Monitoring the oxidation of almond oils by HS-SPME–GC–MS and ATR-FTIR: Application of volatile compounds determination to cultivar authenticity

In this study, the oxidative process of Spanish and American almond oils was monitored by using headspace solid-phase microextraction/gas chromatography–mass spectrometry (HS-SPME/GC–MS) and attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR). Oxidative stability of samples was evaluated after thermal treatment at 100 °C for 1, 3, 5, 7, 10, 15 and 20 days, in order to accelerate the lipid oxidation process. Variations observed in bands of infrared spectra were used to monitor the progress of the oxidation process of almond oils. HS-SPME–GC–MS was used for isolation and determination of volatile compounds in oxidised almond oils. The following aldehydes were identified in all samples: hexanal, (E)-2-heptenal, (E)-2-octenal, nonanal, (E)-2-nonenal, (E,E)-2,4-nonadienal and (E,E)-2,4-decadienal. Determination of volatile compounds resulting from lipid oxidation from three different almond cultivars (Spanish Guara and Marcona and Butte from USA) was performed to obtain a set of parameters for discrimination between Spanish and American cultivars. Successful discrimination was obtained in samples kept under thermal treatment for 7 days, by using HS-SPME/GC–MS combined with multivariate stepwise linear discriminant analysis (LDA).     

Direct enantiomeric analysis of Mentha essential oils

A rapid and fully automated screening of chiral compounds in essential oils, aimed to the selection of natural sources of pure enantiomers of limonene and carvone, is performed by using on-line coupled reversed phase liquid chromatography with gas chromatography and mass spectrometry (RPLC–GC–MS). Essential oils obtained from Mentha spicata and Mentha piperita were analysed by direct injection into RPLC. The reported procedure includes fractionation and clean-up in RPLC, selection of the fraction to be transferred from RPLC to GC, trapping and concentration of the target compounds in the interface, thermal desorption and, finally, enantiomeric resolution and identification of chiral compounds by GC–MS. The presence of (S)-limonene and (R)-carvone as the unique enantiomeric forms existing for both compounds could be unambiguously established by transferring different volume fractions from RPLC to GC. Data obtained demonstrate high separation efficiency and well tunable selectivity in the on-line coupled RPLC–GC–MS analysis of chiral compounds.     

Variable selection for partial least squares analysis of soluble solids content in watermelon using near-infrared diffuse transmission technique

This work is focused on the variable selection in building the partial least squares (PLS) regression model of soluble solids content (SSC) that is used to evaluate quality grading of watermelon. The spectra were obtained by the near infrared (NIR) spectrometer with the device designed for on-line quality grading of watermelon and the spectra of 680–950 nm were adopted to analysis. The variable selection was based on Monte-Carlo uninformative variable elimination (MC-UVE) and genetic algorithm (GA). In comparison of the performances of the full-spectra (680–950 nm) PLS regression model and the feature wavelengths PLS regression model showed that the MC-UVE–GA–PLS model with baseline offset correction combined multiplicative scatter correction (MSC) pretreatment was much better and 14 variables in total were selected. The correlation coefficients between the predicted and actual SSC were 0.885 and 0.845, the root mean square errors were 0.562 °Brix and 0.574 °Brix for calibration and prediction set, respectively. This work can make a great contribution to the research of on-line quality grading for watermelon nondestructively.     

Use of enzymes to elucidate the factors contributing to bitterness in rye flavour

In spite of the health-beneficial character of whole grain rye its use may be limited because of bitter taste. The impact of non-volatile chemical compounds on the bitter taste of rye was analysed by the aid of enzymatic hydrolysis, releasing potentially flavour-active compounds from the rye matrix. Whole grain rye flour–water suspension was treated with hydrolytic enzymes, whereafter portions of the rye suspensions were baked into crackers, assessed for their sensory profile as well as solubilised hydrolysis products. Heat treatment reduced the perceived bitterness. The treatment with enzyme preparation with high protease activity increased the bitterness of rye and also wheat flour both as suspension and as crackers. Other enzymes tested (with high polygalacturonase, endo-glucanase, xylanase or amyloglucosidase activity) had no significant impact on the perceived bitterness. Thus, small molecular weight peptides were considered to be a significant contributor to the bitter note of rye.     

Interactions among salty, sour and bitter compounds

The human gustatory system is capable of responding to and processing the taste of solitary compounds in water. However, the taste system rarely contacts solitary compounds outside the laboratory and has surely evolved to process complex mixtures of sapid chemicals, such as occur in virtually all foods. This review will focus primarily on the lesser-studied interactions between pairs of salty, sour and bitter compounds. Pair-wise interactions among these three taste qualities should be of interest because they constitute a significant proportion (∼30–50%) of possible binary taste interactions. In general, salts and acids enhance each other at moderate concentrations but suppress each other at higher concentrations. Bitter compounds and acids can either enhance or suppress each other depending on the concentrations, the food stimuli and the experimental methods involved. Sodium salts and bitter compounds generally interact so that bitterness is suppressed to some variable degree and the saltiness is unaffected. As will be described below, there are exceptions to all of these generalities.     

