蛇龙珠干红葡萄酒香气成分的GC-MS分析

研究宁夏贺兰山东麓地区蛇龙珠(Cabemet Gemischt)干红葡萄酒香气的化学成分,采用溶液萃取法提取蛇龙珠干红葡萄酒中的香气成分;用气相色谱一质谱进行分离测定,结合计算机检索技术对分离化合物进行鉴定,应用TIC峰面积归一法测定各成分的相对含量;分离出32个峰,鉴定出29个香气化学成分,共占其色谱流出组分总量的98．06％;其中相对含量以3-甲基丁醇(47．97％)、丁二酸二乙酯(16．49％)、苯乙醇(10．33％)、2-羟基丙酸乙酯(6．41％)、2-甲基丙醇(3．51％)、二氢化-2[3氢]-呋喃酮(2．07％)、2,3-丁二醇(1．93％)、四氢化2-甲基噻吩(1．68％)、乙酸乙酯(1．21％)、己醇(0．95％)等成分为主。     

色谱数据可视化及天然植物药指纹特征发现方法

提出一类色谱分析数据可视化方法，并用于发现天然植物药的化学指纹特征。选取中药材川芎作为典型研究对象，采用核主成分分析和空间投影变换法对色谱分析数据进行预处理，提取特征信息，再利用二维灰度映像对变换后的数据进行可视化表达，发现其化学指纹特征，从而直接反映出药材质量类别间的化学模式差异。将该方法用于辨识34个不同产地及等级的川芎样品，结果令人满意，证明其具有视觉模式分辨优点，是表达隐含特征指纹和辨识复杂化学物质体系的有力工具。     

可视化传感阵列对乌龙茶等级的快速识别研究

以金属二聚体卟啉,席夫碱过渡金属配合物和特异性染料为敏感材料,结合溶胶凝胶技术构建了一种新型可视化传感器阵列系统,对9种不同产地不同等级的乌龙茶进行了检测。采用主成分分析,聚类分析技术和欧式距离对检测结果进行分析。该传感阵列系统可以对乌龙茶的产地和等级实现准确的可视化识别与分类,检测耗时为3 min。通过主成分分析获得的前2个主成分所代表的乌龙茶63.6%的信息量即可以实现不同等级茶叶区分。9种乌龙茶的平行实验数据均能100%准确区分,且等级相同产地相同的样本优先聚成一簇。研究结果表明所构建的可视化阵列传感器是一种能快速准确区分乌龙茶等级与产地的方法,在实时快速检测茶叶品质方面有潜在的应用价值。     

红外光谱及Bayes信息融合技术的葡萄酒鉴别研究

建立了将检出限不同的近红外透射光谱技术和中红外衰减全反射光谱技术进行Bayes信息融合后用于葡萄酒鉴别的方法。分别采集3种品种和3种陈酿方式的干红葡萄酒的近红外透射光谱和中红外衰减全反射光谱,用PLS-DA法分别建立基于近红外光谱和中红外光谱的判别模型,用Bayes方法实现两种判别结果的融合修正。信息融合后的结果为:葡萄酒品种鉴别模型的建模集准确率为95.08%,检验集准确率为94.68%,葡萄酒陈酿方式鉴别模型的建模集准确率为98.91%,检验集准确率为98.75%;均优于单独采用一种光谱技术的判别结果。实验表明,信息融合技术有助于模型判别效果的提高,采用Bayes信息融合技术对葡萄酒品种和陈酿方式进行快速识别是可行的。     

昌黎原产地干红葡萄酒的三维荧光光谱特征研究

应用三维荧光光谱技术,研究了昌黎原产地不同品种和年份葡萄酒的三维荧光光谱特征.研究表明,2005年不同葡萄品种酒样的三维荧光特征峰的数目、位置和强度差异显著,可以区分各个品种酒样;而不同酿造年份的赤霞珠酒样均在λex/λem为A:260/365 nm、B:290/370 nm以及C:325/420 nm附近出现荧光特征峰,三维荧光特征峰出现位置一定,但荧光强度差异显著,可以用于区分各个酒样.因此三维荧光光谱技术能提供葡萄酒的指纹特征,据此可鉴别昌黎原产地不同品种和年份的葡萄酒.     

