固相微萃取分析海南地区黑胡椒粉风味成分

采用固相微萃取采集海南地区黑胡椒粉的挥发性成分,用气相色谱-质谱法分析鉴定,并用总离子流色谱峰的峰面积进行归一化定量分析其风味成分,共鉴定出α-蒎烯、β-蒎烯、3-蒈烯、柠檬烯、异松油烯和石竹烯等15种化合物。     

黄牛木果实挥发油的化学成分研究

采用气相色谱-质谱联用技术GC-MS对黄牛木[Cratoxylum cochinchinense (Lour.) Blume]果实挥发油的化学成分进行分析,共鉴定出46种化合物,占其总量的95.361%。在已鉴定的46种化学成分中,含量较高的成分依次为β-石竹烯(24.060%)、油酸(14.629%)、反式-β-罗勒烯(11.572%)、石竹烯氧化物(11.447%)、α-蒎烯(7.540%)。     

超声波萃取番橄榄挥发油化学成分的GC-MS分析

采用超声波法萃取番橄榄不同时期的果实和叶片挥发油,用气相色谱-质谱法对挥发油中各种化学成分进行分析和鉴定。共鉴定出48个化合物,其中37个成分为在该植物中首次报道。其果实挥发油主要成分有:1R-α-蒎烯,22,23-二氢豆甾醇,β-蒎烯,2,2'-亚甲基双-(4-甲基-6-叔丁基苯酚),维生素E;叶片挥发油主要成分有:维生素E,22,23-二氢豆甾醇,1R-α-蒎烯,三十一烷,植醇,β-石竹烯。黄熟的果实中萃取的挥发油的总量明显高于青果,而不同时期的绿叶中萃取的挥发油总量则较为接近。     

长叶榧叶部油挥发性成分的色谱/质谱分析研究

采用气相色谱/质谱(GC-MS)联用法测定了长叶榧叶部精油的挥发性成分,初步发现其主要成分是柠檬烯、反式α-蒎烯、β-蒎烯、顺式α-蒎烯、3-莰烯、6,6-二甲基-2-亚甲基-环庚烷、β-月桂烯,其含量分别为32.2%、12.5%、7.1%、6.6%、6.6%、5.5%、4.4%.     

苎叶蒟叶油的化学成分

采用水蒸气蒸馏法提取苎叶蒟叶中的挥发油,并用气相色谱-质谱联用法对其化学成分进行分析。结果表明：共分离鉴定出41个化合物,占总峰面积的92.87 %;苎叶蒟叶挥发油的主要成分以醇类化合物和烯类化合物为主,醇类化合物有11种,占总峰面积的58.25 %,其中以橙花叔醇2和叶醇的含量为最高,分别为41.98 %和10.04 %;烯类化合物有23种,占总峰面积的26.01 %,其中,以石竹烯和β-蒎烯的含量为最高,分别为9.44 %和2.31 %。     

不同月份黑胡椒精油化学成分的研究

以4个不同月份胡椒鲜果为原料制备成黑胡椒,通过GC-MS对4个不同月份黑胡椒精油的化学成分进行分析。结果表明：（1）胡椒不同月份对胡椒精油化学成分的种类与含量都有显著影响。（2）不同月份黑胡椒精油中含量较多的化学成分主要有3-蒈烯、柠檬烯、石竹烯、α-石竹烯、β-蒎烯、β-月桂烯、δ-榄香烯和α-蒎烯等8种烯类物质。     

“土法”提取杉木屑精油化学成份GC/MS分析及探讨

“土法”提取精油因其设备简单、拆装方便、容易运输、易操作、成本低等特点,在偏远农村广泛使用,本试验对“土法”水蒸汽蒸馏方法提取精油进行化学成份的GC/MS分析,共分出71个色谱峰,采用GC 峰面积归一化法进行定量,其中鉴定出47个化合物,占该精油总量的91.8%。其主要成分为α-柏木烯(22.4%)、柏木醇(20.07%)、α-松油醇(4.29%)、α-蒎烯(2.26%)等,本试验为更好的利用“土法”提取杉木屑精油提供参考,为改进“土法”提取设备提供可靠依据。     

