新型样品前处理技术与液相色谱联用检测农药残留及环境污染物的研究

发布时间：2018-05-28 18:51

本文选题：高效液相色谱 + 金属有机骨架　；参考：《曲阜师范大学》2017年硕士论文

【摘要】：长期以来,食品和环境污染物的存在对人类的健康有着巨大的威胁,其来源广泛,成分复杂多样。长期暴露于这些污染物,即使含量较低,也可能经过人体长期蓄积而引起细胞及组织代谢异常,造成人体免疫功能下降,从而导致各种机能障碍,还有可能诱发肿瘤。因此,开发高效、灵敏的检测方法对食品和环境污染物进行快速检测,对于保护环境以及维护人类健康显得十分重要。为了得到更加准确的分析测定结果,进行仪器分析之前,通常需要选择适当的样品前处理技术,对痕量组分进行萃取分离富集。本文主要研究了几种新型样品前处理方法在污染物萃取方面的应用,并结合高效液相色谱对几类食品及环境污染物进行了检测。主要研究内容如下:第一章:综述了高效液相色谱技术以及金属有机骨架材料的特点,合成方法及相关应用。第二章:采用分散液液微萃取对氯代苯氧酸除草剂进行萃取,并用2-(11H-苯并[a]咔唑-11-基)-乙基-4-甲基苯磺酸(BCETS)衍生试剂对待测物进行标记,结合HPLC-FLD对其进行检测。通过对萃取条件及衍生条件的优化,该方法成功应用于农作物中8种氯代苯氧酸类除草剂的检测。第三章:成功合成了UiO-67金属有机骨架材料,将其作为分散固相萃取吸附剂对几种植物生长调节剂进行萃取富集,并用荧光衍生试剂对待测物进行标记,通过质谱鉴定解释了该类衍生反应的原理,通过对衍生条件以及萃取条件的优化,实现了水果中植物生长调节剂的高灵敏检测。第四章:成功合成了具有大尺寸孔径的JUC-48金属有机骨架材料,通过XRD,扫描电子显微镜鉴定了其结构。利用材料的大尺寸孔径,高比面积的特点将其应用于多环芳烃的富集,结合高效液相色谱分析,建立了多环芳烃的灵敏检测方法,在最优条件下,该方法成功检测了环境水样中7种多环芳烃。第五章:成功地合成了磁性固相微萃取吸附剂Fe_3O_4@JUC-48磁性复合材料,并将其用于磺胺类抗生素的磁固相萃取,该方法操作简单,消耗有机溶剂少,萃取效率高,联合高效液相色谱检测,实现了肉类食品中的6种磺胺类抗生素的高灵敏检测。
[Abstract]:For a long time, the existence of food and environmental pollutants has a great threat to human health. The long-term exposure to these pollutants, even if the content is low, may lead to abnormal metabolism of cells and tissues through long-term accumulation of human body, resulting in the decline of human immune function, resulting in various functional disorders, and may induce tumors. Therefore, it is very important to develop an efficient and sensitive method for the rapid detection of food and environmental pollutants for the protection of the environment and the maintenance of human health. In order to obtain more accurate analytical results, it is usually necessary to select appropriate sample pretreatment techniques for the extraction and enrichment of trace components before instrument analysis. In this paper, the application of several new sample pretreatment methods in pollutant extraction was studied, and several kinds of food and environmental pollutants were detected by high performance liquid chromatography (HPLC). The main contents are as follows: chapter 1: high performance liquid chromatography (HPLC) technology and the characteristics, synthesis methods and applications of organometallic skeleton materials are reviewed. Chapter 2: the chlorophenoxy acid herbicide was extracted by dispersive liquid microextraction and labeled with 2-carbazole (a) carbazole-11-ethyl-4-methylbenzenesulfonic acid (BCETS) derivative reagent. It was determined by HPLC-FLD. The method has been successfully applied to the determination of 8 chlorophenoxy acid herbicides in crops by optimizing the extraction and derivation conditions. Chapter 3: UiO-67 organometallic skeleton materials were successfully synthesized and used as dispersive solid phase extraction adsorbents to extract and enrich several plant growth regulators. The principle of this kind of derivative reaction was explained by mass spectrometry, and the high sensitive detection of plant growth regulator in fruit was realized by optimizing the derivatization conditions and extraction conditions. Chapter 4: the JUC-48 metal-organic skeleton material with large pore size was successfully synthesized and its structure was identified by X-ray diffraction and scanning electron microscope. A sensitive detection method for polycyclic aromatic hydrocarbons (PAHs) was established by using the characteristics of large pore size and high specific area of the materials and the analysis of high performance liquid chromatography (HPLC). Seven polycyclic aromatic hydrocarbons (PAHs) in environmental water samples were successfully determined by this method. Chapter 5: the magnetic solid phase microextraction adsorbent Fe_3O_4@JUC-48 magnetic composite was successfully synthesized and used in the magnetic solid phase extraction of sulfanilamide antibiotics. The method is simple in operation, low in organic solvent consumption and high in extraction efficiency. Six sulfonamides antibiotics in meat food were detected by high performance liquid chromatography (HPLC).
【学位授予单位】：曲阜师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.72;TS207.53;X830

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