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.     

Impact of feeding and rearing systems of Iberian pigs on volatile profile and sensory characteristics of dry-cured loin

The effect of growing pigs on free-range (FR) or in confinement with three different diets [acorn (A), acorn and grass (A-G) and formulated diet (FD)] on composition, volatile profile and sensory characteristics of dry-cured loin was studied. The FR, A and A-G diets, in comparison with FD, induce a higher α- and γ-tocopherol concentration, which limits the TBARs values at 24 h of air exposure. Sixty volatile compounds were identified in the headspace, including 14 aldehydes, 10 hydrocarbons, eight alcohols, five ketones, four furans, four pyrazines, four sulphur compounds, three acids, three esters, three phenols, one pyridine and one pyrrole. Volatiles from amino acid catabolism stressed the difference among batches FR being the batch with the highest level of these compounds. Products from FD showed the lowest fat content and L^∗ value. FR loins obtained the highest scores for appearance, odour and flavour in the rank order test sensory analysis.     

Analysis of volatile compounds of Iberian dry-cured loins with different intramuscular fat contents using SPME-DED

In order to study the effect of both, ripening time and IMF content on the volatile profile of Iberian dry-cured loin, volatile compounds from the headspace of 10 Iberian dry-cured loins with different intramuscular fat contents (IMF), low (average IMF content of 2.3%) and high (average IMF content of 6.7%), at days 40 and 55 of the ripening process were analysed using SPME coupled to a direct extraction device (DED) and subsequent gas chromatography/mass spectrometry (GC/MS). Chromatographic areas of the main chemical families detected (hydrocarbons, aldehydes, alcohols, ketones and acids) increased with ripening time. A higher total chromatographic area was detected in the headspace of high IMF loins compared to low IMF ones. Several volatile compounds derived from lipid oxidative reactions, such as hexanol, octanal, (E,E)-2,4-heptadienal or (E)-2-decenal, and others from the degradation of certain amino acids, such as dimethylsulfide, 3-methylbutanal or phenylacetaldehyde, showed higher chromatographic areas in the headspace of high IMF loins than in low IMF ones. Thus, IMF content could influence both the generation of volatile compounds and the transfer of such compounds from the product matrix to the headspace.     

Analysis of volatile compounds in traditional smoke-cured bacon(CSCB) with different fiber coatings using SPME

The volatile compounds of Chinese traditional smoke-cured bacon (CSCB) were studied using SPMS-GC/MS. There were 48 volatile compounds identified and quantified, which belonged to several classes of chemical: 1 alkane, 16 aldehydes, 5 ketones, 9 alcohols, 4 thioethers and thiols, 3 furans and 10 phenols compounds. All the volatile compounds except for alkane was responsible for CSCB characteristic flavor. The major volatile compounds of CSCB came from smoking, oxidation and Maillard reaction, etc. Many volatile compounds were not reported in previous paper isolated by steam distillation method or nitrogen purge-and-steam distillation method on CSCB. It should be because of different method of isolating volatile substances from CSCB. Among the fibers tested, CAR/PDMS (carboxen/polydimethylsiloxane) fiber coating showed the highest area counts for most volatile compounds. CAR/PDMS coating extracted better those compounds whose linear retention indices (LRI) was lower than 926 (on average) and DVB/CAR/PDMS (divinylbenzene/carboxen/polydimethylsiloxane) those with higher LRI.     

油桃果实挥发性物质的固相微萃取条件优化研究

采用固相微萃取法(SPME)提取油桃果实挥发性成分,并用气相色谱仪(GC)对其进行分析。通过设计两组正交实验对影响SPME的参数条件进行了优化,得到了最佳萃取条件:采用100μmPDMS萃取头,添加氯化钠0.9g,在50℃萃取30min,转子转速为400r/min。在此条件下,油桃果实挥发性物质的萃取效率最好,检测效果最佳。     

Identification of volatile compounds in soymilk using solid-phase microextraction-gas chromatography

Headspace solid-phase microextraction (HS-SPME) gas chromatography was used to analyze volatile compounds in soymilk. The effect of incubation temperature (30–70 °C) and time (5–60 min), sample volume (0.5–5 ml), and type of SPME fiber (65 μm CWAX–DVB, 70 μm PDMS–DVB and 85 μm CAR–PDMS) were studied. All the factors markedly affected sensitivity and selectivity. Among the three fibers tested, the CAR–PDMS fiber had greater sensitivity to a more diverse range of volatile compounds, followed by PDMS–DVB and CWAX–DVB fibers using both soymilk and water with added volatiles as a matrix. SPME optimization conducted using a water matrix with added known soy volatiles, showed the following conditions to be optimal for selectivity and sensitivity: incubation temperature of 40 °C, incubation time of 20 min, and sample volume of 5 ml (for volatile compound concentration of ∼25 ppm). The selected conditions were used for the analysis of volatiles in six commercial soymilk samples. A total of 30 volatile compounds were identified. The results showed significant differences in the total volatiles of the soymilk products. The repeatability of measurements of total volatiles compounds of soymilk was ∼5.4% for four replicate analyses. Similar volatile compounds were present in all the samples analyzed but at different concentrations. The method proposed is simple and can be used to measure both hexanal and/or total volatiles in soymilk samples.     