不同加工方法对胡椒精油化学成分的影响

以70%～80%成熟度的胡椒鲜果为原料,通过不同加工方法制备黑胡椒、白胡椒与青胡椒,并通过GC-MS对其胡椒油化学成分进行分析.结果表明:(1)加工方法不同对胡椒油化学成分的种类与含量都有显著影响.(2)3-蒈烯、柠檬烯、反式-石竹烯、β-蒎烯、L-水芹烯、α-蒎烯6种烯类是3种胡椒精油中含量较多的化学成分.其中,黑胡椒精油中特有成分4种:5-甲基-3-己醇、氨基甲酸叔己脂、木罗烯、α-蛇床烯;白胡椒精油中特有成分7种:2-甲基-2-戊醇、3-甲基-3-戊醇、γ-萜品烯、樟脑、乙酸松油酯、β-檀香烯、δ-杜松烯;青胡椒精油中特有成分5种:朱栾倍半萜、γ-古芸烯、4-甲基-3-己醇、2,5-二甲基-2-己醇、反式3-蒈烯-2-醇.     

胡椒梗中胡椒碱及香气物质研究

对电热鼓风干燥和真空冷冻干燥的胡椒梗主要组分进行分析,并采用固相微萃取-气相色谱-质谱联用法(SPME-GC-MS)对两种干燥方式下胡椒梗中的香气成分进行研究。结果发现,胡椒梗中胡椒碱含量0.07～0.10 g/hg、脂肪含量约0.9%、粗蛋白含量17%～19%、总酚含量2.5%～2.8%、维生素C含量2.8～5.6 mg/hg。胡椒梗中鉴定出的主要化学成分为：芳樟醇、δ-榄香烯、古巴烯、石竹烯、律草烯、杜松烯含量较多,以石竹烯含量最高(≥52.55%)。     

胡椒果与胡椒叶精油化学成分分析

采用水蒸气蒸馏法提取胡椒鲜果、黑胡椒、白胡椒和胡椒叶中的精油,得率分别为1.46%、1.77%、2.30%和1.25%。对精油进行GC-MS分析,分别鉴定得到38、31、36和63种化学物质,δ-榄香烯、3-蒈烯、D-柠檬烯、α-古巴烯、石竹烯和律草烯在果与叶中含量均较高,其中叶中δ-榄香烯含量占38.54%;蒎烯、月桂烯、α-水芹烯和间伞花素在果中含量较高,而在叶中含量较低;甘香烯、α-荜澄茄油烯、β-榄香烯、α-古芸烯、β-古巴烯、α-蛇床烯、花柏烯、4-异亚丙烯-7-甲基-6-亚甲基-2-辛烯酸甲酯和桉油烯醇在叶中含量较高,而果中含量较低或没有。此外,采用电子鼻方法可有效区分胡椒粉和胡椒叶。     

残留溶剂及平衡条件的研究

在顶空气相色谱法测定食用植物油中的残留溶剂的基础上,对残留溶剂顶空分析的平衡条件进行研究。研究结果表明：顶空分析的灵敏度与平衡温度、平衡时间所决定的气相提取效率有关;在一定温度范围内组分的峰面积随平衡温度的增加呈指数规律递增,提高平衡温度有利于提高检测的灵敏度;平衡时间对平衡的影响效果不及平衡温度显著。     

Volatile Organic Compounds,Indole, and Biogenic Amines Assessment in Two Mediterranean Irciniidae (Porifera,Demospongiae)

Solid phase microextraction (SPME) coupled to gas chromatography-mass spectrometry (GC-MS) was employed for the headspace determination of the volatile organic fraction emitted by two of the most common Mediterranean demosponges, Ircinia variabilis and Sarcotragus spinosulus, and of indole and some biogenic amines released by sponges in an aqueous medium. A total of 50/30 µm divinylbenzene/carboxen/polydimethylsiloxane and 75 µm carboxen/polydimethylsiloxane fibers were used for the headspace extraction of low molecular weight sulfur compounds from a hermetically sealed vial containing sponge fragments, while the direct immersion determination of indole and biogenic amines was performed. The biogenic amines were extracted after in-solution derivatization with isobutyl chloroformate. All analytical parameters (linearity, limits of detection, and quantification, precision, and recovery) were evaluated for indole and biogenic amines. SPME-GC-MS proved to be a reliable means of highlighting the differences between molecules released by different sponges, principally responsible for their smell. The combined approaches allowed the identification of several volatile compounds in the headspace and other molecules released by the sponges in an aqueous medium, including indole and the BAs cadaverine, histamine, isobutylamine, isopentylamine, propylamine, 2-phenylethylamine, putrescine and tryptamine. The results obtained represent a further contribution to the picture of odoriferous molecules secreted by sponges.     

