本文選題：喹VA啉-2-羧酸 + 3-甲基喹VA啉-2-羧酸�。� 參考：《天津科技大學》2012年碩士論文

【摘要】：喹VA啉類是人工合成的動物抗菌促生長藥物,其中喹乙醇(OLA)和卡巴氧(CBX)(?)應用最廣的品種,在動物基體中的殘留標識物分別為3-甲基喹VA(?)羧酸(MQCA)和喹嗯啉-2-羧酸(QCA)。 本論文首先合成MQCA,然后以MQCA為模板分子,活化硅球為表面載體,3-氨基丙基三乙氧基硅烷(APTES)為功能單體,四乙氧基硅烷(TEOS)為交聯(lián)劑,采用表面分子印跡和溶膠-凝膠相結合的技術制備了MQCA分子印跡聚合物。通過紅外光譜和吸附試驗對聚合物進行了表征,吸附試驗結果表明聚合物傳質速度快、吸附容量大對QCA和MQCA均有高選擇性。 以此聚合物為固相萃取吸附材料,建立了動物源性食品中QCA和MQCA戈留的在線固相萃取與高效液相色譜儀聯(lián)用檢測方法,并對影響測定結果的上樣溶劑配比,pH值,上樣速度及洗脫時間等主要實驗參數(shù)進行了優(yōu)化。在上樣流速為2.0mL min-1、上樣體積為50mL條件下,對1.0μg L-1QCA和MQCA勺混合標準溶液(pH5.0,甲醇含量1%)進行富集,富集倍數(shù)分別達到1349和1046；九次重復測定的相對標準偏差(RSD,%)小于8%；檢出限(S/N=3)分別為0.8和2.0ng L-1；線性范圍(r20.99)分別為0.03-40μg L-1和0.04-40μg L-1。 同時對豬肉樣品中的痕量QCA和MQCA進行了檢測分析。樣品前處理方法簡單,酸性水解液釋放待分析物后僅用一步乙腈提取就能滿足測定要求,不需要進步的樣品凈化。通過對檢測為空白的新鮮樣品進行濃度為2.0ng g-1,4.0ng g-1,8.0ng g-1的添加,以所建立的分析方法進行富集測定,結果在三個添加濃度下樣品中QCA和MQCA的回收率為67%-80%,從而證明了所建立檢測方法的可行性。
[Abstract]:Quinavalin is a synthetic antibacterial and growth-promoting drug in animals, in which quindoquindox (Ola) and carbamoxime (CBX) (?) The residues in animal matrix of the most widely used species are 3-methylquine VA (?) Carboxylic acid (MQCA) and quinoline-2-carboxylic acid (QCA). In this thesis, MQCA was synthesized firstly, and then the activated silica spheres were used as the surface support, and tetraethoxy silane (TEOS) as crosslinking agent. MQCA molecularly imprinted polymers were prepared by surface molecular imprinting and sol-gel techniques. The polymer was characterized by infrared spectroscopy and adsorption test. The results showed that the mass transfer rate of the polymer was fast and the adsorption capacity was high selectivity to both QCA and MQCA. Using this polymer as solid phase extraction adsorption material, an on-line solid-phase extraction (SPE) and high performance liquid chromatography (HPLC) method for the determination of QCA and MQCA-Goru in animal-derived food was established. The main experimental parameters such as sample rate and elution time were optimized. The mixed standard solution of 1.0 渭 g L-1QCA and MQCA (pH 5.0, methanol content 1%) was enriched at a flow rate of 2.0 mL min-1 and a volume of 50 mL. The enrichment times were 1349 and 1046, respectively, and the relative standard deviation (RSD) of nine times repeated determination was less than 8%. The detection limit (S / N ~ (3) was 0. 8 and 2.0ng L ~ (-1), the linear range (r _ (20.99) was 0.03-40 渭 g / L ~ (-1) and 0.04-40 渭 g / L ~ (-1), respectively. At the same time, trace QCA and MQCA in pork samples were analyzed. The method of sample pretreatment is simple. After the acid hydrolysate releases the analyte, only one step acetonitrile can be extracted to meet the determination requirements, and no progressive sample purification is needed. The fresh samples with blank detection were enriched and determined by adding 4.0 ng / g ~ (-1) 2.0ng g ~ (-1) or 8.0 ng / g ~ (-1) to 2.0ng g ~ (-1). Results the recoveries of QCA and MQCA in the samples were 67-80, which proved the feasibility of the established method.
【學位授予單位】：天津科技大學
【學位級別】：碩士
【學位授予年份】：2012
【分類號】：R318.08

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