Characterization of French and Spanish dry-cured hams: influence of the volatiles from the muscles and the subcutaneous fat quantified by SPME-GC

The influence of the volatile compounds on the characterization of Spanish and French dry-cured hams was studied. Thirty volatiles were quantified in each one of four locations (biceps femoris, semimembranosus and semitendinosus muscles and subcutaneous fat) of 29 dry-cured hams by solid-phase microextraction gas-chromatography (SPME-GC). The Brown–Forsythe univariate test allowed determination of the volatiles that individually could characterize (p < 0.05) the samples by their geographical origin (France, Spain) and breed type (Iberian, white). Stepwise linear discriminant procedure, under very strict conditions (F-to-Enter for a F-distribution > 0.95), then selected the most remarkable volatile compounds. Four compounds from the subcutaneous fat (methyl benzene and octanol) and the semitendinosus muscle (2-butanone and 2-octanone) allowed 100% correct classifications by geographic origin. On the other hand, only two compounds from the subcutaneous fat (octanol) and the biceps femoris muscle (3-methyl 1-butanol) correctly classified all the samples by the breed type. The ability of these variables to classify the samples was checked by the unsupervised procedure of principal components.     

A headspace solid-phase microextraction method development and its application in the determination of volatiles in honeys by gas chromatography

The first part of the paper presents the detailed optimisation of all steps of the determination procedure of volatiles from Polish honeys by headspace solid-phase microextraction (HS-SPME) as the sample preparation method and gas chromatography/mass spectrometry (GC–MS) as the method of final determination. In the result, the following conditions were applied: CAR/PDMS/DVB SPME fibre, the sample composition (5:1 w/w honey to water ratio), 3 g sample size. The other procedure parameters, like the temperatures of individual stages of the process, were also included.     

Evaluation and selection of yeasts isolated from dry-cured Iberian ham by their volatile compound production

One hundred and seventeen yeast strains isolated from dry-cured Iberian ham from the four different protected designations of origin of Spain were investigated for their volatile compound production. The yeast strains were grouped into the two main yeast species usually found in this product (Debaryomyces hansenii and Candida zeylanoides) and 10 different biotypes by restriction mitochondrial DNA analysis. Yeast strains were grown in a designed model culture medium under conditions representative of dry-cured ham processing. Volatile compounds were extracted from this medium using solid-phase micro-extraction and were analysed by gas chromatography/mass spectrometry. Marked differences in volatile compound production were found between D. hansenii and C. zeylanoides and between the mitochondrial DNA patterns of these species. Two of the mitochondrial DNA patterns of D. hansenii exhibited the highest production of the volatile compounds involved in the dry-cured flavour. Consequently, these patterns of D. hansenii should be proposed as starter cultures for dry-cured ham.     

A comparison of solid-phase microextraction (SPME) with simultaneous distillation-extraction (SDE) for the analysis of volatile compounds in heated beef and sheep fats

A comparison has been made on the application of SPME and SDE for the extraction of volatile compounds from heated beef and sheep fats with separation and measurement by gas chromatography-mass spectrometry. As far as we know, this report represents the first time that such a comparison has been made for the measurement of volatile compounds in heated sheep fat. Approximately 100 compounds (in relatively high abundance) were characterised in the volatile profiles of heated beef and sheep fats using both techniques. Differences were observed in the volatile profiles obtained from each technique, independent of compound class. Rather than rate one technique as superior to another, the techniques can be regarded as complementary to each other.     

Effect of pork fat addition on the volatile compounds of foal dry-cured sausage

The effect of fat content on volatile compounds from foal dry-cured sausage was studied. Three batches (10 units per batch) of dry fermented sausages with different pork back fat content (5%, 10% and 20%) were manufactured; low fat (LF), medium fat (MF) and high fat (HF), respectively. A total of 45 volatile compounds were extracted by purge-and-trap and identified by GC-MS in the headspace of the batches. The mixture comprised 11 terpenes, 15 esters, 14 hydrocarbons and 2 alcohols. Spices were responsible for the generation of 14 volatile compounds comprising terpenes and hydrocarbons. After 49 days of ripening volatile compounds from spices represented 52.9, 38.9 and 31.2% of the total area for samples from LF, MF and HF batches, respectively, while lipid autooxidation was responsible for the generation of 8 volatile compounds. The PCA offered a good separation of the mean samples according to their fat content.     