Influence of locally-selected yeast on the chemical and sensorial properties of Albariño white wines

The use of selected yeast strains with improved or novel properties may promote wines with special and original quality attributes. In this paper, changes in the chemical composition (aroma compounds and polyphenols) and sensorial properties of Albariño white wines elaborated with the same must and selected yeast (named as 1, 2 and 3) have been studied in comparison with wines subjected to non-inoculated fermentation (control wine). The results indicated that yeast strain can significantly influence the aroma and polyphenol composition of the wines. Wines elaborated with strain 1 had a higher concentration of terpenes and norisoprenoids, which are compounds closely associated with the fruity and fresh character of Albariño white wines. These same wines had a lower concentration of flavan-3-ols, closely associated with the astringency and bitterness of the wine and the lowest browning potential. The formal sensory analysis conducted by 8 trained judges showed that wines elaborated with strain 1 were preferred by the tasting panel. Therefore, the selection of yeast strains could offer the possibility to modulate sensorial attributes related with the aroma and phenol composition in Albariño white wines.     

Quantitative analysis of volatiles in transesterified coconut oil by headspace-solid-phase microextraction-gas chromatography–mass spectrometry

A simple and fast headspace-solid-phase microextraction (HS-SPME) method coupled with gas chromatography–mass spectrometry (GC–MS) was developed for the analysis of volatile compounds in transesterified coconut oil by applying solvent dilution. Solvent dilution conditions (solvent type and solvent amount) and HS-SPME sampling parameters (adsorption temperature and time) were optimised through monitoring the adsorption result of the selected volatiles (octanoic acid esters) in transesterified coconut oil samples. The incubation of methanol (800 μl)-diluted oil (200 μl) sample at 60 °C for 30 min led to the best result. The method was further validated by determining the calibration linear range, correlation coefficient (R²), accuracy, precision, limit of detection and limit of quantification through spiking standards into the blank matrix consisting of coconut oil and methanol. This method may also be applicable for detection and determination of volatile compounds in other transesterified oil samples.     

Structure determination and sensory evaluation of novel bitter compounds formed from β-acids of hop (Humulus lupulus L.) upon wort boiling

In order to screen for the bitter compounds generated from hop-derived precursors during the wort boiling process, an ethanolic hop extract was fractionated; the fractions obtained were thermally treated under model wort boiling conditions and, then, sensorially evaluated for their bitterness. Besides the isomerisation of the α-acids into the intensely bitter iso-α-acids, the bitterness of the fraction containing the β-acids was also found to be enhanced after wort boiling. To gain first insights into the β-acid-derived bitter compounds, the β-acid colupulone was isolated, thermally treated under wort boiling conditions and, then, investigated for bitter tasting degradation products by means of a taste dilution analysis (TDA). Besides the cohulupone, five previously unreported bitter-tasting colupulone degradation products, all of which exhibited a lingering, β-acid-like bitter taste with low recognition thresholds between 37.9 and 90.3 μmol/l, were isolated and their structures determined as two tricyclocolupone epimers, two dehydrotricyclocolupone epimers, and nortricyclocolupone, respectively, by means of LC–TOF–MS and 1D/2D-NMR spectroscopy.     

灵芝菌固态发酵夏秋梅占红茶风味特征分析

目的 探究灵芝菌固态发酵下夏秋梅占红茶的风味特征。方法 采用高效液相色谱法(high performance liquid chromatography,HPLC)、电子舌(electronic tongue,E-tongue)与气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)相结合,利用多元统计分析,对夏秋梅占灵芝菌茶的滋味与香气品质特征进行判定。结果 与夏秋梅占红茶相比,梅占灵芝菌茶在滋味与香气特征上具有差异, HPLC检测结果显示儿茶素类、咖啡碱类苦涩味物质及部分氨基酸类物质含量显著下降,电子舌结果表明甜味响应值增加,苦味、鲜味响应值降低。其中梅占灵芝菌茶中脯氨酸、没食子酸、儿茶素没食子酸与苦味特性呈显著负相关,天冬氨酸、丙氨酸与涩味特性呈显著负相关,丙氨酸与鲜味特性呈极显著正相关,没食子儿茶素与鲜味特性呈显著正相关。挥发性成分上,建立正交偏最小二乘法-判别分析(orthogonal partial least squares-discriminant analysis, OPLS-DA)模型,选取模型中变量重要性投影(v...     

Odour active aroma compounds of sea fig (Microcosmus sulcatus)

Sea fig is an original shellfish appreciated for its powerful “marine, iodized” flavour. Different methods of analysis by gas chromatography, coupled with olfactometry (GC–O), were studied and compared. Subsequently, odour-active aroma compounds of sea fig extract were analyzed by OSME and CHARM analysis. Twenty-nine olfactive areas were observed by OSME, and 18 by CHARM analysis. Volatile compounds of the extract were analyzed by mass spectrometry and specific detectors associated with the GC. Twenty molecules, responsible for these odours were elucidated. Among them, 12 were directly identified by GC–MS, and the remaining 8 only by GC–O and standard sample injection. Moreover, 10 volatile sulfur-containing compounds were revealed as the major olfactive contributors. The two principal character-impact compounds possessed “marine, fresh” and “fishy, crustaceous” odours. The first could not be identified; however, trimethylamine was attributed to the other, and defined as a key compound of sea fig aroma.     

