三叶鬼针草挥发性成分的研究

采用同时蒸馏萃取贵州三叶鬼针草不同部位挥发油，并用气相色谱-质谱进行分离测定，对比研究了它们的化学成分，共分离出69种成分，鉴定出53个化合物，主要成分为炔类、萜烯化合物及其衍生物；含量较高的化合物有(Z)-1，11-十三二烯-3，5，7，9-四炔(19．41％～37．16％)、石竹烯(15．68％～16．62％)、大牻桡牛儿烯-D(5．52％～18．50％)等。     

谱图检索结合二级质谱定性分析烟草中挥发性成分

采用同时蒸馏萃取法提取烟叶中的挥发性成分,利用气相色谱-质谱联用仪(GC-MS)分离测定,通过谱库检索和匹配度定性结合色谱保留指数方法鉴定烟叶中挥发性成分,并引入离子阱二级质谱对谱库检索匹配度差距小、含量低,背景干扰大的物质准确定性.采用谱图检索结合二级质谱定性共鉴定144个化合物,其中104个化合物在烟草挥发性成分的文献中已有报道,报道中有9个化合物是通过二级质谱定性,其余40个化合物还未见报道.结果表明,离子阱二级质谱定性的引入提高了对未知化合物定性的准确性和可靠性,适合于烟叶这类复杂植物体系的化学组分研究.     

气质联用法分析澳洲坚果壳的挥发性成分

分别建立了微波萃取和顶空直接进样GC/MS法对澳洲坚果壳的挥发性成分进行了分析。从澳洲坚果壳共分离鉴定了37个挥发性成分,包含烯烃、酸类、醛类、酮类、内酯类等,且澳洲坚果壳乙醇提取物具有令人愉悦的香味,其香气风格与原样迥异,具有成为香精香料来源的潜质。     

同时蒸馏萃取法分析紫苏叶挥发性化学成分

1 引言 紫苏是具有特异香气的唇形科一年生草本植物,紫苏叶具有相当可贵的药用、食用、工业用开发价值,本文用同时蒸馏萃取法提取了紫苏叶的挥发性成分,用GC/MS联用法分离鉴定出44种化合物,     

顶空固相微萃取-气质联用技术分析5种荷花的挥发性成分

采用顶空固相微萃取-气相色谱质谱联用(HS-SPME-GC-MS)技术分析测定了5个品种荷花中的挥发性成分.考察了不同萃取头和萃取温度对荷花挥发性成分萃取的影响,选用65μm PDMS/DVB SPME萃取头和25℃室温萃取荷花中的挥发性成分得到较好的萃取效果.应用峰面积归一化法测定各挥发性成分的相对含量,5个品种共鉴...     

同时蒸馏萃取-气相色谱/质谱法分析烟草中挥发性成分

本文对云南12种烟叶中挥发性成分进行提取分离,气相色谱/质谱测定.系统地对同时蒸馏萃取条件和色谱分离条件进行优化,结合谱库检索和匹配度定性方法鉴定149种化合物,并对其中的35种重要香气成分进行了定量分析,包括酮类7种、醇类6种、烯烃类4种、烟碱类3种、烷烃类2种、醛类2种、酯类2种、呋喃类2种等.该方法具有81.09％～97.45％的高回收率.结果表明,同时蒸馏萃取集采样、萃取、浓缩于一体,操作简单快速,适合于烟草中挥发性成分的提取,结合气相色谱/质谱联用仪(GC-MS)分离测定,能准确对挥发性成分进行定性和定量分析.     

3种人工结香方法所得沉香挥发性成分的SPME/GC-MS分析

采用固相微萃取(SPME)富集生物、化学及物理(火钻)法所得沉香的挥发性成分,用气相色谱-质谱联用技术(GC-MS)分离鉴别,然后对这3种人工结香方法进行评价。研究发现沉香的挥发性成分主要由倍半萜、芳香族等化合物组成,但由于结香方法不同,其化学成分及含量有很大差别。以沉香的6种特征性有效成分苄基丙酮、对甲氧基苄基丙酮、沉香呋喃、沉香螺旋醇、苍术醇、白木香醛及其含量作为评价沉香品质的主要指标,其中火钻法所得沉香中沉香螺旋醇的相对含量最高,约为5.5%;生物结香法所得沉香的特征成分的总含量最高,为16.6%;其次为火钻法所得的沉香,约为13.6%;化学法所得沉香的特征成分总含量相对较低。结果表明生物法的结香效果最好,其次为火钻法,均优于化学法。     