Application of solid-phase microextraction to the analysis of volatile compounds in virgin olive oils from five new cultivars

Evaluation and identification of wild olive genetic resources allowed us to select new olive varieties and to recognize Tunisian grove richness and diversity. Five new olive cultivars were previously selected among populations of wild olive plants on the basis of agronomic and chemical evaluations. Their virgin olive oils were analysed for their fatty acid composition, quality indices (Free acidity, PV and UV characteristics) and oxidative stability. They were then submitted to solid phase microextraction (SPME) and their volatile compositions were determined.     

Differentiation of yeasts growing on dry-cured Iberian ham by mitochondrial DNA restriction analysis, RAPD-PCR and their volatile compounds production

The efficiency of mitochondrial DNA (mtDNA) restriction analysis, RAPD-PCR and volatile compounds analysis to differentiate yeast biotypes involved in flavour development of dry-cured Iberian ham throughout the ripening process is evaluated. For this purpose, 86 yeasts isolated from Iberian hams in the main ripening stages at different industries of the four Protected Designations of Origin of this product, were used. The combination of mtDNA restriction analysis and RAPD-PCR using the primer (GACA)₄ showed a higher variability in the yeast species detected than obtained using only mtDNA restriction analysis. Only two species, Debaryomyces hansenii and Candida zeylanoides, were identified throughout the whole ripening process and a wide diversity of biotypes was found in these two species, with those of D. hansenii predominating. Clear differences between biotypes were detected in the generation of volatile compounds, with the biotype C2-2 of D. hansenii showing the highest concentrations of volatiles. The combined use of mtDNA restriction analysis and RAPD-PCR distinguishes yeast biotypes with different production of volatile compounds. In addition, analysis of the production profile of volatile compounds is needed to differentiate yeast strains of the same biotype recovered at different stages of ripening. Thus, the combination of these three methods could be very useful to select or monitor yeasts as starter cultures in dry-cured meat products.     

Generation of volatile flavour compounds as affected by the chemical composition of different dry-cured ham sections

The composition of different dry-cured ham sections has been determined in order to study their contribution to flavour generation. The proteins, free amino acids, free fatty acids and volatile compounds were analysed in different sections of dry-cured hams with 7 and 12 months of processing. The main differences among sections were detected in free amino acids and volatile compounds. To sum up, there was a higher concentration of free amino acids in the centre section than in the butt and shank sections. However, after 12 m of ripening the difference among sections was lower and only the butt was the one with the lowest concentration. Similar results were obtained in the content of volatile compounds, the centre part of the hams contained a higher proportion of volatile compounds after 7 m of ripening than the shank and butt sections. Nevertheless, in 12 months dry-cured hams there are changes in the proportions of volatile compounds being the centre section the one with the highest proportion of volatile compounds due not only to the higher concentration of free amino acids but also to the oxidation of unsaturated fatty acids.     

Determination of volatile compounds and quality parameters of traditional Istrian dry-cured ham

The aim of this work was to determine the characteristics of Istrian dry-cured ham by instrumental methods and sensory analysis. The aroma-active compounds of Istrian dry-cured ham from 2010 and 2012 were investigated by using headspace-solid phase microextraction (SPME) and gas chromatography–mass spectrometry (GC–MS). Samples of biceps femoris were also evaluated by measuring physical and chemical characteristics. 92 volatile aroma compounds of Istrian dry-cured ham were found. Volatile compounds belonged to several chemical groups: aldehydes (51.4; 51.3%), terpenes (16.5; 16.4%), alcohols (15.5; 13.2%), ketones (8.6; 7.4%), alkanes (3.8; 5.7%), esters (1.3; 1.6%), aromatic hydrocarbons (0.8; 3.9%) and acids (0.6; 0.9%). Principal component analysis (PCA) showed that fat content, tenderness and melting texture were positively correlated. Terpenes were strongly correlated with flavour of added spices. Sweet taste and the presence of esters were positively correlated as well as negative odour, raw meat flavour and water content.     

