本文選題：丙烯酰胺 + 毛細(xì)管電泳　； 參考：《蘇州科技大學(xué)》2017年碩士論文

【摘要】：毛細(xì)管電泳(Capillary Electrophoresis,CE)以其高效、快速、經(jīng)濟(jì)及較低的檢出限等優(yōu)點,被廣泛應(yīng)用于環(huán)境、醫(yī)藥、生物等領(lǐng)域。丙烯酰胺是一種極性小分子化合物,由于其具有神經(jīng)毒性、遺傳毒性和致癌性,對人體健康構(gòu)成潛在威脅。食品加熱過程往往產(chǎn)生丙烯酰胺,但目前的研究集中于面制品,對米制品的研究較少,同時污水處理中往往加入含有丙烯酰胺的絮凝劑,因此本文以污泥、水樣及米制品中丙烯酰胺為研究對象,建立了基質(zhì)分散固相萃取-毛細(xì)管電泳法提取和測定了米制品、污水和剩余污泥中丙烯酰胺的分析方法并成功應(yīng)用于實際樣品的測定。此外,還用離線衍生毛細(xì)管電泳檢測米制品和水樣中丙烯酰胺。論文主要內(nèi)容有:第一章:先重點介紹了丙烯酰胺的基本性質(zhì)、產(chǎn)生機(jī)理及檢測方法,并對現(xiàn)有方法的優(yōu)缺點進(jìn)行了比較,然后對毛細(xì)管電泳的基本原理、組成、多種分離模式及毛細(xì)管電泳的特點進(jìn)行了描述。第二章:應(yīng)用基質(zhì)分散固相萃取-毛細(xì)管電泳法提取和測定了污泥及米制品中丙烯酰胺。優(yōu)化了色譜條件、分散劑的選擇及用量、洗脫劑的選擇及用量等參數(shù),最優(yōu)樣品前處理和分離條件為:C18及弗羅里硅土混合作為吸附劑,兩者的質(zhì)量比為1:4,樣品與吸附劑質(zhì)量比為5:9,洗脫液為丙酮:二氯甲烷=6:4(V/V)的混合溶劑,洗脫劑的體積為10 m L;以20 mmol/L硼砂(p H=8.4)做為緩沖溶液,在15 k V恒壓下進(jìn)行分離,所建立的分析方法的線性范圍為10~200μg/m L,相關(guān)系數(shù)為0.9998,丙烯酰胺的檢出限為0.62μg/m L(S/N=3),樣品中丙烯酰胺的回收率為77.2%~104.2%。該方法測得的污泥、雪餅、鍋巴、米老頭、小小酥樣品的丙烯酰胺含量分別為1.02 mg/kg,8.39 mg/kg,27.3 mg/kg,31.9mg/kg,29.7 mg/kg,RSD為1.36%~6.41%。該方法簡便、準(zhǔn)確可靠,可用于米制品及污泥樣品中丙烯酰胺檢測。第三章:離線衍生毛細(xì)管電泳檢測米制品和水樣中丙烯酰胺�？疾炝吮０费苌臈l件,最佳條件為:以水超聲提取,間巰基苯甲酸作為衍生劑,硼砂作為催化劑,在45℃水浴加熱反應(yīng)5小時,乙酸乙酯萃取。以20 mmol/L硼砂(p H=8.97)做緩沖溶液,在15 k V恒壓下進(jìn)行分離。在優(yōu)化的條件下,方法的線性范圍為10~200μg/m L,相關(guān)系數(shù)為0.9986,檢測限0.21μg/m L(S/N=3)。優(yōu)化的條件下,測得水樣、雪餅、鍋巴、米老頭、小小酥樣品中丙烯酰胺的含量分別0,7.14 mg/kg,24.7 mg/kg,28.3mg/kg,28.9mg/kg。該衍生反應(yīng)條件溫和,峰面積是原相同濃度丙烯酰胺峰面積的5倍,可適用于米制品及水樣中丙烯酰胺的檢測。
[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，

本文編號：1745147