行分析，经过试验系统研究并建立了16种邻苯二甲酸酯类污染物的分析方法，确定了线性范围、线性相关性以及最低检出限，很好地满足了分析检测邻苯二甲酸酯类化合物的需要。以食用油、液态奶、叶类蔬菜为材料，优化了前处理方法。食用油经乙腈提取SILICA/PSA玻璃混合型固相萃取柱净化，回收率在80.0%～105.0%，相对标准偏差（n=6）在2.7%～5.7%之间，结果表明该分析方法准确度、精密度良好；液态奶和叶类蔬菜分别进行了不同有机溶剂提取试验，确定提取溶剂正己烷、乙醚、乙腈的提取比例。结果表明邻苯二甲酸酯类化合物在液态奶中的回收率为80.0%～104.0%，相对标准偏差（n=6）为2.1%～5.1%，叶类蔬菜样品中的回收率为75.4%～110.6%，相对标准偏差（n=6）为3.8%～12.4%。
[Abstract]:Phthalic acid esters are important plasticizers, which are widely used in the production of plastic products, and are also used in other neighborhoods, such as cosmetics, flavor and so on. Phthalate is also a kind of environmental hormone, which can have harmful effects on human body. With the extensive use of plastic products, the content of phthalate in the environment is increasing, and the phthalate in the environment will migrate into food, and then into the human body, which is harmful to human health. Although phthalate has a degradation pathway, its degradation is very slow. Therefore, it is necessary and necessary to establish a rapid, accurate and safe analytical method while reducing the use of plastic products. In this paper, 16 kinds of phthalate plasticizers (dimethyl phthalate, diethyl phthalate, diisobutyl phthalate, dibutyl phthalate, dimethoxy phthalate, dimethyl phthalate, diethyl phthalate, diisobutyl phthalate, dibutyl phthalate, dimethoxy phthalate) have been selected. BMEPN, Ding Ji benzyl phthalate, 2-ethylhexyl phthalate, dimethyl phthalate 2-ethoxy, dipentyl phthalate, dihexyl phthalate, Ding Ji benzyl phthalate, 2-ethylhexyl phthalate, benzyl phthalate, 2-ethylhexane phthalate, dipentyl phthalate, dihexyl phthalate, benzyl phthalate, hexyl phthalate, diethyl hexane phthalate, dipentyl phthalate, dihexyl phthalate. Hep, BnBPN, DCHPU, DEHPN, DOP) and DNPN) were used as the research objects, and the results were as follows: (1) Ester (Hep), (dibutoxy phthalate) ethyl (BnBPN), DHPX (dicyclohexyl phthalate), (dibutylhexyl phthalate) (DOP) and DNPN (DNPN) were used as the objects of the study. The DB-5MS capillary column was selected, the injection temperature was determined, and the qualitative analysis was carried out by ion detection (Simm). The analytical method of 16 phthalate esters was established by gas chromatography-mass spectrometry (GC-MS). The linear range, the linear correlation and the minimum detection limit were determined, which satisfied the needs of analysis and detection of phthalates. Using edible oil, liquid milk and leafy vegetables as materials, the pretreatment method was optimized. The purification of edible oil by acetonitrile SILICA/PSA glass mixed solid phase extraction column showed that the recovery rate was 80. 0% and the relative standard deviation was 2. 757%. The results showed that the method was accurate and accurate. The extraction ratio of n-hexane, ether and acetonitrile in liquid milk and leaf vegetables were determined by different organic solvents. The results showed that the recovery rate of phthalates in liquid milk was 80. 0 and 10. 0, and the relative standard deviation was 2. 1 and 5. 1. The recovery rate in leaf vegetables was 75. 4% and 110.6, and the relative standard deviation was 3. 8 and 12. 4, respectively.
【学位授予单位】：河南大学
【学位级别】：硕士
【学位授予年份】：2013
【分类号】：O657.63;R155.51

【参考文献】