Solid-phase microextraction for headspace analysis of key volatile compounds in orange beverage emulsion

Headspace solid-phase microextraction (HS-SPME) gas chromatography was used to analyze target flavor compounds in orange beverage emulsion. The effects of SPME fiber (PDMS 100 μm, CAR/PDMS 75 μm, PDMS/DVB 65 μm and DVB/CAR/PDMS 50/30 μm), adsorption temperature (25–45 °C), adsorption time (5–25 min), sample concentration (1–100%), sample amount (5–12.5 g), pH (2.5–9.5), salt type (K₂CO₃, Na₂CO₃, NaCl and Na₂SO₄), salt amounts (0–30%) and stirring mode were studied to develop HS-SPME condition for obtaining the highest extraction efficiency and aroma recovery. For the head space volatile extraction, the optimum conditions were: CAR/PDMS fiber, adsorption at 45 °C for 15 min, 5 g of diluted beverage emulsion (1:100), 15% (w/w) of NaCl with stirring and original pH 4. The main volatile flavor compounds were: limonene, 94.9%; myrcene, 1.2%; ethyl butyrate, 1.1%; γ-terpinene, 0.41%; linalool, 0.36%; 3-carene, 0.16%; decanal, 0.12%; ethyl acetate, 0.1%; 1-octanol, 0.06%; geranial, 0.05%; β-pinene, 0.04%; octanal, 0.03%; α-pinene, 0.03%; and neral, 0.03%. The linearity was very good in the considered concentration ranges (R² ? 0.97). Average recoveries ranged from 88.3% to 121.7% and showed good accuracy for the proposed analytical method. Average relative standard deviation (RSD) for five replicate analyses was found to be less than 14%. The limit of detection (LOD) ranged from 0.06 to 2.27 mg/l for all volatile flavor compounds and confirmed the feasibility of the HS-SPME technique for headspace analysis of orange beverage emulsion. The method was successfully applied for headspace analysis of five commercial orange beverage emulsions.     

固相微萃取条件优化及发酵菜粕风味物质分析

研究固相微萃取与气质联用研究发酵菜粕的风味物质及比较不同品种菜粕发酵前后风味物质的变化,以峰面积及峰数为指标,通过萃取头、萃取温度、吸附时间和样品量的优化,确定了固相微萃取和气质联用研究发酵菜粕风味固相微萃取的条件,并比较了3种代表性菜粕发酵前后风味物质及硫苷组分和含量的变化。结果表明,固相微萃取最佳条件是:50/30μm DVB/CAR/PDMS(DCP)萃取头,温度70℃,吸附30 min,样品量2 g,其中萃取头和吸附温度显著影响萃取效率。发酵前后菜粕的挥发性组分及含量变化都较大,发酵后风味物质的总量都显著增加,硫苷的含量明显降低,表明发酵不但显著增加了风味物质的含量改变了风味,而显著降低了抗营养物质硫苷的含量。     

固相微萃取技术分析番茄香气成分的方法建立

除了酸甜苦咸四种基本味觉外,消费者选择食品时,食品所释放出来的香气也是一个考虑因素。通过固相微萃取结合气相色谱技术,可以很好地分离和鉴定番茄中的香气成分,最佳测定条件是:固相微萃取萃取头选用CW/DVB,吸附时间是25min,吸附温度为40℃,解析时间为4min,采样瓶中样品量为6g;气谱条件是:不分流进样,色谱柱为极性柱,采用程序升温进行分离鉴定。     

Analysis of volatile compounds of eucalyptus honey by solid phase extraction followed by gas chromatography coupled to mass spectrometry

Solid-phase extraction (SPE) followed by gas chromatography coupled to mass spectrometry has been used for the analysis of volatile compounds of eucalyptus honey. Different amounts of honey and dichloromethane were employed to optimize solid-phase extraction conditions. The best result was obtained with 20 g of honey eluted with 60 mL of dichloromethane. This method presented a good precision for volatile compounds usually found in honeys and allowed the quantification of 35 volatile compounds (terpenes and derivatives, furan and pyran compounds, ketones, benzene compounds, acids, and norisoprenoids) of eucalyptus honey.     

Differentiation of “Claret”, Rosé, Red and Blend wines based on the content of volatile compounds by headspace solid-phase microextraction and gas chromatography

We studied 46 samples of wine from Denomination of Origin of La Rioja: 8 rosé, 8 “claret”, 10 red, 10 artificial blend and 10 ungrouped wines (3 rosé, 2 “claret”, 2 red and 3 blend). The samples were analysed by gas chromatography using headspace-solid-phase microextraction (HS-SPME) with a Carbowax-divinylbenzene (CW/DVB) fibre. The variables considered were 3-methyl butyl acetate, 3-methyl-1-butanol, ethyl hexanoate, 1-hexanol, ethyl octanoate, diethyl succinate, hexanoic acid, 2-phenylethanol, octanoic acid, decanoic acid and geraniol, all significant for distinguishing the types of wines except 3 metil-1-butanol and 1-hexanol. The different wine samples were classified by multivariate statistical methods. Good differentiation between the different groups of samples was achieved by means of principal component analysis and hierarchical cluster analysis. Linear discriminant analysis was used to differentiate and classify these wines. 3-methyl-butyl acetate, ethyl octanoate, diethyl succinate, hexanoic acid, 2-phenylethanol and decanoic acid were the most discriminant variables and gave 100% recognition ability and 100% prediction ability.