【摘要】：QuEChERS(quick,easy,cheap,effective,rugged and safe)方法自2003年提出以來(lái),被廣泛應(yīng)用于不同基質(zhì)中有機(jī)和無(wú)機(jī)化合物的分析。該方法最初的研究對(duì)象是水果、蔬菜等農(nóng)產(chǎn)品,基質(zhì)成分較為簡(jiǎn)單,采用傳統(tǒng)QuEChERS方法即可得到較好的結(jié)果。隨著QuEChERS方法的不斷發(fā)展,已有的標(biāo)準(zhǔn)樣品前處理方法已不能滿足復(fù)雜基質(zhì)(如有機(jī)肥、飼料等)的檢測(cè)要求,故本論文以QuEChERS技術(shù)為基礎(chǔ),結(jié)合不同的改進(jìn)方法,對(duì)復(fù)雜基質(zhì)進(jìn)行提取與凈化,并結(jié)合超高效液相色譜-串聯(lián)質(zhì)譜進(jìn)行分析,具體內(nèi)容如下:1.闡述了QuEChERS方法的原理、進(jìn)展及應(yīng)用;同時(shí)簡(jiǎn)要介紹了獸藥與霉菌毒素。2.建立了以QuEChERS方法結(jié)合柱凈化為前處理手段,結(jié)合超高效液相色譜-串聯(lián)質(zhì)譜同時(shí)測(cè)定有機(jī)肥中46種抗生素的分析檢測(cè)方法�？疾炝�4種改進(jìn)方式對(duì)三類抗生素的提取效果的影響,確定了最佳前處理方法。該方法能同時(shí)滿足三類抗生素的檢測(cè)要求,并成功應(yīng)用于實(shí)際有機(jī)肥樣品中獸藥殘留的測(cè)定。3.以氟喹諾酮類抗生素為研究對(duì)象,將QuEChERS方法與氟喹諾酮免疫膠體金快速檢測(cè)試劑板相結(jié)合,建立了一種快速篩查有機(jī)肥中氟喹諾酮?dú)埩絷?yáng)性樣品的分析方法。以QuEChERS方法為依據(jù),對(duì)提取溶液種類與pH值、吸附劑種類與用量等因素進(jìn)行優(yōu)化,確定了最佳前處理方法。該方法操作簡(jiǎn)單,耗時(shí)較短,不需要特殊儀器,能夠現(xiàn)場(chǎng)對(duì)樣品進(jìn)行前處理并立即得到結(jié)果,為快速篩查氟喹諾酮?dú)埩絷?yáng)性樣品提供技術(shù)支持。4.建立了QuEChERS結(jié)合超高效液相色譜-串聯(lián)質(zhì)譜同時(shí)測(cè)定飼料中13種霉菌毒素的分析方法。將功能化磁性材料應(yīng)用于QuEChERS方法,通過(guò)回收利用,降低了實(shí)驗(yàn)成本,并對(duì)提取溶劑、磁性吸附劑的種類與用量等因素進(jìn)行優(yōu)化,確定了最佳萃取條件。本方法能快速簡(jiǎn)便的完成前處理過(guò)程,并成功運(yùn)用于實(shí)際飼料樣品的分析檢測(cè),為養(yǎng)殖業(yè)飼料的質(zhì)量控制提供科學(xué)依據(jù)。
[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.
【學(xué)位授予單位】：浙江工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TS207.5;O657.63

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