水产品中药物残留检测的前处理方法研究

发布时间：2018-04-09 00:37

本文选题：水产品　切入点：四环素类　出处：《福州大学》2014年硕士论文

【摘要】：食品安全问题已经成为全球关注的热点问题,主要是由农药残留、兽药残留、重金属、饲料添加剂、污染物质以及其他危害人体健康的物质引起的。水产品中抗生素残留备受关注,由于水产品质量安全事件频繁发生,因此建立操作简单,快速简便的检测监控体系具有重要的意义。本论文主要针对水产品中几类常见的药物残留,分别建立了可行有效的提取、净化、富集的前处理方法,并应用液相色谱串联质谱法(HPLC-MS-MS)技术检测其药物残留。论文共分为四章：第一章,绪论。主要介绍了水产品中的药物残留,水产品中的抗生素,样品前处理技术以及分析检测方法,同时介绍了本论文的研究目的和研究内容。第二章,鳗鱼中四环素类药物前处理方法的研究。以四种四环素类药物作为目标分析物,主要优化了该方法的提取剂、提取剂的pH、固相萃取柱(SPE)吸附性填料、填料量的选择、固相萃取柱洗脱剂的选择、以及在不同比例下合成土霉素分子印迹聚合物等条件对目标物分离状况的影响。在最优条件下,4种目标物在50-250μg/L浓度范围内线性关系较好,相关系数在0.9947～0.9994。土霉素、四环素、金霉素的检测限为10.0 μg/kg,强力霉素的检测限为5.0 μg/kg。第三章,鳗鱼中喹诺酮类药物前处理方法的研究。主要研究了鳗鱼中喹诺酮类药物的前处理方法,优化了该方法的提取剂,选择吸附性填料和氧氟沙星分子印迹聚合物(OFLMIP)为固相萃取柱,对样品液进行富集和净化。商品化的固相萃取柱可以富集和净化11种喹诺酮类药物,回收率低；本论文中合成的分子印迹聚合物填充的OFLMIP固相萃取柱可以净化6种喹诺酮类药物,回收率较高。FLU、OFL、ENR、DIF、OXA、NAA的检测限为2μg/kg, NOR、ORB、SPA、 SAR、PEF的检测限为5μg/kg。第四章,鳗鱼中硝基呋喃类药物代谢物前处理方法的研究。主要研究了一种快速衍生硝基呋喃类代谢物的方法,优化了硝基呋喃代谢物的衍生时间和衍生温度,选择最佳的提取剂,用固相萃取柱进行富集和净化,最后采用HPLC-MS-MS技术检测。结果表明,以三个水平进行样品加标回收率实验,平均回收率范围在79.50～108.13%,相对标准偏差在1.10～6.79%,AOZ、SEM、AMOZ、AHD的检测限分别为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 卤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.
【学位授予单位】：福州大学
【学位级别】：硕士
【学位授予年份】：2014
【分类号】：R155.5

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