毛细管电泳测定环境样品和加热食品中丙烯酰胺的研究

发布时间：2018-04-13 15:45

  本文选题：丙烯酰胺 + 毛细管电泳　； 参考：《苏州科技大学》2017年硕士论文

【摘要】：毛细管电泳(Capillary Electrophoresis,CE)以其高效、快速、经济及较低的检出限等优点,被广泛应用于环境、医药、生物等领域。丙烯酰胺是一种极性小分子化合物,由于其具有神经毒性、遗传毒性和致癌性,对人体健康构成潜在威胁。食品加热过程往往产生丙烯酰胺,但目前的研究集中于面制品,对米制品的研究较少,同时污水处理中往往加入含有丙烯酰胺的絮凝剂,因此本文以污泥、水样及米制品中丙烯酰胺为研究对象,建立了基质分散固相萃取-毛细管电泳法提取和测定了米制品、污水和剩余污泥中丙烯酰胺的分析方法并成功应用于实际样品的测定。此外,还用离线衍生毛细管电泳检测米制品和水样中丙烯酰胺。论文主要内容有:第一章:先重点介绍了丙烯酰胺的基本性质、产生机理及检测方法,并对现有方法的优缺点进行了比较,然后对毛细管电泳的基本原理、组成、多种分离模式及毛细管电泳的特点进行了描述。第二章:应用基质分散固相萃取-毛细管电泳法提取和测定了污泥及米制品中丙烯酰胺。优化了色谱条件、分散剂的选择及用量、洗脱剂的选择及用量等参数,最优样品前处理和分离条件为:C18及弗罗里硅土混合作为吸附剂,两者的质量比为1:4,样品与吸附剂质量比为5:9,洗脱液为丙酮:二氯甲烷=6:4(V/V)的混合溶剂,洗脱剂的体积为10 m L;以20 mmol/L硼砂(p H=8.4)做为缓冲溶液,在15 k V恒压下进行分离,所建立的分析方法的线性范围为10~200μg/m L,相关系数为0.9998,丙烯酰胺的检出限为0.62μg/m L(S/N=3),样品中丙烯酰胺的回收率为77.2%~104.2%。该方法测得的污泥、雪饼、锅巴、米老头、小小酥样品的丙烯酰胺含量分别为1.02 mg/kg,8.39 mg/kg,27.3 mg/kg,31.9mg/kg,29.7 mg/kg,RSD为1.36%~6.41%。该方法简便、准确可靠,可用于米制品及污泥样品中丙烯酰胺检测。第三章:离线衍生毛细管电泳检测米制品和水样中丙烯酰胺。考察了丙烯酰胺衍生的条件,最佳条件为:以水超声提取,间巯基苯甲酸作为衍生剂,硼砂作为催化剂,在45℃水浴加热反应5小时,乙酸乙酯萃取。以20 mmol/L硼砂(p H=8.97)做缓冲溶液,在15 k V恒压下进行分离。在优化的条件下,方法的线性范围为10~200μg/m L,相关系数为0.9986,检测限0.21μg/m L(S/N=3)。优化的条件下,测得水样、雪饼、锅巴、米老头、小小酥样品中丙烯酰胺的含量分别0,7.14 mg/kg,24.7 mg/kg,28.3mg/kg,28.9mg/kg。该衍生反应条件温和,峰面积是原相同浓度丙烯酰胺峰面积的5倍,可适用于米制品及水样中丙烯酰胺的检测。
[Abstract]:Capillary ElectrophoresisCe (CE) has been widely used in the fields of environment, medicine, biology and so on because of its high efficiency, rapidity, economy and low detection limit.Acrylamide is a kind of polar small molecular compound. Because of its neurotoxicity, genetic toxicity and carcinogenicity, acrylamide poses a potential threat to human health.Acrylamide is often produced in the process of food heating, but the current research is focused on flour products, and the research on rice products is less. At the same time, the flocculant containing acrylamide is often added to the sewage treatment.Acrylamide in water samples and rice products was studied. A method for the extraction and determination of acrylamide in rice products, sewage and surplus sludge by matrix dispersive solid-phase extraction-capillary electrophoresis was established and successfully applied to the determination of practical samples.In addition, acrylamide in rice products and water samples was determined by off-line capillary electrophoresis.The main contents of this paper are as follows: in Chapter 1, the basic properties, mechanism of acrylamide production and detection methods are introduced, and the advantages and disadvantages of the existing methods are compared, and then the basic principle and composition of capillary electrophoresis are discussed.Several separation modes and the characteristics of capillary electrophoresis were described.Chapter 2: acrylamide in sludge and rice products was extracted and determined by matrix dispersive solid phase extraction-capillary electrophoresis.The chromatographic conditions, the selection and dosage of dispersant, the selection and dosage of eluent were optimized. The optimum conditions of sample pretreatment and separation were as follows: 1. C18 and Florisil were mixed as adsorbents.The mass ratio of the two is 1: 4, the mass ratio of sample to adsorbent is 5: 9, the eluant is acetone: dichloromethane 6: 4 V / V), the volume of eluant is 10 mL, the buffer solution is 20 mmol/L borax, and the separation is carried out under the constant pressure of 15 kV.The linear range of the method is 10 ~ 200 渭 g / mL, the correlation coefficient is 0.9998, the detection limit of acrylamide is 0.62 渭 g / m ~ (-1) N ~ (-1) N ~ (3 +), and the recovery rate of acrylamide is 77.2% ~ 104.2%.The method is simple, accurate and reliable, and can be used for the determination of acrylamide in rice products and sludge samples.Chapter 3: determination of acrylamide in rice products and water samples by off-line capillary electrophoresis.The optimum conditions of acrylamide derivatization were as follows: extraction with water ultrasonic, m-mercaptobenzoic acid as derivative, borax as catalyst, heating reaction at 45 鈩，

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