本文選題：離子液體分散液液微萃取尿樣 + 3-羥基苯并[a]芘��； 參考：《中國(guó)科學(xué)技術(shù)大學(xué)》2016年碩士論文

【摘要】：隨著分析技術(shù)的發(fā)展,樣品前處理技術(shù)朝著高效、快速、綠色、自動(dòng)化與微型化的方向發(fā)展。本論文綜述了幾種常見(jiàn)的基于相分配及相吸附原理的樣品前處理技術(shù),分別介紹了它們的原理、特點(diǎn)及應(yīng)用。在充分調(diào)研文獻(xiàn)的基礎(chǔ)上,本論文主要進(jìn)行了以下幾部分的研究工作：1.建立了離子液體-分散液液微萃�。咝б合嗌V-熒光檢測(cè)法測(cè)定吸煙人群尿樣中3-羥基苯并[a]芘的分析方法。尿樣經(jīng)酶解、濾膜過(guò)濾后,采用[C8MIM][PF6]為萃取劑進(jìn)行分散液液微萃取富集,移取沉積相進(jìn)行液相色譜分析。實(shí)驗(yàn)對(duì)酶解條件、萃取條件及熒光測(cè)量條件進(jìn)行了優(yōu)化。在最佳的實(shí)驗(yàn)條件下,方法在1.5-150ng/L濃度范圍內(nèi)具備良好的線性關(guān)系(r20.996),富集倍數(shù)約為180。檢出限(LOD)和測(cè)定下限(LOQ)分別為0.45和1.5 ng/L。加標(biāo)回收率為85.6-94.6%,相對(duì)標(biāo)準(zhǔn)偏差(RSD)為3.4-5.2%。2.建立了離子液體-分散液液微萃取-丹磺酰氯衍生／高效液相色譜串聯(lián)質(zhì)譜法測(cè)定尿樣中3-羥基苯并[a]芘的分析方法。尿樣經(jīng)酶解、濾膜過(guò)濾、采用[C8MIM][PF6]為萃取劑進(jìn)行分散液液微萃取富集后,采用丹磺酰氯作為衍生試劑對(duì)3-OHBaP進(jìn)行化學(xué)衍生,移取沉積相進(jìn)行液相色譜串聯(lián)質(zhì)譜分析。實(shí)驗(yàn)對(duì)丹磺酰氯衍生條件進(jìn)行了優(yōu)化。在最佳的實(shí)驗(yàn)條件下,方法在0.6~50.0 ng/L濃度范圍內(nèi)具備良好的線性關(guān)系(r2≥0.9918)。LOD與LOQ分別為0.2和0.58 ng/L。加標(biāo)回收率為87.8%～96.2%,RSD為3.3%~6.8%。3.在分散液液微萃取與磁性固相萃取的基礎(chǔ)上,研究了一種新型的分散固液微萃取技術(shù)。建立了磁性分散固液微萃取-在線熱解析-氣質(zhì)聯(lián)用法測(cè)定煙葉中易揮發(fā)的中性香氣成分的分析方法。本文自制了CIP-SiO2-PDMS磁性吸附劑,通過(guò)紅外、熱重、透射電鏡、掃描電鏡等方法對(duì)材料進(jìn)行了表征。實(shí)驗(yàn)對(duì)CIP-SiO2-PDMS磁性吸附劑的合成條件、萃取條件和解析條件進(jìn)行了優(yōu)化。最后采用本方法對(duì)若干種揮發(fā)性中性香氣成分進(jìn)行了分析。
[Abstract]:With the development of analytical technology, sample pretreatment technology develops towards high efficiency, fast, green, automation and miniaturization.In this paper, several common sample pretreatment techniques based on phase distribution and phase adsorption are reviewed, and their principles, characteristics and applications are introduced respectively.On the basis of full investigation and research, this paper mainly carried out the following parts of the research work: 1.A method for the determination of 3-hydroxybenzo [a] pyrene in urine samples of smoking population by ion liquid-dispersible liquid microextraction / high performance liquid chromatography-fluorescence detection was established.Urine samples were hydrolyzed by enzyme and filtrated by filter membrane, then [C8MIM] [PF6] was used as extractant for dispersible liquid microextraction enrichment, and the deposition phase was removed for liquid chromatographic analysis.The conditions of enzymatic hydrolysis, extraction and fluorescence measurement were optimized.Under the optimum experimental conditions, the method has a good linear relationship in the concentration range of 1.5-150ng/L, r20.996, and the enrichment factor is about 180.The detection limit (LOD) and the determination limit (LOQ) were 0.45 and 1.5 ng / L, respectively.The recoveries were 85.6-94.6 and the relative standard deviation (RSDs) was 3.4-5.2. 2.A method for the determination of 3-hydroxybenzo [a] pyrene in urine by ion liquid-dispersible liquid microextraction with dansulfoyl chloride derivation / high performance liquid chromatography tandem mass spectrometry was established.Urine samples were hydrolyzed by enzyme, filtrated by filter membrane, and enriched with [C8MIM] [PF6] as extractant. After microextraction and enrichment with [C8MIM] [PF6] as extractant, the 3-OHBaP was chemically derivated by dansulfoyl chloride, and the deposition phase was removed and analyzed by liquid chromatography tandem mass spectrometry (LC-MS).The derivatization conditions of dansulfonyl chloride were optimized.Under the optimum experimental conditions, the linear relationship between 0.9918).LOD 鈮，

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