紫罗兰花挥发油化学成分分析及其在卷烟加香中的评价

研究紫罗兰花挥发油的挥发性成分及其卷烟加香效果。采用同时蒸馏萃取法提取紫罗兰花挥发油,利用气相色谱—飞行时间质谱(GC-TOFMS)联用技术对其化学成分进行分离鉴定,采用峰面积归一化法计算各个组分相对含量,并将其加入卷烟中进行感官评吸。共鉴定了66个化合物,占检出化合物总量的79.03%,主要成分为2-β-蒎烯(13.28%)、3-蒈烯(10.16%)、(-)-异喇叭烯(4.80%)、β-波旁烯(4.53%)、斯巴醇(3.39%)和β-杜松烯(3.29%)等;评吸结果发现:适量浓度的紫罗兰挥发油能提高卷烟整体的协调性,提升卷烟的香气质和香气量,降低对口腔、鼻腔的刺激性,减少杂气,回味甜香,余味清爽。紫罗兰挥发油中化学成分丰富,主要为萜类及其含氧衍生物,其中,许多化合物具有芳香性和药用活性。     

昆仑雪菊挥发物GC-MS分析

比较了水蒸气蒸馏法和固相微萃取法对昆仑雪菊发挥性成分萃取能力和萃取物种类的区别。分别利用水蒸气蒸馏法(HD)和顶空―固相微萃取法(HS-SPME)对昆仑雪菊挥发物进行萃取富集,用气相色谱―质谱法分析测定。结果表明,两种方法共提取、鉴定出65种化合物,其中水蒸气蒸馏法鉴定出49个化合物,顶空固相微萃取方法鉴定出35个化合物;两种方法相同的化合物共19个,占水蒸气蒸馏法鉴定化合物的78%,占固相微萃取法鉴定化合物的91%。两种提取方法得到的挥发物组分有部分差异,因此同时采用两种方法能够更加全面、完整地对昆仑雪菊的挥发性组分进行分析。     

水蒸气蒸馏提取与顶空进样GC-MS分析高良姜挥发性成分

比较了水蒸气蒸馏法和顶空加热法提取高良姜挥发性成分的方法,并进行GC-MS分析。结果表明,两种提取方法无论在成分还是其相对含量均存在一定的差异。采用顶空进样技术可鉴定出31个挥发性化学成分,采用水蒸气蒸馏法可鉴定出31个挥发性化学成分,两种方法共有成分为16种。两种样品采集方法分别提供了高良姜不同沸点挥发物的化学信息,运用这两种方法可以建立更全面的高良姜挥发性成分GC-MS表征体系。     

Rapid identification of volatile compounds in aromatic plants by automatic thermal desorption — GC-MS

Summary Thermal desorption is a valuable method for the fractionation of plant volatile components, which can be carried out on-line with GC analysis. The use of coupled GC-MS affords additional qualitative information, of special interest for plant species whose composition has not been previously studied. Some examples of the application of automatic thermal desorption, coupled to GC-MS to the identification and characterization of volatile components of plants of different families are given.     

Analysis of volatile organic compounds in fuel oil by headspace GC-MS

Fuel oils are mostly used in marine applications and in power plants. They are known to contain hazardous volatile organic compounds (VOCs) that are of health and environmental importance. Chlorinated compounds, phenolic compounds, styrenes, indene, dicyclopentadiene, dihydrodicyclopentadiene, cumene, benzene, toluene, ethylbenzene and xylenes are some of the VOCs that have found their way into fuel oil through various streams during bunkering operation. Chromatographic analysis of VOCs in the presence of complex matrices in fuel oil is one of the major challenges encountered when dealing with products of that nature. An analytical procedure using automated static headspace gas chromatography–mass spectrometry was developed for the analysis of these compounds in fuel oil. Styrene D8 and phenol D6 were used as internal standards for quantitation. Phenol D6 was used for the quantitation of phenolic compounds, while styrene D8 was used for the quantitation of other target analytes. The influence of headspace parameters on analyte response such as temperature, incubation time and sample amount were all investigated and optimised. Linear calibration curves were achieved for all components with determination coefficients R² > 0.995. Repeatability, limit of detection, limit of quantitation and recovery were reported. The matrix effect in fuel oil was minimised by 1:1 dilution with mineral oil. This method was successfully applied to the analysis of commercial samples.     

