Analysis of the headspace volatiles of freshly brewed arabica coffee using solid-phase microextraction

ABSTRACT:  Headspace volatiles of freshly brewed drip coffee were investigated by gas chromatography/mass spectrometry (GC/MS) and gas chromatography/olfactometry (GC/O, CharmAnalysis™) analyses. For this purpose, a solid-phase microextraction (SPME) sampling method for the headspace volatiles of freshly brewed drip coffee was developed. SPME fiber coated with divinylbenzene (DVB)/carboxen/polydimethylsiloxane (PDMS) was selected from 6 types, and sampling time was determined at 2 min. The headspace coffee volatiles stayed constant in proportion for the first 2 min to keep the freshness of the brewed coffee aroma. Using this sampling method, the headspace volatiles of freshly brewed drip coffee (Ethiopian arabica coffee, roast degree: L value; 23) were examined by GC/MS and GC/O analyses. From the GC/O results, 1-(3,4-dihydro-2 H -pyrrol-2-yl)-ethanone (nutty-roast odor) and 4-(4'-hydroxyphenyl)-2-butanone (raspberry ketone, sweet-fruity odor) were newly detected as components in the aroma of coffee.     

Volatile components of raw and smoked black bream (Brama raii) and rainbow trout (Oncorhynchus mykiss) studied by means of solid phase microextraction and gas chromatography/mass spectrometry

Solid phase microextraction followed by gas chromatography/mass spectrometry of raw and smoked black bream and rainbow trout was carried out. The volatile components of the raw fish belong to a limited number of groups of compounds. Raw black bream has a higher presence of acids than raw trout, while the latter contains more alcohols, hydrocarbons, esters and phenol derivatives; both contain similar concentrations of saturated aldehydes. The volatiles of the smoked fish basically comprise the compounds also detected in the raw fish together with others produced during the processing. Smoke components detected in both smoked fish species were mainly phenol, guaiacol and syringol derivatives, ketones, acetic acid and some polycyclic aromatic hydrocarbons. Smoked black bream contained a higher number and higher concentrations of smoke components than smoked rainbow trout. Large variations in concentrations of smoke components in the smoked fish samples indicated that the smoking process had not been totally homogeneous. The presence of autoxidatively derived compounds, such as unsaturated aldehydes, was mainly detected in some smoked bream samples, showing that this degradation process is not occurring homogeneously. The usefulness of the applied techniques for the study of volatile components of raw and smoked fish is shown. © 2002 Society of Chemical Industry     

Volatile compounds on the surface and within Iberian dry-cured loin

The profile of volatile compounds from external and internal areas of Iberian dry-cured loin was studied by headspace solid-phase microextraction. Higher levels of 16 volatile compounds (hexane, decane, 3-methylbutanal, several sulphur compounds and some aromatic hydrocarbons) were detected in the outer part of the loins. These differences could be owing to several factors, such as greater exposure to oxygen and dehydration conditions in the surface of the product, which favour oxidation reactions and Strecker degradation of amino acids. Moreover, the addition of spices on the surface and the proximity of a mould layer growing on the surface of the product could also contribute to the higher levels of these compounds on the external layer. However, other sulphur compounds coming from spices showed similar levels on the surface and within the loins. This different behaviour could be a consequence of different diffusion rates depending on the features of the compound and the matrix.     

SDE和SPME法对鲊海椒发酵中香气组成的比较分析

为确定评价鲊海椒挥发性香气组成的最优方法,以粳米粉为淀粉原料制备鲊海椒,采用固相微萃取（solidphase microextraction,SPME）法和同时蒸馏萃取（simultaneous distillation extraction,SDE）法并结合感官评价比较研究其在发酵过程中风味物质的变化。结果发现,SPME法萃取发酵0、45 d和90 d鲊海椒挥发性成分种类分别为76、131 种和122 种,SDE法挥发性成分分别为23、42 种和82 种;随着发酵时间的延长,SDE法挥发性香气成分增加,而SPME法在发酵45 d时挥发性香气物质种类达峰值并保持稳定。酯类是鲊海椒发酵过程中主要的挥发性成分,采用SPME法和SDE法萃取发酵45～90 d鲊海椒,分别检出挥发性酯类42～50 种（相对含量46.7%～55.3%）和15～27 种（相对含量60.28%～67.28%）;SPME法检出较多醇类、醛类,发酵45～90 d鲊海椒醇类14～21 种（相对含量15.7%～22.6%）和醛类17 种（相对含量5.8%～12.3%）。SPME法可萃取得到更多低沸点、小分子化合物;而SDE法得到更多高沸点化合物;感官评定显示发酵45 d后的鲊海椒色泽鲜艳,具有特殊的酸味和醇香味。结果表明,采用SPME法结合SDE法评价鲊海椒挥发性香气组成更加全面客观,鲊海椒适宜发酵时间为45～90 d。     