Screening of musty-earthy compounds from tainted cork using water-based soaks followed by headspace solid-phase microextraction and gas chromatography–mass spectrometry

Compounds responsible for musty-earthy off-flavours in cork, namely 2-methylisoborneol (MIB), geosmin (GSM), 2,4,6-trichloroanisole (TCA) and 2-methoxy-3-isopropylpyrazine (IPMP), were determined from tainted cork using water-based soaks followed by headspace solid-phase microextraction and gas chromatography–mass spectrometry (HS-SPME–GC–MS). The influence of the fibre coating used and of the extraction time and temperature were investigated for the joint analysis of MIB, GSM, TCA and IPMP. Considering the obtained results, an extraction time of 30 min at a temperature of 50 °C were fixed as experimental conditions, using a divinylbenzene/carboxen-polydimethylsiloxane/polydimethylsiloxane (DVB/CAR/PDMS) fibre. Quality parameters of the chromatographic method were obtained and good recoveries (117–128%) were found in spiked aqueous cork macerates. Using the same experimental conditions, the presence of guaiacol, 2,3,4,6-tetrachloroanisole (TeCA), pentachloroanisole (PCA), 2,4,6-tribromoanisole (TBA) and 2-methoxy-3,5-dimethylpyrazine (MDMP) could also be evaluated in a single chromatogram. From all the compounds analyzed in tainted samples, TCA and guaiacol were the only contaminants present and only TCA concentrations were found above its perception threshold in water.     

Volatile flavor constituents in roasted pork of Mini-pig

Volatiles from roasted pork of Mini-pig were first investigated by solid phase microextraction (SPME) as well as simultaneous distillation and solvent extraction (SDE) combined with gas chromatography and mass spectrometry (GC–MS). Total of 86 different compounds were identified with aldehydes being the most abundant followed by the spice components such as estragole, trans-anethole, eugenol and so on. Compared with other cooked meat products, much low amount of aliphatic alcohols were present in the roasted Mini-pig pork. The SDE isolation was preferred in the characterization of meat flavor considering that semi-quantitative data was conveniently obtained, more components were revealed, artifact formation was limited and aromatic profile was representative of the meat sample. By gas chromatography and olfactometry (GC–O), 45 olfactory regions were exposed and 43 flavors were located. Finally, 17 important flavor substances in the SDE extract were quantified by gas chromatography and flame ionization detector (GC–FID) using calibration curves of authentic chemicals.     

Sensory quality of turnip greens and turnip tops grown in northwestern Spain

In Galicia (northwestern Spain), Brassica rapa var. rapa L. includes turnip greens and turnip tops as vegetable products that are characterized by a particular sulfurous aroma, pungent flavor, and a bitter taste. In this work, 12 local varieties grown as turnip greens and turnip tops were evaluated to define the sensory attributes, to relate them with secondary metabolites, and to select those sensorial traits that better describe these crops. Results showed differences in the sensory profiles of B. rapa varieties. Turnip greens were significantly different regarding aroma intensity, leaf color, and salty taste, while turnip tops were for color and firmness of leaves, moistness and fibrosity in mouth, sharpness, and bitter taste. Secondary metabolites as glucosinolates in turnip greens and phenolic compounds in turnip tops were highly correlated with texture and flavor. Glucosinolates, especially progoitrin (in turnip greens) and gluconapin (in turnip tops), showed correlation with bitter taste and aftertaste persistence. Correlation between sensory traits showed highest values between leaf firmness and stalk firmness (R = 0.94**), leaf firmness and fibrosity (R = 0.92**), aftertaste persistence and bitterness (R = 0.91**), and between bitterness and moistness (R = −0.89**).     

Electronic nose and GC–MS analysis of volatile compounds in Tuber magnatum Pico: Evaluation of different storage conditions

The characteristic aromatic composition of white truffles (Tuber magnatum Pico) determines its culinary and commercial value. However modifications of truffle organoleptic proprieties occur during preservation. A study of headspace of white truffles by using Electronic nose (E-nose), gas chromatography–mass spectrometry (GC–MS) and sensory analyses was performed. Truffles were stored at different conditions for 7 days: +4 and +8 °C wrapped in blotting paper or covered by rice or none of the above. Headspace E-nose measurements and sensory analyses were performed each day. Statistical multivariate analysis of the data showed the capability of E-nose to predict sensorial analysis scores and to monitor aroma profile changes during storage. Truffle’s volatile molecules were also extracted by headspace solid phase microextraction technique and separated and identified by GC–MS. Partial Components Analysis of data was performed. E-nose and GC–MS results were in agreement and showed that truffle storage in paper at +8 °C seemed to be the best storage condition.