SPME/GC/MS分析小一点红挥发性化学成分

利用固相微萃取/气相色谱/质谱(SPME/GC/MS)联用技术对小一点红挥发性成分进行研究。共鉴定出25种化学成分,占挥发性总成分的91.99%。小一点红主要挥发性化学成分是β-月桂烯(51.18%),3,7,11,15-四甲基-2-十六烯-1-醇(21.55%),β-水芹烯(8.42%),n-十六酸(2.48%)等。     

枇杷果实挥发油中的化学成分

采用水蒸气蒸馏法提取枇杷果实的挥发油,利用气相色谱-质谱联用技术对挥发油化学成分进行分析,从挥发油中鉴定出25种化合物,占挥发油总量的95.41％％.挥发油以酸、酯、醛为主,其中含量较高的成分为棕榈酸、油酸、亚油酸、糠醛、油酸乙酯、十八碳-9,12-二烯酸乙酯、巴西酸亚乙酯、棕榈酸乙酯、7-十八碳烯酸甲酯、十七烷、亚油酸甲酯.     

柚子皮挥发油化学成分分析

使用水蒸气蒸馏法提取柚子皮中的挥发油,利用气相色谱-质谱联用技术对柚子皮化学成分进行分离鉴定,采用色谱峰面积归一化法确定各成分的相对含量。分析结果表明,共检测出62种组分,鉴定了其中的31种组分,占挥发油组分总量的50.0%。主要成分是β-蒎烯、4,4A,5,6,7,8-六氢-4,4A-二甲基-6-(1-甲基亚乙基)-(4R-顺)-2(3H)-萘酮、氧化芳樟醇、(E,E)-3,7,11,15-四甲基-1,6,10,14-十六碳四烯-3-醇。     

干红枣ASE提取物的GC/MS分析及其在卷烟中的应用

采用加速溶剂萃取法（ASE）萃取干枣中的香味成分,并进行毛细管气相色谱/质谱（GC/MS）分析和卷烟加香应用效果研究。结果表明：利用GC/MS从干红枣ASE提取物中共鉴定出35个挥发性成分,其中主要香味成分是：5-羟甲基糠醛、环十六内酯、十五-14-烯酸、2,3-二氢-3,5-二羟基-6-甲基-4H-吡喃-4-酮、棕榈酸、2-羟基-环十五酮、十八-9-烯醛、十八-9-烯酸、氧杂环十三-2-酮、1,3-环戊二酮和己酸等。香味轮廓分析法和卷烟应用实验显示：干红枣ASE提取物能有效地掩盖卷烟杂气,提高烟香丰富性,使烟气柔和细腻。     

杜康酒香气成分的GC/MS分析

采用液液萃取法提取杜康酒中的香气成分,通过气相色谱-质谱联用(GC-MS)技术对杜康酒中的香气成分进行分析鉴定,共检测到了39种香气成分.其中酯类22种,酸类8种,醇类6种,烷类物质2种.含量较高的物质有己酸乙酯、乳酸乙酯、已酸、乙酸、丁酸乙酯等物质,     

栽培宽叶缬草中的精油成分分析

采用水蒸气蒸馏法提取宽叶缬草精油,气相色谱-质谱分析其组成。从栽培宽叶缬草的精油成分中鉴定出6个化合物,共占精油总量的94.92%。它们分别是乙酸龙胆酯（60.19%）、（-）乙-酸桃金娘烯醇酯（3.87%）、α-乙酸松油酯（1.55%）、乙酰基蒈烯（1.68%）、α-芹子烯（26.07%）和（Z,E）α--法呢烯（1.56%）。结果表明乙酸龙胆酯和α-芹子烯是栽培缬草的主要成分。     