Dough and bread made from high- and low-protein flours by vacuum mixing: Part 2. Yeast activity,dough proofing and bread quality

The combined effects of reduced mixer headspace pressure and mixing duration on the yeast activity, proofing and quality of dough and bread made from both high-protein flour (HPF) and low-protein flour (LPF) were addressed in this study. Rheofermentometer analysis showed that a reduction in mixer headspace pressure up to 0.08 MPa did not affect the overall gassing power of yeast in either of the two dough matrices. An increase in mixing duration sped up the mass transfer rate of CO₂ at the initial stage of fermentation, leading to a faster expansion of dough volume at the beginning. Moreover, an increase in mixing time promoted dough development and gas inclusion, which resulted in a increased volume of dough and bread, as well as a softer texture of both baked bread and steamed bread. In general, reduced headspace pressure produced baked bread of smaller volume, denser structure and harder texture. On the other hand, vacuum mixing produced steamed bread with softer texture without significantly changing the bread’s volume and porosity.     

顶空固相微萃取-气质联用法分析白茶的香气成分

采用顶空固相微萃取-气质联用法分析比较了白毫银针和白牡丹两种典型白茶及同一品种鲜叶制成的绿茶、红茶的香气成分。结果表明,白茶与绿茶、红茶在香气组成上存在明显差异。白茶的香气成分以醇类化合物为主,在白毫银针和白牡丹中含量分别达到70.74%和60.13%,明显高于绿茶（27.56%）和红茶（45.30%）;白茶的酯类含量高于绿茶和红茶,醛类、酮类和碳氢化合物等含量低于绿茶和红茶,酸类、杂氧化合物等在白茶中未检出。β-芳樟醇及其氧化物、香叶醇、水杨酸甲酯、苯乙醇、苯甲醇等是白茶香气的主要成分,分别占白毫银针香气提取物总量的35.70%、23.47%、5.87%、7.06%、2.02%,分别占白牡丹香气提取物总量的35.40%、11.94%、10.72%、6.80%、2.71%。     

Analysis of Headspace Compounds of Distillers Grains using SPME in Conjunction with GC/MS and TGA

Chemical composition of headspace compounds of distillers grains was investigated using solid phase microextraction (SPME) along with GC/MS and TGA. Dryer feed (DF) and distillers dried grains (DDG) from a local distillery were utilised for this study. A SUPELCO 75 μm Carboxen/PDMS SPME fibre was found suitable for extraction of analytes from grains. Samples were placed in small vials (40 mL from SUPELCO) filled to one-third of their capacity. SPME was exposed to the headspace for 1 to 2 h. The fibre was then thermally desorbed in GC injection port for separation and identification. The gas chromatogram showed as many as 64 compounds eluting out of the column, the number being greater in DF as compared to DDG. Thermogravimetric analysis (TGA) was performed on the grains to study the oxidative stability of the compounds. SPME fiber was inserted directly into TGA purge gas outlet to study the compounds being evolved. Three weight loss transitions were observed in the TGA curve of DF and DDG. The components from the three transitions were captured by SPME and analysed by GC/MS for identification. TGA helped in determining the degradation stages of grains thereby indicating the temperature limits in drying grains. Difference between the heated and unheated DF and DDG have been discussed in detail.     

