本文選題：水產(chǎn)品　切入點：四環(huán)素類　出處：《福州大學》2014年碩士論文

【摘要】：食品安全問題已經(jīng)成為全球關(guān)注的熱點問題,主要是由農(nóng)藥殘留、獸藥殘留、重金屬、飼料添加劑、污染物質(zhì)以及其他危害人體健康的物質(zhì)引起的。水產(chǎn)品中抗生素殘留備受關(guān)注,由于水產(chǎn)品質(zhì)量安全事件頻繁發(fā)生,因此建立操作簡單,快速簡便的檢測監(jiān)控體系具有重要的意義。本論文主要針對水產(chǎn)品中幾類常見的藥物殘留,分別建立了可行有效的提取、凈化、富集的前處理方法,并應(yīng)用液相色譜串聯(lián)質(zhì)譜法(HPLC-MS-MS)技術(shù)檢測其藥物殘留。論文共分為四章：第一章,緒論。主要介紹了水產(chǎn)品中的藥物殘留,水產(chǎn)品中的抗生素,樣品前處理技術(shù)以及分析檢測方法,同時介紹了本論文的研究目的和研究內(nèi)容。第二章,鰻魚中四環(huán)素類藥物前處理方法的研究。以四種四環(huán)素類藥物作為目標分析物,主要優(yōu)化了該方法的提取劑、提取劑的pH、固相萃取柱(SPE)吸附性填料、填料量的選擇、固相萃取柱洗脫劑的選擇、以及在不同比例下合成土霉素分子印跡聚合物等條件對目標物分離狀況的影響。在最優(yōu)條件下,4種目標物在50-250μg/L濃度范圍內(nèi)線性關(guān)系較好,相關(guān)系數(shù)在0.9947～0.9994。土霉素、四環(huán)素、金霉素的檢測限為10.0 μg/kg,強力霉素的檢測限為5.0 μg/kg。第三章,鰻魚中喹諾酮類藥物前處理方法的研究。主要研究了鰻魚中喹諾酮類藥物的前處理方法,優(yōu)化了該方法的提取劑,選擇吸附性填料和氧氟沙星分子印跡聚合物(OFLMIP)為固相萃取柱,對樣品液進行富集和凈化。商品化的固相萃取柱可以富集和凈化11種喹諾酮類藥物,回收率低；本論文中合成的分子印跡聚合物填充的OFLMIP固相萃取柱可以凈化6種喹諾酮類藥物,回收率較高。FLU、OFL、ENR、DIF、OXA、NAA的檢測限為2μg/kg, NOR、ORB、SPA、 SAR、PEF的檢測限為5μg/kg。第四章,鰻魚中硝基呋喃類藥物代謝物前處理方法的研究。主要研究了一種快速衍生硝基呋喃類代謝物的方法,優(yōu)化了硝基呋喃代謝物的衍生時間和衍生溫度,選擇最佳的提取劑,用固相萃取柱進行富集和凈化,最后采用HPLC-MS-MS技術(shù)檢測。結(jié)果表明,以三個水平進行樣品加標回收率實驗,平均回收率范圍在79.50～108.13%,相對標準偏差在1.10～6.79%,AOZ、SEM、AMOZ、AHD的檢測限分別為0.1 μg/kg.0.5 μg/kg.0.2 μg/kg.0.5μg/kgo
[Abstract]:Food safety has become a global hot issue, mainly caused by pesticide residues, veterinary drug residues, heavy metals, feed additives, pollutants and other substances harmful to human health.Antibiotic residues in aquatic products are of great concern. Because of the frequent occurrence of aquatic product quality and safety incidents, it is of great significance to establish a simple, rapid and simple detection and monitoring system.In this paper, a feasible and effective method of extraction, purification and enrichment was established for several kinds of common drug residues in aquatic products. HPLC-MS-MSM was used to detect the drug residues in aquatic products.The thesis is divided into four chapters: chapter one, introduction.This paper mainly introduces the drug residues in aquatic products, antibiotics in aquatic products, sample pretreatment techniques and analytical methods, and introduces the purpose and content of this paper.In the second chapter, the pretreatment method of tetracycline drugs in eel was studied.With four tetracycline drugs as the target analyte, the extraction agent, the pH of extraction agent, the adsorptive filler of SPE, the selection of packing amount and the selection of eluant for solid phase extraction column were optimized.The effects of the conditions such as the synthesis of oxytetracycline molecularly imprinted polymer at different ratios on the separation of the target materials were investigated.Under the optimum conditions, the linear range of the four target compounds is 50-250 渭 g / L, and the correlation coefficient is 0.9947 ~ 0.9994.The detection limit of oxytetracycline, tetracycline and chlortetracycline was 10.0 渭 g / kg, and that of doxycycline was 5.0 渭 g / kg.In the third chapter, the pretreatment method of quinolones in eel was studied.The pretreatment method of quinolones in eel was studied. The extraction agent of the method was optimized. The absorbent filler and ofloxacin molecularly imprinted polymer (OFLMIP) were selected as solid phase extraction column to enrich and purify the sample liquid.The commercial solid phase extraction column can enrich and purify 11 quinolones, and the recovery rate is low. The OFLMIP solid-phase extraction column filled with molecularly imprinted polymer can purify 6 quinolones.The detection limit of OXANAA was 2 渭 g / kg, the detection limit of ORBX SPAA and PEF was 5 渭 g / kg.In chapter 4, the pretreatment method of nitrofuran metabolites in eel was studied.A method of fast derivatization of nitrofuran metabolites was studied in this paper. The derivative time and temperature of nitrofuran metabolites were optimized, the optimum extraction agent was selected, and the solid phase extraction column was used for enrichment and purification. Finally, HPLC-MS-MS technique was used to detect nitrofuran metabolites.The results showed that the average recovery range was 79.50 鹵108.13 and the relative standard deviation was 1.10 ~ 6.79. The detection limit of AMOZ AHD was 0.1 渭 g/kg.0.5 渭 g/kg.0.2 渭 g/kg.0.5 渭 g/kgo, respectively.
【學位授予單位】：福州大學
【學位級別】：碩士
【學位授予年份】：2014
【分類號】：R155.5

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