梁山慈竹挥发油成分的GC/MS分析及抑菌活性评价

采用水蒸气蒸馏法,从梁山慈竹竹秆及竹叶中提取挥发油,通过气相色谱-质谱联用法对梁山慈竹竹秆及竹叶挥发性成分进行分析,采用面积归-化法测定了挥发油中各组分的相对质量分数,利用抑菌圈法分别对枯草芽孢杆菌、金黄色葡萄球菌、番茄青枯菌、大肠杆菌进行抑菌性研究.结果显示,从竹秆和竹叶水蒸气蒸馏所得挥发油中分别检测出40种和76种化合物,其中竹秆中主要成分为14-甲基十五烷酸甲酯（20.83％）,8,11-十八碳二烯酸甲酯（20.23％）,棕榈酸（15.27％）,亚麻酸甲酯（12.07％）,棕榈酸乙酯（4.87％）,叶绿醇（3.78％）;竹叶中主要成分为：2-乙基呋喃（（4.51％）、（E）-2-己烯醛（5.73％）、植酮（4.29％）、棕榈酸乙酯（11.5％）、叶绿醇（4.81％）.其中竹秆精油对金黄色葡萄球菌有着很强的抑制能力,竹叶精油对水稻白叶枯菌抑制能力明显.     

顶空固相微萃取法分析安吉白茶香气成分

以安吉白茶为研究对象,采用全自动顶空-固相微萃取(Headspace solid-phase microextraction,HS-SPME)提取其香气物质,用气相色谱-质谱法(GC-MS)鉴定香气组分,并采用色谱峰面积归一化法计算各成分的相对百分含量.结果在安吉白茶中检出香气成分73个,占挥发性成分总量的95.59％,主要以酯类(30.17％)、醇类(27.75％)、酮类(13.75％)和碳氢化合物(9.24％)为主.安吉白茶的香气成分主要是十六烷酸甲酯、香叶醇、十六烷酸、亚麻酸甲酯、植醇、植酮、二氢猕猴桃内酯、亚油酸甲酯、β-紫罗酮、雪松醇、茉莉酮、橙花叔醇、芳樟醇、咖啡因、香叶基丙酮等.     

山绿茶化学成分的研究

硅胶柱色谱、凝胶柱色谱分离,高效液相色谱纯化,得到单体化合物,用各种有机波谱鉴定化合物结构。分离得到6个化合物,鉴定为:α-香树脂素(Ⅰ),乌索酸(Ⅱ),3β,19α-二羟基乌索-12-烯-24,28-二酸(Ⅳ),2α,3β,23-三羟基乌索-12-烯-28-羧酸(),3β,19α,20β-三羟基乌索-12-烯-24,28-二羧酸(V),3β,19α-二羟基乌索-12-烯-23,28-二羧酸(Ⅲ)。化合物Ⅰ,Ⅲ,Ⅳ,Ⅴ,Ⅵ都是首次从该植物中分离得到。     

独活浸膏的热裂解产物分析

采用在线热裂解-气相色谱质谱联用技术(Py-GC-MS),模拟卷烟燃吸状态,对独活浸膏进行热裂解,裂解产物经气相色谱-质谱联用仪分析。结果表明:独活浸膏的热裂解产物中共鉴定出51种成分,主要有5-羟甲基糠醛(29.00%)、甲氧基欧芹酚(18.79%)、(Z,Z)-9,12-亚油酸(5.76%)、(E)-2-甲基-2-丁烯酸(3.64%)、5-甲基糠醛(2.79%)、十六酸(2.67%)、2,3-二氢-3,5-二羟基-6-甲基-4H-吡喃-4-酮(1.55%)、糠醛(1.29%)等致香物质,该结果为独活浸膏在卷烟中的应用提供理论依据。     

Hydrolysis and retro‐aldol cleavage of ethyl threo‐2‐(1‐adamantyl)‐3‐hydroxybutyrate: competing reactions