不同时期套袋对“瑞光19号”油桃果实挥发性成分及着色的影响

为探讨不同时期套袋对油桃果实风味品质的影响,对陕西关中主栽油桃品种"瑞光19号"进行了3个不同时期的桃专用果袋套袋实验。以不套袋果实为对照,利用固相微萃取-气相色谱-质谱联用技术测定果实的挥发性物质。结果表明:供试桃共检测到83种挥发性物质。其中特征香气物质的总含量从高到低的顺序为:对照盛花后40 d套袋(2014年5月14日)盛花后45 d套袋(2014年5月19日)盛花后50 d套袋(2014年5月24日)。与不套袋果实相比,不同时期套袋果实均提高了醇类物质的相对含量,但降低了醛类、酯类和酮类物质的相对含量;本实验共检测到3种内酯类和2种萜类特征香气物质,其中芳樟醇和γ-癸内酯存在显著相关性;此外,套袋主要影响了"瑞光19号"果实的香气成分和果面着色情况,果实套袋时间越早着色越好,其中盛花后40 d套袋后果实的着色好并且果香味浓,综合表现最佳。     

顶空固相微萃取-气相色谱/质谱分析啤酒微量香味组分的研究

采用顶空固相微萃取 (HS SPME)技术结合气相色谱 质谱法 (GC/MS)对啤酒的微量香味组分进行了分析研究 ,共分离和鉴定了 41种化合物 ,它们分别属于酯类、醇类、酸类、醛类、酚类、含硫化合物和含氧杂环化合物。这些结果拓展了SPME技术在啤酒香味组分研究中的应用 ,它不仅可成为高级醇、挥发酯定量分析的基础 ,而且使啤酒酵母味、酒花香、氧化味的量化评价成为可能。文中除表列了分析结果外 ,还对SPME方法的特点及所分析组分与啤酒质量控制之间的相关性作了研讨。     

黑果腺肋花楸酒与赤霞珠葡萄酒香气物质对比分析

以赤霞珠葡萄酒为参照分析黑果腺肋花楸发酵酒的香气物质组成并进行感官品评,评价其酿酒潜质,为开发适宜消费者口味的黑果腺肋花楸酒提供参考。采用顶空固相微萃取结合气相色谱-质谱分析酒的香气物质成分。结果显示：黑果腺肋花楸酒香气物质含量为赤霞珠葡萄酒的2.73 倍,香气物质种类分别为41 种和40 种,其中共有的18 种。醇类物质含量最高,分别占总香气的62.11%和73.87%。依据香气活度值,酯类物质对酒的香气贡献最大,分别为36.57%和22.04%。黑果腺肋花楸酒的主体香气物质是大马士酮、辛酸乙酯、正己酸乙酯和乙酸异戊酯,而赤霞珠葡萄酒则为α-紫罗酮、辛酸乙酯、正己酸乙酯和苯乙醛。2 款酒中共有香气物质对香气贡献占比分别为34.20%和21.81%,说明具有一定的相似性,而大马士酮和α-紫罗酮对酒香气值的贡献分别为63.22%和76.36%,形成了各自酒的特色。经感官品评,黑果腺肋花楸酒比赤霞珠葡萄酒总得分高2 分,黑果腺肋花楸作为黑色浆果具有开发酿酒的价值。     

顶空气相分析技术及其应用

综述了现代顶空分析方法的分类及其应用。顶空气相色谱法(HS-GC)是测定样品中痕量易挥发化合物的重要分析方法,近年快速发展。是一项有着广阔应用前景的技术。     

啤酒中酒花香组分分析方法的研究及其在啤酒酒花香气质量评定中的应用

采用顶空固相微萃取-GC／MS技术，建立了啤酒中酒花香组分的分析方法，可以准确测定里哪醇、β-香茅醇、α-萜品醇、香叶醇、反式-橙花叔醇、乙酸香茅酯、香叶酸甲酯、乙酸香叶酯等8种酒花香组分。应用本方法测定了市售不同品牌啤酒的酒花香组分含量，通过统计分析并结合感官评定，评价了不同品牌啤酒的酒花香质量，本方法的建立有助于啤酒酒花香的量化评定。     

顶空固相微萃取- 气相色谱/质谱法分析霸王花挥发性成分

目的：探索分析霸王花挥发油化学成分的方法。方法：采用聚二甲基硅氧烷萃取头室温顶空微萃取20min、初始柱温60℃、程序升温至250℃、进样口温度250℃的气相色谱条件,EI 离子源、电子能量70eV 的质谱条件进行气相色谱/ 质谱法分析。结果表明：共鉴定出49 种化合物,主要挥发性成分及其含量为倍半萜及其含氧衍生物(27.78%)、脂肪族化合物(25.14%)、酯(14.40%)、2,6- 二叔丁基对甲酚(10.08%)和硅氧烷类化合物(6.27%)。结论：无溶剂的顶空萃取- 气相色谱/ 质谱联用技术可作为霸王花挥发性成分分析的有效方法。