气相色谱结合化学计量学区分大米贮藏时间与产地

香气是衡量大米质量的一个主要因素,对大米的食用品质有重要影响。该文以顶空固相微萃取(SPME)技术为基础,采用气相色谱法分别分析了不同贮藏时间和不同产地大米样本的挥发性成分,通过主成分分析法(PCA)和偏最小二乘判别分析法(PLS-DA)对大米样本进行分类和判别分析。PCA及PLS投影图显示不同储藏时间的大米明显聚为4类,通过留一交叉验证法(LOO)计算PLS预报的准确率为96%,相对标准误差为8.2%。同时,PCA投影图中可将4个不同产地的大米样本进行区分,分类效果显著;所建PLSDA模型可靠,不同产地大米样本均能被准确识别,正确率为100%。以顶空固相微萃取/气相色谱检测大米中挥发性成分,利用主成分分析法和偏最小二乘判别分析法鉴别大米新鲜程度和产地具有可行性。     

可视化阵列传感器技术鉴别不同香型白酒

决定白酒香型的物质种类繁多,成分复杂.采用可视化阵列传感器技术对中国白酒五大香型的代表酒样进行检测,在可视化区分的基础上采用分层聚类分析、主成分分析等统计分析方法,对检测结果进行分析.不同香型的白酒在聚类分析中可以正确归类,利用主成分分析得到的前3个主成分所代表的白酒75.8%的信息量就可以将不同香型白酒完全区分开,表...     

基于气相色谱-离子迁移谱的不同产地西洋参挥发性成分分析北大核心CSCD

基于气相色谱-离子迁移谱(GC-IMS)技术对加拿大、美国、中国山东、辽宁、吉林5个产地的西洋参样品进行挥发性成分分析。从不同产地的西洋参样品中共鉴定出53种挥发性成分,包括醛类(13个)、醇类(13个)、酮类(10个)、酯类(7个)、萜类(3个)、吡嗪类(3个)、其他类(4个)。GC-IMS指纹图谱和偏最小二乘-判别分析(PLS-DA)得分图显示不同产地西洋参的挥发性成分存在显著差异,通过VIP值>1和含量比值>2筛选出23种差异挥发性成分。加拿大产2,5-二甲基吡嗪、α-蒎烯、丁酸乙酯、丙酸乙酯等成分的含量显著高于其它产区;美国产2-甲基-2-戊烯醛、2-庚酮、2-庚烯醛、2-辛烯醛等成分的含量较高;中国产芳樟醇等成分的含量较高。基于GC-IMS的挥发性成分分析可对不同产地的西洋参进行有效区分,为西洋参产地鉴别、溯源和品质评价提供了理论指导。     

脐橙果皮的室温和热辅助表面解吸常压化学电离质谱的比较

以脐橙果皮为研究对象,比较了室温和热辅助表面解吸常压化学电离源(DAPCI)的解吸电离特性,结合串联质谱技术,对果皮中香气、糖、黄酮类等主要成分进行了鉴定,并通过主成分分析(PCA)方法对热辅助DAPCI-MS所获外果皮指纹谱图信息进行分析,进而区分了3个不同产地脐橙。 结果表明,室温DAPCI-MS对脐橙果皮中的香气成分具有较强的解吸电离能力,而热辅助DAPCI-MS则更适合于分析果皮中的黄酮类和糖类及其衍生物。 DAPCI-MS具有灵敏度高、分析速度快等特点,有望成为农产品品质快速检测与产地识别研究的新方法。     

基于新型可视化学传感阵列的氨基酸快速识别

以卟啉和其衍生物及指示剂为传感元件,构建了一种对氨基酸敏感的可视传感阵列.可视化学传感阵列以交互响应的敏感元件组成阵列,对不同物质产生特异的响应,并通过信号识别处理系统,将检测结果以图谱的方式显示,实现检测的可视化.研究中筛选了对氨基酸敏感的36种化学物质,构建了6×6的传感阵列,使用自主研发的阵列数据采集与处理系统,对10种具有代表性的常见氨基酸进行了检测,氨基酸溶液与阵列的反应时间为5 min.对实验检测结果数据采用主成分分析和判别分析进行了计算和分析.实验结果显示,通过阵列响应的可视差图可以将浓度为375 μmol/L的10种氨基酸明显区分.判别分析结果显示,本可视阵列对氨基酸识别的准确率达到97%.二维主成分散点图和判别分析散点图对10种氨基酸都有显著分辨效果.本可视传感阵列可用于氨基酸的快速识别.     