The hydrolysis of ethyl threo‐2‐(1‐adamantyl)‐3‐hydroxybutyrate ( 1 ) and the parent ester ethyl 3‐hydroxybutyrate ( 4 ) has been studied experimentally and computationally. In the hydrolysis of threo‐ester 1 with 2 M NaOH, predominantly retro‐aldol product was observed, whereas the hydrolyzed product was present in a minor amount. When the reaction is carried out under the same conditions with the parent ester ethyl 3‐hydroxybutyrate ( 4 ), hydrolyzed product is exclusively observed. The competitive pathways, namely hydrolysis and the retro‐aldol reaction for 1 and 4 were investigated using DFT calculations in the both gas and solvent phase. The calculated results in the solvent phase at B3LYP/6–31 + G* level revealed that the formation of retro‐aldol products is kinetically preferred over the hydrolysis of threo‐ester 1 in the presence of a base. However, the parent ester 4 showed that the retro‐aldol process is less favored than the hydrolysis process under similar conditions. The steric effect imposed by the bulky adamantyl group to enhance the activation barriers for the hydrolysis of the ethyl threo‐2‐(1‐adamantyl)‐3‐hydroxybutyrate ( 1 ) was further supported by the calculations performed with tert‐butyl group at the α‐carbon atom of ethyl 3‐hydroxybutyrate ( 7 ). Copyright © 2010 John Wiley & Sons, Ltd.     

新疆紫花苜蓿籽脂肪酸化学成分的分析

采用索氏提取法提取新疆紫花苜蓿籽中的脂肪酸成分,进行甲酯化处理后用气相色谱-质谱联用技术分离和鉴定脂肪酸成分的组成和含量。结果表明,从紫花苜蓿籽中共分离鉴定出11种脂肪酸成分,占总量的86.71%,主要包括9,12,15-十八碳三烯酸（37.06%）、亚油酸（25.25%）、8-十四烯酸（8.1%）、棕榈酸（10.33%）等脂肪酸,其中不饱和脂肪酸占62.31%。     

用紫外光谱法测定共轭亚油酸乙酯的含量

在226-240nm波长范围内，采用紫外可见分光光度法测定了不同浓度的共轭亚油酸乙酯的吸光度，绘制出样品在不同浓度时的吸光度曲线，找出适宜的浓度范围，作线性回归分析，得到样品浓度和吸光度的线性关系。利用PE Autosystem XL-TurboMass测得样品中共轭亚油酸乙酯的准确浓度，结合回归系数给出了测定共轭亚油酸乙酯含量的经验公式。     

Laser prepared organic heterostructures based on star-shaped arylenevinylene compounds

This paper presents some studies about the preparation by matrix-assisted pulsed laser evaporation (MAPLE) technique of organic bulk heterojunctions made from the mixture of a star-shaped arylenevinylene compound, 4,4′,4″-tris[(4′-diphenylamino)styryl] triphenylamine as donor and fullerene derivative, [6, 6]-phenyl C61 butyric acid butyl ester, as acceptor, in the weight ratio 1:2. The mixed layer has been characterized by spectroscopic (UV–Vis, Fourier transform infrared) and microscopic (AFM) methods, and the effects of the deposition conditions (number of pulses) and of a buffer layer of poly(aniline-co-aniline propane sulfonic acid) or poly(3,4-ethylenedioxythiophene) poly(styrenesulfonate) have been analyzed. The study of the electrical properties has revealed a typical solar cell behavior for the heterostructure glass/ITO/poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)/4,4′,4″-tris[(4′-diphenylamino)styryl] triphenylamine: [6, 6]-phenyl C61 butyric acid butyl ester/Al, confirming that MAPLE could be an adequate method for the preparation of active layer based on bulk heterojunction for solar cells.     

1-二茂铁乙基膦酸的合成与表征

以1-二茂铁乙醇为原料,与三氯化磷反应后加入乙醇酯化,经Michaelis-Arbuzov重排合成1-二茂铁乙基膦酸二乙酯,再通过Me3SiBr-Et3N体系水解制得1-二茂铁乙基膦酸。利用IR、NMR、MS等实验手段对目标产物进行了表征,结果表明与预期结构相符。以1-二茂铁乙醇计算,总收率为35%。     

Investigation of the interaction of alkyl iodide vapours with a carbon surface by kinetic and isotopic methods

The rate of desorption of ethyl, propyl and butyl iodides adsorbed by active carbon was examined at various temperatures. From the desorption curves obtained, the kinetic equation of desorption, the activation energies of desorption and the corresponding partition functions were determined.     