3种不同萃取方法对黑胡椒香气物质的气质联用分析

为探究不同提取方法对黑胡椒挥发性成分的影响,本研究以黑胡椒为材料,利用顶空固相微萃取法（HS-SPME）、戊烷:乙醚（1:1）溶剂萃取法和甲基叔丁基醚（MTBE）溶剂萃取法对黑胡椒中的香气成分进行提取,结合气相色谱质谱联用法（gas chromatography-mass spectrometry）和主成分分析法（PCA）对提取的香气物质进行分析。3种提取方法共得到6类（烯类、醇类、酚类、烃类、崁类、烯类氧化物）33种物质。戊烷:乙醚（1:1）溶剂萃取法、MTBE溶剂萃取法及顶空固相微萃取法分别检测到25、23、27种挥发性化合物,其中,相对含量较高的化合物均为3-蒈烯、柠檬烯、β-石竹烯、β-蒎烯。2种溶剂萃取法中,戊烷:乙醚（1:1）溶剂萃取法检测到的特有化合物有α-松油烯、α-松油醇、β-金合欢烯;与2种溶剂萃取法相比,顶空固相微萃取法（HS-SPME）检测到的特有化合物有樟脑、4-萜烯醇、2-(4-甲基苯基)丙-2-醇、橙花醇、香树烯、β-甜没药烯和愈创兰油烃。结合主成分分析得出,β-蒎烯、3-蒈烯、柠檬烯、β-石竹烯对黑胡椒香气风味贡献率较大,其中顶空固相微萃取法（HS-SPME）与2种溶剂萃取法所得成分差异明显。在溶剂萃取法中,戊烷:乙醚（1:1）溶剂萃取法优于MTBE溶剂萃取法。溶剂萃取法与顶空固相微萃取法所得物质在种类与数量上均存在差异。在胡椒香气物质检测时,将2种方法相结合可以更大程度保证所得化合物种类的丰富性和全面性。     

Volatile organic compounds as a diagnostic marker of late blight infected potato plants: A pilot study

Volatiles from potato plants infected with Phytophthora infestans (Mont.) de Bary were monitored by in situ headspace sampling. The sampling was done in four periods i.e. 28–42, 52–66, 76–90, and 100–114 h after inoculation (HAI). The headspace samples were analyzed by a gas chromatography–flame ionization detector (GC–FID) to assess the differences in volatile fingerprints between the infected-plant group and control groups, i.e. non-inoculated-plant and empty-vessel groups. The samples were subsequently analyzed by gas chromatography–mass spectrometry to identify specific peaks observed by GC–FID. Spore germination, infection, symptom development and sporulation were also monitored to ascertain the disease developmental stage when marker volatiles were first generated. The first symptoms of infection were visible after two days. Three marker volatiles i.e. (E)-2-hexenal, 5-ethyl-2(5H)-furanone and benzene-ethanol were found in the third and fourth trapping periods (3–4 days after inoculation) when sporangiophores were already formed. The volatile metabolites from blighted plants could be applied for sensor development to detect the occurrence of the disease in the field as well as for investigation of volatile production in relation to plant responses to infection.     

不同极性色谱柱在滇红香气成分分析中的对比研究

采用顶空固相微萃取(HS-SPME)对滇红的香气成分进行富集,分别使用两种不同极性的色谱柱进行色谱分离,气质联用(GC-MS)检测分析,比较了非极性色谱柱HP-5MS和极性色谱柱CP-Wax对红茶香气成分分离效果的差异。结果表明,两种不同极性色谱柱对红茶香气成分的分离效果均表现良好,但分析结果存在一定的差异。因此在对红茶中不同的香气成分进行研究分析时,应根据分析目标的不同选择合适的色谱柱。     

顶空固相微萃取结合GC/MS分析普洱大叶种乔木茶花香气成分

运用全自动顶空固相微萃取技术(Headspace solid-phase microextraction,HS-SPME)对云南普洱地区生产的大叶种乔木茶花样品中的挥发性成分进行提取,并采用气相色谱-质谱技术(Gas chromatography-mass spectrometry,GC/MS)进行定性定量分析;同时与该类茶树制成的普洱生茶的挥发性成分进行了比较。结果表明,从普洱大叶种乔木茶花和普洱生茶中鉴定出挥发性成分分别为9种和67种,主要以碳氢化合物和醇类挥发性化合物为主。通过对比发现,普洱大叶种乔木茶花中的挥发性成分均存在于普洱生茶的挥发性成分之中,这些成分均具有一定香气特性。本研究表明,普洱大叶种乔木茶花可作为独立饮品,有类似于茶叶的香味感受,或者可与茶叶混合以提高或改善茶叶产品的香气风味。