Dicationic ionic liquid stationary phase for GC-MS analysis of volatile compounds in herbal plants

The seeming “dual nature” of ionic liquids (ILs) for separating both apolar and polar compounds suggests that ILs may have a great potential for complex samples like essential oils from herbal plants that contain a great variety of compounds. In the present work, a geminal dicationic IL, 1,9-di(3-vinylimidazolium)nonane bis[(trifluoromethyl)sulfonyl]imidate, was investigated for this purpose. To find the best way to achieve satisfactory separations simultaneously for the compounds in essential oils, the dicationic IL was used as the stationary phase for capillary gas chromatography (GC) in two ways, either in its pure state or as a mixed stationary phase with monocationic ILs and a polysiloxane diluent. Interestingly, it was found that the mixed stationary phase exhibited a much better selectivity for polar and nonpolar compounds than either the dicationic IL or the polysiloxane, suggesting that a kind of synergistic effect occurred when these stationary phases were combined in the way described. A comparison with two commercial stationary phases (polar and nonpolar) indicated that this novel mixed stationary phase behaved in a way closer to a polar stationary phase in terms of selectivity and elution order. The present work demonstrates that the mixed stationary phase is efficient and selective and can be an alternative choice for the GC analysis of samples of complex composition. Figure Divinyldiimidazolium-based ionic liquid stationary phase     

Rapid determination of volatile compounds in grapes by HS-SPME coupled with GC-MS

Volatile compounds of grapes are responsible of varietal aroma. At the moment, methods used for analysis of these compounds are solvent-based, time-consuming and generally require large amounts of sample. In order to obtain an appropriate technique to study grape volatile compounds, HS-SPME method has been developed. The optimal sampling conditions were: 70 °C for 20 min with a 65-μm PDMS/DVB fibre. Sixteen volatile compounds have been quantified in pulp and skins of Muscat grapes. Terpenes, mainly linalool, geraniol and nerol, have been the volatiles present in the highest concentration, since these compounds contribute, to a larger extent, to the aroma of Muscat grapes and wines. So the proposed technique can be used for the characterisation of grape varieties or cultivars and for the determination of the aromatic maturity of grapes.     

Trace determination of volatile sulfur compounds by solid-phase microextraction and GC-MS

A method was developed for the simultaneous determination of the following nine volatile sulfur compounds in gas samples: carbon disulfide, carbonyl sulfide, ethyl sulfide, ethyl methyl sulfide, hydrogen sulfide, isopropanethiol, methanethiol, methyl disulfide and methyl sulfide. The target compounds were preconcentrated by solid-phase microextraction (SPME) and determined by gas chromatography combined with mass spectrometry. Experimental design was employed to optimize the extraction time and temperature and concurrent detection of the nine compounds was achieved by using an SPME fiber coated with Carboxen-polydimethylsiloxane (75 microns). Detection limits ranged from 1 ppt (v/v) for carbon disulfide to 350 ppt (v/v) for hydrogen sulfide and calibration functions were linear up to 20 ppb (v/v) for all the compounds investigated.     

