本文關鍵詞： 農藥殘留 液相色譜-串聯(lián)質譜 固相萃取 樣品稀釋 基質效應　出處：《山東大學》2017年碩士論文　論文類型：學位論文

【摘要】：農藥殘留檢測已經成為全球食品安全和環(huán)境監(jiān)測中的重要組成部分。許多國家和國際組織都制定了嚴格的限量標準,規(guī)定了農產品中農藥最大殘留限量(MRLs),保證食品安全及進出口貿易。隨著農藥殘留的廣泛重視,許多分析方法已經報道過。其中,液相色譜-串聯(lián)質譜因其高選擇性、高靈敏度而受到廣泛關注,是農藥殘留分析中的有力檢測技術。根據以上分析,本研究利用液相色譜-串聯(lián)質譜對果蔬中的強極性農藥和農藥多殘留測定進行了研究。本論文共分為三章:第一章為緒論,概述了農藥殘留分析中常用的前處理方法及檢測技術,詳細介紹了固相萃取及QuEChERS凈化方法,以及液相色譜-質譜聯(lián)用的檢測技術,主要包括液相色譜分離、低分辨串聯(lián)質譜和高分辨質譜的介紹。第二章利用液相色譜-串聯(lián)質譜(LC-MS/MS)檢測技術,對6種樣品中(蘋果、黃瓜、番茄、絲瓜、甘藍和茄子)的兩種高度親水性氨基糖苷類物質春雷霉素和井岡霉素-A進行了研究。使用乙腈和含有0.1%甲酸的水作為流動相,結果表明,ReproSil100C18色譜柱能夠用于強極性物質的保留,得到的良好峰形和響應值。甲醇和水混合溶劑(70:30,v/v,pH = 5.5)作為提取劑。HLB-SCX串聯(lián)固相萃取得到的基質效應在-12.6-6.11%之間,平均回收率在81.7-108%之間,并且RSDs低于13%。按照歐盟SANTE 11945/2015標準進行方法驗證。結果證明,該方法適合復雜水果和蔬菜樣品中的春雷霉素和井岡霉素-A的測定。第三章采用簡化的QuEChERS提取方法與超高效液相色譜-串聯(lián)質譜(UPLC-MS/MS)相結合,快捷、準確地對甘藍、生菜、番茄和甜椒四種蔬菜中的16種農藥進行檢測。分析過程中采用超高效液相色譜,16種農藥在10 min內能夠完全洗脫。樣品經0.2%甲酸乙腈(0.2:99.8,v/v)提取后,提取劑用甲醇/水(50:50,v/v)1:1稀釋后用于UPLC-MS/MS定量分析。在添加回收實驗中,添加水平為4,20,40 μg/kg,每個加標水平平行做五次。該方法的回收率為72.2-119%,相對標準偏差(RSDs)均小于17%,實現了農藥多殘留測定。該方法適合蔬菜中農藥多殘留測定。
[Abstract]:Pesticide residue detection has become an important part of global food safety and environmental monitoring. Many countries and international organizations have established strict limit standards. The maximum pesticide residue limit (MRLsN) in agricultural products is stipulated to ensure food safety and import and export trade. With the extensive attention paid to pesticide residues, many analytical methods have been reported. Among them, liquid chromatography-tandem mass spectrometry (LC-MS) is characterized by its high selectivity. High sensitivity and widespread concern, is a pesticide residue analysis of the force detection technology. According to the above analysis, In this study, the determination of strong polar pesticides and multi-residues in fruits and vegetables by liquid chromatography-tandem mass spectrometry (LC-MS) was studied. The methods of pretreatment and detection in pesticide residue analysis were summarized. The methods of solid phase extraction (SPE) and QuEChERS purification, as well as the detection techniques by liquid chromatography-mass spectrometry (LC-MS) were introduced in detail, including liquid chromatographic separation. Introduction of low Resolution tandem Mass Spectrometry and High Resolution Mass Spectrometry. In Chapter 2, six samples (apple, cucumber, tomato, loofah, luffa) were detected by liquid chromatography-tandem mass spectrometry (LC-MS / MS). Two highly hydrophilic aminoglycoside substances, vermilycin and Jinggangmycin A, were studied in cabbage and eggplant. Acetonitrile and water containing 0.1% formic acid were used as mobile phase. The results showed that ReproSil100C18 column could be used for the retention of highly polar substances. The results showed that the matrix effect of methanol / water mixed solvent 70: 30 v / v / v / v = 5.5) was -12.6-6.11%, and the average recovery was 81.7-108%, which was used as extractant. HLB-SCX was used as extractant in series solid-phase extraction, and the results showed that the matrix effect was in the range of -12.6-6.11%, and the average recovery was between 81.7-108%. And the RSDs is lower than 13. The method is verified according to the EU SANTE 11945/2015 standard. The result shows that, This method is suitable for the determination of vermicycin and Jinggangmycin A in complex fruit and vegetable samples. In Chapter 3, a simplified QuEChERS extraction method is combined with UPLC-MS / MS to rapidly and accurately determine cabbage and lettuce. Sixteen kinds of pesticides in tomato and sweet pepper vegetables were detected. In the process of analysis, 16 kinds of pesticides could be completely eluted in 10 min. The samples were extracted by acetonitrile 0.2% formate (0.2: 99.8 v / v). The extractant was diluted with methanol / water 50: 50 v / v / v / 1 for quantitative analysis of UPLC-MS/MS. The addition level was 40 渭 g 路kg ~ (-1) and each standard level was used for five times. The recovery rate of the method was 72.2-119, and the relative standard deviation (RSDs) was less than 17. The method was suitable for the determination of multi-residue pesticide in vegetables.
【學位授予單位】：山東大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TS255.7;O657.63

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