Geographical origin of Sauvignon Blanc wines predicted by mass spectrometry and metal oxide based electronic nose

Analysis of 34 Sauvignon Blanc wine samples from three different countries and six regions was performed by gas chromatography-mass spectrometry (GC-MS). Linear discriminant analysis (LDA) showed that there were three distinct clusters or classes of wines with different aroma profiles. Wines from the Loire region in France and Australian wines from Tasmania and Western Australia were found to have similar aroma patterns. New Zealand wines from the Marlborough region as well as the Australian ones from Victoria were grouped together based on the volatile composition. Wines from South Australia region formed one discrete class. Seven analytes, most of them esters, were found to be the relevant chemical compounds that characterized the classes. The grouping information obtained by GC-MS, was used to train metal oxide based electronic (MOS-Enose) and mass spectrometry based electronic (MS-Enose) noses. The combined use of solid phase microextraction (SPME) and ethanol removal prior to MOS-Enose analysis, allowed an average error of prediction of the regional origins of Sauvignon Blanc wines of 6.5% compared to 24% when static headspace (SHS) was employed. For MS-Enose, the misclassification rate was higher probably due to the requirement to delimit the m/z range considered.     

Development of a mixed-mode solid phase extraction method and further gas chromatography mass spectrometry for the analysis of 3-alkyl-2-methoxypyrazines in wine

A new method for analysing 3-isopropyl-2-methoxypyrazine, 3-sec-butyl-2-methoxypyrazine and 3-isobutyl-2-methoxypyrazine in wine has been developed and applied to wine. The analytes are extracted from 25 mL of wine in a solid-phase extraction cartridge filled with 60 mg of cation-exchange mixed-mode sorbent. Analytes are recovered with triethylamine in dichloromethane and the organic extract is analysed by GC-SIM-MS using 3-isopropyl-2-ethoxypyrazine as internal standard. The detection limits of the method are in all cases under 1 ng/L, below the olfactory thresholds of the compounds in wine. The repeatability of the method is around 15% for levels in wine of 2 ng/L. Linearity is satisfactory and recoveries are in all cases close to 100% with RSD between 13% and 20%. The method has been applied to the analysis of 12 Chilean white and 8 Spanish red wines. The levels found suggest that 3-alkyl-2-methoxypyrazines can exert a significant sensory contribution to the aroma of Chilean Sauvignon Blanc wines, while most likely they play a nearly negligible role on traditional Ribera and Rioja Spanish red wines.     

Contribution of non-volatile and aroma fractions to in-mouth sensory properties of red wines: Wine reconstitution strategies and sensory sorting task

This work explores to what extent the aroma or the non-volatile fractions of red wines are responsible for the overall flavor differences perceived in-mouth. For this purpose, 14 samples (4 commercial and 10 reconstituted wines), were sorted by a panel of 30 trained assessors according to their sensory in-mouth similarities. Reconstituted wines were prepared by adding the same volatile fraction (coming from a red wine) to the non-volatile fraction of 10 different red wines showing large differences in perceived astringency. Sorting was performed under three different conditions: (a) no aroma perception: nose-close condition (NA), (b) retronasal aroma perception only (RA), and (c) allowing retro- and involuntary orthonasal aroma perception (ROA). Similarity estimates were derived from the sorting and submitted to multidimensional scaling (MDS) followed by hierarchical cluster analysis (HCA). Results have clearly shown that, globally, aroma perception is not the major driver of the in-mouth sensory perception of red wine, which is undoubtedly primarily driven by the perception of astringency and by the chemical compounds causing it, particularly protein precipitable proanthocyanidins (PAs). However, aroma perception plays a significant role on the perception of sweetness and bitterness. The impact of aroma seems to be more important whenever astringency, total polyphenols and protein precipitable PAs levels are smaller. Results also indicate that when a red-black fruit odor nuance is clearly perceived in conditions in which orthonasal odor perception is allowed, a strong reduction in astringency takes place. Such red-black fruit odor nuance seems to be the result of a specific aroma release pattern as a consequence of the interaction between aroma compounds and the non-volatile matrix.     

Combination of several mass spectrometry ionization modes: a multiblock analysis for a rapid characterization of the red wine polyphenolic composition

In the present study, direct flow injection mass spectrometry was investigated for rapid characterization of the polyphenolic composition of red wines. Atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) (in both positive and negative ion modes) have been simultaneously used for a more comprehensive analysis of the samples studied. In this way, four mass spectra have been recorded for each wine. Each spectrum was considered as a fingerprint related to the chemical composition. This methodology was applied to a large number of Beaujolais wines from different grades and different vintages.This data set was processed using a chemometrical multiblock analysis, which allowed to synthesize the whole information collected. The results obtained showed that the wine fingerprints address the composition of the main polyphenolic compounds present in the red wines and can discriminate groups of wines showing different polyphenolic compositions. Multiblock analysis appears as a very promising tool to deal with several data tables of multivariate signals in order to define, by combining the whole information, the best operating protocol according to the desired analytical objectives.     

