本文選題：懸浮固化-分散液液微萃取(DLLME-SFO) + 空氣輔助-分散液液微萃取(AALLME)��； 參考：《貴州師范大學》2017年碩士論文

【摘要】：在食品農(nóng)藥殘留分析中,樣品預(yù)處理步驟非常關(guān)鍵。分散液液微萃取(DLLME)技術(shù)作為一種新型樣品前處理技術(shù),克服了傳統(tǒng)樣品預(yù)處理技術(shù)或繁雜耗時、或?qū)嶒灣杀具^高、抑或處理效果不佳等缺點,滿足理想方法所應(yīng)具備的成本低、準確度高、選擇性高、靈敏度高、重現(xiàn)性良好的要求,在其不斷發(fā)展的過程中,一直備受關(guān)注。本文是在總結(jié)前人研究工作的基礎(chǔ)上,利用三種新型分散液液微萃取方法對食品中的常見農(nóng)藥殘留進行了應(yīng)用分析研究,內(nèi)容如下:1.建立了懸浮固化-分散液液微萃取-氣相色譜法(DLLME-SFO-GC)測定野木瓜中9種有機氯農(nóng)藥殘留量的方法。樣品經(jīng)石油醚提取、濃硫酸凈化、懸浮固化-分散液液微萃取法濃縮后,用氣相色譜-電子捕獲檢測器(ECD)檢測,外標法定量。結(jié)果表明,9種農(nóng)藥在1.0~100.0μg/L范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)R2在0.99以上,方法檢出限(LOD)為0.01~0.07μg/kg。9種有機氯農(nóng)藥在1.75、7.00、28.00μg/kg三個濃度水平添加下,平均回收率范圍為83.3~116.7%,相對標準偏差(RSD)范圍為1.5~14%。該方法靈敏度高,成功應(yīng)用于野木瓜中9種有機氯農(nóng)藥殘留的測定。2.建立了空氣輔助-分散液液微萃取-氣相色譜法(AALLME-GC)測定水果中7種有機磷農(nóng)藥殘留量的新方法。樣品經(jīng)乙酸乙酯提取、空氣輔助-分散液液微萃取法濃縮后,用氣相色譜-火焰光度檢測器(FPD)檢測,采用外標法對有機磷農(nóng)藥殘留進行定量。在優(yōu)化后的實驗條件下,7種農(nóng)藥均在40.0~4000.0μg/L范圍內(nèi)線性關(guān)系良好,R2在0.99以上,LOD為0.24~1.32μg/kg。采用三個不同濃度水平(12.0、300.0、1000.0μg/kg)進行了加標回收實驗,結(jié)果表明,7種有機磷農(nóng)藥的平均回收率范圍為82.0~114.8%,RSD范圍為1.8~15.2%,該方法準確靈敏,成功應(yīng)用于野木瓜、蘋果、梨、葡萄中7種有機磷農(nóng)藥殘留的測定。3.開發(fā)了一種簡便快速的微萃取技術(shù)即空氣輔助-懸浮固化-分散液液微萃取(AALLME-SFO)用以萃取果汁中4種擬除蟲菊酯農(nóng)藥殘留。本方法無需分散劑,用少量的低密度有機溶劑作萃取劑,被富集后的分析物經(jīng)ECD檢測,外標法定量。在優(yōu)化后的實驗條件下,4種擬除蟲菊酯農(nóng)藥LOD低(0.01~0.03μg/L),在5.0~500.0μg/L范圍內(nèi)線性關(guān)系良好,R2在0.99以上。在5、100、400μg/L三個濃度水平添加下,平均回收率范圍為82.6~113.6%,RSD范圍為1.4~14.1%,以上結(jié)果表明,該方法對果汁中四種擬除蟲菊酯類農(nóng)藥的測定具有優(yōu)越的性能。綜上,本文對不同類型的DLLME技術(shù)進行了研究,通過超聲輔助、空氣輔助等方式開發(fā)了三種新型DLLME技術(shù)測定食品中的常見農(nóng)藥殘留,對固體基質(zhì)上DLLME技術(shù)的應(yīng)用進行探索的同時,也極大地提高了分析性能。
[Abstract]:In food pesticide residue analysis, sample pretreatment is very important. Dispersion liquid microextraction (DLLME), as a new sample pretreatment technology, overcomes the disadvantages of traditional sample pretreatment technology, such as excessive time consuming, high experimental cost or poor treatment effect, and meets the low cost of the ideal method. The requirements of high accuracy, high selectivity, high sensitivity and good reproducibility have attracted much attention in the process of its continuous development. On the basis of summarizing the previous research work, three new dispersible liquid microextraction methods were used to analyze the common pesticide residues in food. The contents are as follows: 1. A method for the determination of 9 organochlorine pesticide residues in papaya by suspension solidification, dispersion liquid microextraction and gas chromatography (DLME-SFO-GC) was established. The samples were extracted by petroleum ether, purified by concentrated sulfuric acid, concentrated by suspension solidification-dispersion liquid microextraction, detected by gas chromatography-electron capture detector (ECD) and quantified by external standard method. The results showed that the linear range of nine pesticides was 1.0 渭 g / L, the correlation coefficient R2 was above 0.99. The detection limit (LOD) of the method was 0.01n 0.07 渭 g/kg.9 and the average recovery range was 83.3116.7 渭 g/kg and the relative standard deviation was 1.5%. The method is highly sensitive and has been successfully applied to the determination of 9 organochlorine pesticide residues in papaya. A new method for the determination of seven organophosphorus pesticide residues in fruit by air assisted dispersible liquid microextraction and gas chromatography (AALLME-GC) was established. The samples were extracted by ethyl acetate and concentrated by air-assisted dispersible liquid microextraction. The organophosphorus pesticide residues were determined by gas chromatography-flame photometric detector (FPD) and external standard method. Under the optimized experimental conditions, the linear range of seven pesticides was within the range of 40.0 渭 g / L and 4000.0 渭 g / L, respectively. The linear range of R2 was 0.99 and the LOD was 0.240.32 渭 g / kg 路L ~ (-1) 路L ~ (-1) 路L ~ (-1) 路L ~ (-1). The standard addition and recovery experiments were carried out at three different concentration levels (12.0300.0 渭 g/kg). The results showed that the average recovery range of seven organophosphorus pesticides was 82.0 ~ 114.80.The method was accurate and sensitive, and was successfully applied to wild papaya, apple and pear. Determination of 7 organophosphorus pesticide residues in grape A simple and rapid microextraction technique called air assisted suspension solidification dispersion liquid microextraction (AALLME-SFO) was developed for the extraction of four pyrethroid pesticide residues in fruit juice. In this method, a small amount of low density organic solvent was used as extractant without dispersant. The enriched analytes were detected by ECD and quantified by external standard method. Under the optimized experimental conditions, the LOD of four pyrethroid pesticides was low (0.01 ~ 0.03 渭 g / L), and the linear relationship was higher than 0.99 in the range of 5.0 ~ 500.0 渭 g / L. The average recovery range was 82.6 渭 g / L, 113.6% and 1.4 渭 g / L, respectively. The results showed that the method had excellent performance for the determination of four pyrethroid pesticides in fruit juice. In this paper, three new DLLME technologies were developed to determine common pesticide residues in food by means of ultrasonic and air assisted, and the application of DLLME technology on solid matrix was explored at the same time. It also greatly improves the analytical performance.
【學位授予單位】：貴州師范大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TS207.53;O658.2

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