QuEChERS方法在复杂基质中兽药残留及霉菌毒素分析检测中的应用

发布时间：2019-02-26 18:06

【摘要】：QuEChERS(quick,easy,cheap,effective,rugged and safe)方法自2003年提出以来,被广泛应用于不同基质中有机和无机化合物的分析。该方法最初的研究对象是水果、蔬菜等农产品,基质成分较为简单,采用传统QuEChERS方法即可得到较好的结果。随着QuEChERS方法的不断发展,已有的标准样品前处理方法已不能满足复杂基质(如有机肥、饲料等)的检测要求,故本论文以QuEChERS技术为基础,结合不同的改进方法,对复杂基质进行提取与净化,并结合超高效液相色谱-串联质谱进行分析,具体内容如下:1.阐述了QuEChERS方法的原理、进展及应用;同时简要介绍了兽药与霉菌毒素。2.建立了以QuEChERS方法结合柱净化为前处理手段,结合超高效液相色谱-串联质谱同时测定有机肥中46种抗生素的分析检测方法。考察了4种改进方式对三类抗生素的提取效果的影响,确定了最佳前处理方法。该方法能同时满足三类抗生素的检测要求,并成功应用于实际有机肥样品中兽药残留的测定。3.以氟喹诺酮类抗生素为研究对象,将QuEChERS方法与氟喹诺酮免疫胶体金快速检测试剂板相结合,建立了一种快速筛查有机肥中氟喹诺酮残留阳性样品的分析方法。以QuEChERS方法为依据,对提取溶液种类与pH值、吸附剂种类与用量等因素进行优化,确定了最佳前处理方法。该方法操作简单,耗时较短,不需要特殊仪器,能够现场对样品进行前处理并立即得到结果,为快速筛查氟喹诺酮残留阳性样品提供技术支持。4.建立了QuEChERS结合超高效液相色谱-串联质谱同时测定饲料中13种霉菌毒素的分析方法。将功能化磁性材料应用于QuEChERS方法,通过回收利用,降低了实验成本,并对提取溶剂、磁性吸附剂的种类与用量等因素进行优化,确定了最佳萃取条件。本方法能快速简便的完成前处理过程,并成功运用于实际饲料样品的分析检测,为养殖业饲料的质量控制提供科学依据。
[Abstract]:QuEChERS (quick,easy,cheap,effective,rugged and safe) has been widely used in the analysis of organic and inorganic compounds in different substrates since it was proposed in 2003. The original research object of this method is fruit, vegetable and other agricultural products, the matrix composition is relatively simple, the traditional QuEChERS method can get better results. With the development of QuEChERS method, the existing standard sample pretreatment methods can no longer meet the requirements of complex substrates (such as organic fertilizer, feed, etc.). Therefore, this paper is based on QuEChERS technology and combined with different improved methods. The complex matrix was extracted and purified, and analyzed by ultra-high performance liquid chromatography-tandem mass spectrometry. The main contents are as follows: 1. The principle, development and application of QuEChERS method were described, and the veterinary drugs and mycotoxins were briefly introduced. A method was developed for the simultaneous determination of 46 antibiotics in organic fertilizer by QuEChERS method combined with column purification and ultra-high performance liquid chromatography-tandem mass spectrometry (ultra-high performance liquid chromatography-tandem mass spectrometry). The effects of four improved methods on the extraction efficiency of three kinds of antibiotics were investigated, and the optimal pretreatment method was determined. This method can meet the requirements of three kinds of antibiotics at the same time, and has been successfully applied to the determination of veterinary drug residues in practical organic fertilizer samples. 3. A rapid screening method of fluoroquinolone residue positive samples in organic fertilizer was established by combining the QuEChERS method with fluoroquinolone immunogold rapid detection reagent plate with fluoroquinolone antibiotics as the object of study. The method of rapid detection of fluoroquinolone residues in organic fertilizer was established by combining fluoroquinolone assay with fluoroquinolone immunogold assay. Based on the QuEChERS method, the optimum pretreatment method was determined by optimizing the factors such as the kinds and pH value of extraction solution, the type and dosage of adsorbents and so on. This method has the advantages of simple operation, short time consuming and no special instrument. It can pre-process the samples on the spot and get the results immediately. It can provide technical support for rapid screening of fluoroquinolone residue positive samples. 4. A method for simultaneous determination of 13 mycotoxins in feed by QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry was established. The functionalized magnetic material was applied to QuEChERS method. The experimental cost was reduced by recovery and utilization. The optimum extraction conditions were determined by optimizing the extraction solvent, the type and dosage of magnetic adsorbents, and so on. This method can be used in the analysis and detection of feed samples and provide scientific basis for the quality control of feed in breeding industry. The method can be used to finish the pre-treatment process quickly and simply and successfully applied to the analysis and detection of actual feed samples.
【学位授予单位】：浙江工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TS207.5;O657.63

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