Beyond the characterization of wine aroma compounds: looking for analytical approaches in trying to understand aroma perception during wine consumption

The volatile compounds present in wines are responsible for the quality of the wine aroma. The analysis of these compounds requires different analytical techniques depending on the type of compounds and their concentration. The importance at sensorial level of each compound should be evaluated by using olfactometric techniques and reconstitution and omission studies. In addition, wine aroma is influenced by other factors such as wine matrix, which could affect the compounds’ volatility, decreasing or increasing their concentration in the headspace above the wine. Moreover, when a wine is consumed, several oral physiological variables could affect aroma perception. The focus of this review is to outline the most recent advances in wine aroma analysis and the most innovative techniques in trying to elucidate the main factors that influence wine aroma perception during consumption.     

Changes in wine volatile compounds of varietal wines during ageing in wood barrels

Twelve single-variety wines were aged in new American oak barrels. A control wine of each variety without ageing in wood was also studied. The volatile aroma composition of these wines was analysed after the following combinations of time in wood and time in bottle: 0 months in wood plus 18 months in bottle, 4 months in wood plus 14 months in bottle, 9 months in wood plus 12 months in barrel and 12 months in barrel plus 6 months in bottle.The data obtained were studied by two different multivariate methods: factor analysis by principal components and stepwise linear discriminant analysis. The results obtained showed that the capacity of wine to extract the volatile compounds from the wood depended on the variety of grape used. Furthermore, it was also found that the changes in the volatile composition of the wines induced by the wood ageing were more important during the first 4 months. In addition, the volatile compounds studied allowed to differentiate and correctly classify the wines according to the time they had been in contact with the wood.     

Screening of key odorants and anthocyanin compounds of cv. Okuzgozu (Vitis vinifera L.) red wines with a free run and pressed pomace using GC‐MS‐Olfactometry and LC‐MS‐MS

The principal purpose of the present work is to characterize the aroma, aroma‐active, and anthocyanin profiles of Okuzgozu wines and to observe the effect of the pomace pressing technique on these parameters. A total of 58 and 59 volatile compounds were identified and quantified in free‐run juice wine (FRW) and pressed pomace wine (PW). Alcohols were found as the most dominant group among aroma compounds followed by esters and acids. However, among all these compounds, only 11 and 13 of them could be considered as key odorants in aromatic extracts of FRW and PW, respectively. According to GC‐MS‐O analysis, ethyl octanoate (fruity), phenyl ethyl acetate (fruity), and 2‐phenyl ethanol (flowery) were found as the main contributors to the overall scent of both wines. Beyond the aroma profiles, anthocyanin contents of both types of wines were also investigated, and total 14 and 15 anthocyanins were identified and quantified in FRW and PW. Malvidin‐3‐glycoside and its acetyl and coumaroyl forms were identified as the dominant anthocyanins in both wines. It is worth noting the pressing application (2.0 atm) led to an increase of some unpleasant notes in the aroma providing chemical, pharmacy, and fermented aromas in wine. On the other hand, the wines produced with pressed pomace presented higher amounts of anthocyanins.     

Commercial Mannoproteins Improve the Mouthfeel and Colour of Wines Obtained by Excessive Tannin Extraction

In the production of red wines, the pressing of marcs and extended maceration techniques can increase the extraction of phenolic compounds, often imparting high bitterness and astringency to finished wines. Among various oenological products, mannoproteins have been shown to improve the mouthfeel of red wines. In this work, extended maceration (E), marc-pressed (P), and free-run (F) Sangiovese wines were aged for six months in contact with three different commercial mannoprotein-rich yeast extracts (MP, MS, and MF) at a concentration of 20 g/hL. Phenolic compounds were measured in treated and control wines, and sensory characteristics related to the astringency, aroma, and colour of the wines were studied. A multivariate analysis revealed that mannoproteins had a different effect depending on the anthocyanin/tannin (A/T) ratio of the wine. When tannins are strongly present (extended maceration wines with A/T = 0.2), the MP conferred mouthcoating and soft and velvety sensations, as well as colour stability to the wine. At A/T = 0.3, as in marc-pressed wines, both MF and MP improved the mouthfeel and colour of Sangiovese. However, in free-run wine, where the A/T ratio is 0.5, the formation of polymeric pigments was allowed by all treatments and correlated with silk, velvet, and mouthcoat subqualities. A decrease in bitterness was also obtained. Commercial mannoproteins may represent a way to improve the mouthfeel and colour of very tannic wines.