三维荧光结合AWRCQLD测量化妆品中三种添加剂

没食子酸(GA a),学名为3,4,5-三羟基苯甲酸(分子式为C 7H 6O 5),通常以水合物的形式存在,作为一种重要的有机原料,广泛的存在于植物中。有研究证明GA a具有抗氧化、抗炎、抗肿瘤、抗病毒、抗突变等多种作用。因此GA a常作为抗氧化剂添加于化妆品中。对羟基苯甲酸(p-HA),分子式为C 7H 6O 3,其中的R基为甲基、乙基、丙基、丁基或庚烷基时分别称为对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯和对羟基苯甲酸庚酯。p-HA酯类的抗菌性强、毒性低、抑菌作用不受pH影响,因此常添加于化妆品及药物中用作防腐剂。间苯二酚(RE)又称1,3苯二酚或间二苯酚(分子式为C 6H 6O 2)。RE具有杀菌作用,可作为防腐剂添加于化妆品中。以没食子酸(GA a)、对羟基苯甲酸(p-HA)和间苯二酚(RE)三种化妆品常用添加剂为目标分析物,通过引入第四维—溶剂,构建四维荧光光谱数据,使用甲醇(光谱级)、乙醇(光谱级)、超纯水分别获得三组实验样本,三组样本的配置方法与加入药品量相同。使用FS920稳态荧光光谱仪对样本进行检测,设置激发波长为210~330 nm,间隔4 nm记录一个数据;发射波长为280~480 nm,间隔2 nm记录一个数据。初始发射波长总是滞后激发波长10 nm,由此可消除一级瑞利散射的干扰。随后使用空白扣除法对初始荧光数据进行预处理,去除了溶剂的拉曼散射。最后,采用核一致诊断法确定待测样本的组分数为3,使用交替加权残差约束四线性分解(alternating weighted residual constrained quadratic decomposition,AWRCQLD)算法对预处理后的三维荧光光谱数据进行分解。结果表明,AWRCQLD算法分解得到GA a、p-HA和RE的激发、发射光谱图与目标光谱几乎重叠,能实现光谱重叠严重的GA a、p-HA和RE的快速定性和定量分析。     

Hydrothermal decomposition of esters under high pressure

Abstract

The hydrothermal decomposition of two esters (methyl formate and ethyl formate) was studied in the absence of oxygen over the temperature range of 373 – 673 K at pressures from 15 to 35MPa for residence times between 72 and 600s. At hydrothermal conditions, the esters were hydrolyzed to formic acid and the corresponding alcohols in equilibrium yields of more than 90%, and the disappearance rate of ester was more promoted with increasing temperature than with increasing pressure. In supercritical water, the conversion of the esters reached 100% at short times. From reaction experiments with various catalysts, it was found that the hydrolysis of alkyl formates was accelerated by acid, while retarded by base in a manner different from that in usual water. In addition, a delayed reaction start observed in ester disappearance. profiles suggested strongly a catalytic action of formic acid produced by hydrolysis.     

无规共聚物与均聚物共混体系的相容性

用核磁共振方法(NMR)及差示扫描量热法(DSC)测定了苯乙烯-丙烯腈(SAN)无规共聚物与均聚物系列聚甲基丙烯酸甲酯(PMMA),聚甲基丙烯酸乙酯(PEMA),聚甲基丙烯酸正丁酯(PnBMA),聚甲基丙烯酸异丁酯(PiBMA)共混体系的有关参数,比较全面地研究了影响SAN与聚甲基丙烯酸酯类(PMAs)相容性的因素,对它们相容性的本质进行了探讨,得出了一些重要结论.