本文選題：超聲微波輔助萃取 + 固相微萃取�。� 參考：《浙江工業(yè)大學》2017年碩士論文

【摘要】：微波輔助萃取(microwave assisted extraction,MAE)作為一種高效的萃取技術(shù),已在天然產(chǎn)物萃取和食品藥品分析領(lǐng)域得到了廣泛應用。相比靜態(tài)微波萃取模式,超聲微波輔助萃取(ultrasonic/microwave asstited extraction,UMAE)具有更明顯的優(yōu)勢,因為超聲加快了目標化合物的傳質(zhì)速度,降低了熱不穩(wěn)定化合物因長時間微波照射而引起的降解。在已發(fā)表的關(guān)于超聲微波輔助萃取的研究中,萃取劑一般采用水或者傳統(tǒng)的有機溶劑,本文引入低共熔溶劑(deep eutectic solvent,DES)對植物樣品進行預處理,使得提取出的揮發(fā)性有機物(volatile organic compound,VOC)更為豐富,精油得率更高。環(huán)境中VOC主要使用氣相色譜質(zhì)譜聯(lián)用(gas chromatography-mass spectrometry,GC-MS)法進行檢測,VOC直接進入儀器會出現(xiàn)信號響應不高,質(zhì)譜分辨率差,儀器受樣品濕度影響大等問題,通過三級冷阱技術(shù)凈化和濃縮樣品,使得上述問題得到改善。本文具體內(nèi)容如下:1)建立了一種以DES為基礎(chǔ)的微波輔助水蒸汽蒸餾(deep eutectic solvent-microwave assisted steam distillation,DES-MASD)提取八角茴香揮發(fā)性精油的方法。對萃取過程中的參數(shù)進行了優(yōu)化。在最優(yōu)條件下對八角茴香進行揮發(fā)性精油的提取,DES-MASD的精油得率為5.3%,MASD的精油得率為3.0%,兩者結(jié)果有著明顯差別。精油組分的分析,DES-MASD能得到較MASD更多的揮發(fā)性物質(zhì)。實驗結(jié)果表明,DES-MASD是一種新型的高效提取八角茴香揮發(fā)性精油的綠色前處理技術(shù)。2)建立了一種新型的以DES為基礎(chǔ)的超聲微波協(xié)同-頂空固相微萃取(deep eutectic solvent-ultrasonic/microwave asstited steam distillation-headspace solid phase microextraction,DES-UMASD-SPME)結(jié)合GC-MS的方法分析測定八角茴香中的揮發(fā)性精油成分。采用單因素實驗對影響該方法的因素進行了優(yōu)化。將最優(yōu)條件下得到的樣品分析結(jié)果與DES-MASD進行了比較,DES-UMASD-SPME法使用更少的樣品消耗更低的DES體積和更短的萃取時間。結(jié)果表明:DES-UMASD-SPME是一種快速、高效的實驗方法,可以快速的對八角茴香進行提取和分析揮發(fā)性成分,消耗樣品量少,沒有污染,符合綠色分析化學的需求。3)建立了一種三級冷阱技術(shù)參與的環(huán)境中VOC的富集與檢測的方法。優(yōu)化了大氣預濃縮儀的三級冷阱的捕集溫度,對TO15標氣進行了一系列測試:繪制了標準曲線(0.5-10 nmol/mol)得到了目標化合物的平均相對響應因子(average relative response factor,ˉˉˉˉˉRRF),它們的相對標準偏差(relative standard deviation,RSD)在4.47-28.12%之間;方法的精密度為2.81-18.68%;方法的檢出限(method detection limit,MDL)為0.22-2.17 nmol/mol;通過中低兩個水平濃度的加標,得到方法的回收率為72.51-113.67%。對某工廠的環(huán)境空氣樣進行了檢測,得到結(jié)果有高濃度的N,N-二甲基乙酰胺存在。以上實驗結(jié)果表明,三級冷阱前處理參與的環(huán)境中VOC的富集與檢測方法是一種高效可靠的方法,它的檢測限低,靈敏度高,不消耗有機試劑沒有污染,符合環(huán)境中VOC監(jiān)測的需求,符合綠色分析化學的需求。
[Abstract]:Microwave assisted extraction (MAE), as an efficient extraction technology, has been widely used in the field of natural product extraction and food and drug analysis. Compared with the static microwave extraction model, ultrasonic microwave assisted extraction (ultrasonic/microwave asstited extraction, UMAE) has a more obvious advantage because of ultrasound. The mass transfer speed of the target compound was accelerated and the degradation of thermal unstable compounds caused by the long time microwave irradiation was reduced. In the published study on ultrasonic microwave assisted extraction, the extractants generally used water or traditional organic solvents. This paper introduced the low eutectic solution (deep eutectic solvent, DES) to plant samples. The extraction of volatile organic compounds (volatile organic compound, VOC) is more abundant and the yield of essential oil is higher. In the environment, VOC is mainly detected by gas chromatography-mass spectrometry (gas chromatography-mass spectrometry, GC-MS), and VOC directly enters the instrument with low signal response, poor resolution of mass spectrometry, and instrument sample. The problem is improved by purifying and concentrating samples by three stage cold trap technology. The contents of this paper are as follows: 1) a DES based microwave assisted steam distillation (deep eutectic solvent-microwave assisted steam distillation, DES-MASD) is established to extract the volatile essential oil of the star anise The parameters in the extraction process were optimized. Under the optimal conditions, the extraction of volatile essential oil from the star anise was obtained, the yield of essential oil of DES-MASD was 5.3% and the yield of essential oil of MASD was 3%. The results of the two were distinctly different. The analysis of essential oil components, DES-MASD could get more MASD volatile substances. The experimental results showed that DES-MA SD is a new green pretreatment technology.2 for efficient extraction of the volatile essential oil of anise fennel. A new type of DES based ultrasonic microwave synergetic solid phase microextraction (deep eutectic solvent-ultrasonic/microwave asstited steam distillation-headspace solid phase microextraction) has been established. The GC-MS method was used to determine the volatile essential oil in the star anise. The factors affecting the method were optimized by single factor experiment. The result of the sample analysis obtained under the optimal condition was compared with that of the DES-MASD. The DES-UMASD-SPME method used less samples to consume lower DES volume and shorter extraction time. Ming: DES-UMASD-SPME is a fast and efficient experimental method, which can quickly extract and analyze volatile components of star anise, consume less sample, not pollute, meet the requirement of green analytical chemistry.3). A method of enrichment and detection of VOC in the environment of three stage cold trap is established. The preconcentration of air Preconcentration is optimized. The capture temperature of the three stage cold trap has been tested for a series of TO15 standard gases: the standard curve (0.5-10 nmol/mol) has been drawn to obtain the average relative response factor of the target compounds (average relative response factor, - to - - - - RRF), and their relative standard deviation (relative standard deviation, RSD) is between the methods. The precision of the method is 2.81-18.68%; the detection limit of the method (method detection limit, MDL) is 0.22-2.17 nmol/mol; the recovery rate of the method is 72.51-113.67%. to a factory's ambient air sample through the addition of two level concentrations at the middle and low levels. The results have high concentration N, N- two methyl acetamide. The enrichment and detection method of VOC in the environment of three stage cold well pretreatment is a highly efficient and reliable method. Its detection limit is low, the sensitivity is high, no organic reagent is consumed and no pollution is consumed. It meets the needs of VOC monitoring in the environment and meets the requirements of green analytical chemistry.
【學位授予單位】：浙江工業(yè)大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O656

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