烟草科技
煙草科技
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TOBACCO SCIENCE & TECHNOLOGY
2014年
10期
61-66
,共6页
吴亿勤%杨柳%秦云华%杨继%缪明明%徐济仓
吳億勤%楊柳%秦雲華%楊繼%繆明明%徐濟倉
오억근%양류%진운화%양계%무명명%서제창
单液滴微萃取%逸出气分析%热解行为%叶黄素
單液滴微萃取%逸齣氣分析%熱解行為%葉黃素
단액적미췌취%일출기분석%열해행위%협황소
Single drop microextraction(SDME)%Released gas analysis%Pyrolysis behavior%Lutein
为研究空气氛围中叶黄素的热解行为,设计了捕集热重逸出组分的自动单液滴微萃取(SDME)装置,并与气相色谱/质谱(GC/MS)结合。根据TG/DTA(差热分析)结果,在155~400℃范围内,划分16个温度段连续取样。通过比较每个温度段的质量损失和裂解产物的总峰面积,分析了以乙醇为萃取剂SDME的萃取效果。通过监测43种主要逸出组分相对含量的动态变化,对叶黄素在空气氛围中发生热裂解的可能机理进行了推导。结果表明:①优化后热分析条件为升温速率5℃/min,载气流量400 mL/min。②SDME对于裂解产物中挥发性组分具有优异的萃取效果。③GC/MS鉴别出的主要裂解成分包括酮类、醛类、醇类、烯烃和芳香烃类化合物,其中最重要的裂解产物有β-大马酮、巨豆三烯酮和氧化异佛尔酮。
為研究空氣氛圍中葉黃素的熱解行為,設計瞭捕集熱重逸齣組分的自動單液滴微萃取(SDME)裝置,併與氣相色譜/質譜(GC/MS)結閤。根據TG/DTA(差熱分析)結果,在155~400℃範圍內,劃分16箇溫度段連續取樣。通過比較每箇溫度段的質量損失和裂解產物的總峰麵積,分析瞭以乙醇為萃取劑SDME的萃取效果。通過鑑測43種主要逸齣組分相對含量的動態變化,對葉黃素在空氣氛圍中髮生熱裂解的可能機理進行瞭推導。結果錶明:①優化後熱分析條件為升溫速率5℃/min,載氣流量400 mL/min。②SDME對于裂解產物中揮髮性組分具有優異的萃取效果。③GC/MS鑒彆齣的主要裂解成分包括酮類、醛類、醇類、烯烴和芳香烴類化閤物,其中最重要的裂解產物有β-大馬酮、巨豆三烯酮和氧化異彿爾酮。
위연구공기분위중협황소적열해행위,설계료포집열중일출조분적자동단액적미췌취(SDME)장치,병여기상색보/질보(GC/MS)결합。근거TG/DTA(차열분석)결과,재155~400℃범위내,화분16개온도단련속취양。통과비교매개온도단적질량손실화렬해산물적총봉면적,분석료이을순위췌취제SDME적췌취효과。통과감측43충주요일출조분상대함량적동태변화,대협황소재공기분위중발생열렬해적가능궤리진행료추도。결과표명:①우화후열분석조건위승온속솔5℃/min,재기류량400 mL/min。②SDME대우렬해산물중휘발성조분구유우이적췌취효과。③GC/MS감별출적주요렬해성분포괄동류、철류、순류、희경화방향경류화합물,기중최중요적렬해산물유β-대마동、거두삼희동화양화이불이동。
To investigate the pyrolysis behavior of lutein in air, an automatic single drop microextraction (SDME) device for trapping the released fractions was designed and coupled with gas chromatography-mass spectrometry. According to the results of differential thermal-thermo gravimetric analysis (TG-DTA), the pyrolysis process was divided into 16 temperature sections in the range of 155-400℃, and the released fractions at each section were sampled successively. The extract effect of SDME with ethanol as a solvent was analyzed by comparing the mass loss in each temperature section with the total peak area of pyrolysis products. The probable mechanism of lutein pyrolysis in air was inferred on the basis of dynamically monitoring the changes of relative contents of 43 main pyrolysis components. The results indicated that: 1) The optimized conditions for the thermoanalyzer were: temperature ascending rate 5℃/minute and carrier gas flow rate 400 mL/minute. 2) SDME performed excellently in the extraction of volatile components in pyrolysis products. 3) The main components identified by GC/MS included ketones, aldehydes, alcohols, alkenes and aromatic hydrocarbons, the most important pyrolysis products were β-damascenone, megastigmatrienone and 4-oxoisophorone.