顶空固相微萃取-气相色谱-质谱联用分析纺织品中挥发性有机物

建立了顶空固相微萃取（HSSPME）-气相色谱（GC）-质谱（MS）联用测定纺织品中甲苯、4-乙烯基环己烯、苯乙烯、萘和1-苯基环己烯5种挥发性有机物（VOCs）的分析方法。选择聚二甲基硅氧烷（PDMS）作为萃取涂层,优化了SPME的萃取条件,包括平衡时间、萃取时间、萃取温度、顶空体积、离子强度、搅拌速度、解吸温度和时间以及GC—MS仪器条件。对于甲苯、4-乙烯基环己烯、苯乙烯、萘和1-苯基环己烯方法线性范围分别为0．087～870、3．32～3320、2．28～2280、0．015～150和0．050～50．0ng／g;检出限分别为0．005、0．042、0．670、0．008和0．011ng／g。实际样品加标回收率在80．1％～122％之间,RSD在0．8％～8．6％之间。方法符合纺织品中痕量VOCs的快速分析要求。     

Sample stacking with in-column silylation for less volatile polar compounds using GC-MS

This paper presents sample stacking with in-column silylation (SIS) for quantitative analysis of less volatile polar compounds using gas chromatography-mass spectrometry (GC-MS). This was achieved by the combination of sandwiched in-column silylation and multiple injections (up to 100 times or 100 μL in total). N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) was used as a silylating reagent. For the SIS technique, samples were introduced multiple N times (N = 2~100) into a capillary column in between BSTFA injections. The quantitative characteristic of SIS technique was studied using bisphenol A (BPA) as a model compound. The sandwiched in-column silylation for the less volatile polar compounds effectively replaced polar hydrogen with trimethylsilyl group to reduce sample adsorption and band broadening. Meanwhile, multiple injections at the SIS technique contributed to increase the sensitivity quantitatively. The capability and limitation of this analytical approach were further investigated with various types of compounds such as hydroxyls, carboxylic acids, and amine.     

气相色谱-质谱法检测塑料食品包装材料中的五种挥发性有机物

建立了使用气相色谱-质谱仪检测塑料食品包装材料中常见的5种挥发性有机物(苯、甲苯、乙酸乙酯、乙酸丁酯、丁酮)的分析方法.实验中以欧盟标准EU 10/2011限定的4种模拟液为提取介质,二氯甲烷为有机萃取溶剂,对样品的前处理、色谱分离条件和质谱检测条件进行了优化.在最优化的实验条件下,这5种有机物能够完全分离,且在0.5~20.0mg/L浓度范围内线性较好,相关系数大于0.999 7,仪器精密度的相对标准偏差为1.08%~2.52%之间,样品在不同模拟液中的加标回收率介于81%~118%之间,最低检出限可达0.02 mg/m2.使用该方法测定了5种不同用途的塑料包装材料中的溶剂残留量,方法简便、快速、重现性好,完全能满足塑料包装材料中溶剂残留量的分析.     

超临界流体萃取-GC-MS分析西黄丸中挥发性成分

建立西黄丸中挥发油成分乙酸辛酯的含量测定方法,为西黄丸的质控标准提供依据。方法:超临界CO2萃取西黄丸中挥发油成分,采用气相色谱法测定乙酸辛酯含量;研究压力、温度、时间和粒度因素对挥发油得率与乙酸辛酯含量的影响,并进行了化学计量学分析。采用GC-MS分析了适宜条件的挥发油的成分。综合考虑挥发油得率和乙酸辛酯含量双指标,确定的西黄丸挥发油萃取条件为:粉碎粒度为80目,萃取压力为25 MPa,温度为40℃,时间为2 h。在此条件下,挥发油得率达到7.76%,乙酸辛酯含量达到0.72 mg·g^-1。通过指纹图谱、主成分分析(PCA)、正交偏最小二乘判别分析(OPLS-DA)化学计量学分析可知,不同萃取条件对所提取的挥发油物质组分及其含量没有显著性差异。GC-MS鉴定出的主要成分有(1S-endo)-2-甲基-3-亚甲基-2-(4-甲基-3--3-戊烯基)-二环[2.2.1庚烷、10α-羟基日本刺参萜、(±)-麝香酮、4-亚甲基-2,8,8-三甲基-2-乙烯基-双环[5.2.0]壬烷和2-甲基-4-(2,6,6-三甲基-1-环己烯-1-基)丁醛。结论:西黄丸挥发油成分适宜萃取条件,及建立的乙酸辛酯含量测定方法准确、可靠,为有效控制西黄丸质量,完善其质量标准及进一步的药效成分研究提供了科学依据。