挥发组分论文：两种香型天然香料挥发组分的研究.doc

挥发组分论文：两种香型天然香料挥发组分的研究【中文摘要】本文对挥发组分的提取方法,水蒸气蒸馏法和固相微萃取法条件进行优化;在最佳条件下提取挥发组分,通过GC-MS联用分析芳香型、辛香型香气成分;利用气相色谱内标法定量分析芳香型香气主成分正丁酸、苯甲醛,辛香型香气主成分桉树脑、茴香精;用荧光光谱法研究其抗氧化性。采用水蒸气蒸馏法以样品粉碎过0.45 mm筛,浸泡12 h,水蒸气蒸馏6 h;固相微萃取法以萃取头型号75m CAR/PDMS,样品平衡时间40 min,萃取温度70,萃取时间60 min,解吸时间4 min。在此最佳条件下提取芳香型、辛香型样品挥发组分。通过GC-MS联用测定两种提取方法下芳香型、辛香型样品挥发油并比较其组分差异。利用气相色谱法对芳香型挥发主成分正丁酸、苯甲醛和辛香型挥发主成分桉树脑、茴香精做内标法定量分析,芳香型、辛香型分别以乙酸、萘为内标物。利用荧光光度法通过测定样品对羟基自由基的清除率分析各种样品的抗氧化性。最佳条件为缓冲盐溶液pH 7.0,苯甲酸与过氧化氢摩尔比0.003,过氧化氢用量0.5 mL,Co2+浓度5.210-4 mol/L对两种香型样品抗氧化进行测定与比较。结果表明:GC-MS检测芳香型样品中挥发组分主要是苯甲醛、正丁酸;辛香型样品中挥发组分主要是茴香精、桉树脑。固相微萃取分析结果多为头香,挥发性组分数目少,鉴定出的醛类种类多含量高。水蒸气蒸馏所得挥发性组分多为中香和尾香,检出组分全面,鉴定出含量较高正丁酸。GC定量分析杏花及花蕾中苯甲醛含量较其它花中高;杏各部位中杏仁苯甲醛含量较高,杏肉中正丁酸含量较高;动态分析杏叶苯甲醛含量逐渐降低。对羟基自由基清除力杏花、桃花强于蔷薇科其它花,杏仁强于杏其它部位。采用水蒸气蒸馏和固相微萃取技术结合气相色谱-质谱法鉴定挥发组分较全面,气相色谱法定量分析挥发组分中有效成分简单、快捷、精准,由荧光光谱法分析样品挥发油抗氧化性可知,芳香型、辛香型天然香料挥发油有强弱不同的抗氧化性。【英文摘要】In this paper, method of extracting the volatile components including steam distillation and solid phase micro-extraction were optimized; the volatile components are extracted under optimal conditions and aromatic, spicy aroma components are analyzed by GC-MS. Butyric acid, benzaldehyde of principal components in aromatic and eucalyptol, fennel essence of volatile components are analyzed by gas chromatography; antioxidant are studied by fluorescence spectroscopy.Samples was crushed through 0.45mm sieve, soaked 12h, steam distilled 6h by steam distillation; 75m CAR/PDMS of SPME fiber model, equilibrium time 40 min, extraction temperature 70,extraction time 60 min, desorption time 4 min are used by solid phase micro extraction.Aromatic, spicy-type sample volatile component is extracted under the optimal conditions. Aromatic, spicy-type components of essential oil samples are measured and compared by GC-MS. Butyric acid, benzaldehyde of volatile in aromatic components and eucalyptol,fennel essence of volatile components in spicy type are quantitative analyzed by gas chromatography.Acetic acid, naphthalene are used as internal standard for Aromatic, spicy types components. The antioxidant activity of various samples is analyzed by fluorescence spectrometry which depend on determining sample rate of hydroxyl radicals.Antioxidant activity of two aromatic samples is measured and compared under the best conditions: buffer salt solution pH 7.0, acid and hydrogen peroxide molar ratio 0.003, hydrogen peroxide 0.5mL, concentration of the Co+ 5.210-4 mol/L.The results show that: the volatile aromatic components of the sample is mainly benzaldehyde, butyric acid and spice-type samples fennel volatile component is mainly fennel essence, eucalyptol by GC-MS. More first fragrance, the less number of volatile compounds,and many kinds of content aldehydes identified by solid phase micro extraction. In the composition of fragrant incense and tail is identified including higher content of butyric acid by steam distillation and volatile components detected are comprehensive. GC quantitative analysis show that:content of benzaldehyde is higher than other flowers in Apricot flower and flower buds;Content of benzaldehyde in Apricot almond is higher than that which is in various parts of Apricot, the highest content of Apricot is butyric acid; the content of benzaldehyde is decreased in dynamic leaves. Hydroxyl radical scavenging of apricot, peach flower is stronger than the other flower and almond is Stronger than other parts of apricot.The volatile components identified are more comprehensive by steam distillation and solid phase micro extraction combined gas chromatography - mass spectrometry.The active ingredients of volatile components are analyzed quantitative by gas chromatography, and the method is simple, fast and accurate.The antioxidant of volatile oil in samples is analyzed by fluorescence spectroscopy, and this study shows that aromatic, spicy fragrance of natural essential oil type has different antioxidant strength.【关键词】挥发组分 提取方法 GC-MS GC 抗氧化性【英文关键词】volatile components extraction GC-MS GC antioxidant【目录】两种香型天然香料挥发组分的研究摘要4-5ABSTRACT5-6第一章 前言9-121.1 挥发油简介9-101.1.1 挥发油概念91.1.2 挥发油的主要化学组成9-101.1.3 植物性天然香料的抗氧化性101.2 香料的历史10-111.3 研究背景11-12第二章 天然香料的提取分析与应用12-152.1 植物性天然香料的提取12-142.1.1 影响香料组成的环境因素122.1.2 提取技术12-142.2 分离与分析方法142.2.1 分离技术142.2.2 分析方法142.3 天然香料的应用14-15第三章 GC-MS 分析天然香料挥发性化学成分15-583.1 主要仪器、试剂与材料15-163.1.1 主要仪器与试剂153.1.2 样品与处理15-163.2 水蒸气蒸馏法与气质联用分析挥发组分化学成分16-373.2.1 水蒸气蒸馏条件实验16-213.2.2 芳香型样品香气分析21-333.2.3 辛香型样品香气分析33-363.2.4 结论36-373.3 固相微萃取法与气质联用分析挥发组分化学成分37-563.3.1 固相微萃取条件实验37-423.3.2 芳香型样品香气分析42-513.3.3 辛香型香气成分分析51-563.3.4 结论563.4 结果与讨论56-58第四章 气相色谱法分析主成分含量58-694.1 主要仪器试剂与样品58-594.1.1 主要仪器584.1.2 样品584.1.3 色谱条件58-594.2 芳香性物质中正丁酸、苯甲醛的定量分析59-644.2.1 定量校正因子测定59-604.2.2 标准曲线的绘制60-614.2.3 精密度实验614.2.4 稳定性实验614.2.5 重现性实验61-624.2.6 回收率实验624.2.7 最低检出限624.2.8 样品中正丁酸、苯甲醛含量的测定62-644.2.9 结果644.3 辛香物质中茴香精、桉树脑的定量分析64-694.3.1 定量校正因子测定64-654.3.2 标准曲线的绘制65-664.3.3 精密度实验664.