Optimization of equilibrium headspace analysis of volatile flavor compounds of malaysian soursop (Annona muricata): Comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS)

Headspace solid-phase microextraction (HS-SPME) coupled to comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS) was applied for equilibrium headspace analysis of Malaysian soursop (Annona muricata) volatile flavor compounds. A two-level fractional factorial design (2^5-1) was used to determine the effect of SPME variables, namely, SPME fibers, adsorption temperature, extraction time, amount of salt, sample amount and sample concentration on the extraction efficiency of volatile flavor compounds. A total of 37 volatile compounds were identified, comprising 21 esters, 6 alcohols, 3 terpenes, 2 acids, 2 ketones, 2 aldehydes and an aromatic with different hydrophobicities (log P) ranging between −0.14 and 4.83. Extraction using 10 g of diluted (5% w/w) blended soursop pulp with CAR/PDMS fiber at 25 °C for 30 min and 30% (w/w) of NaCl under stirring mode resulted in the highest extraction efficiency of volatile flavor compounds. The principal component analysis score discriminated the influence of SPME variables on the equilibrium headspace concentration of target volatile compounds.     

Establishment of Monstera deliciosa fruit volatile metabolomic profile at different ripening stages using solid-phase microextraction combined with gas chromatography–mass spectrometry

The volatile metabolomic profile of Monstera deliciosa fruits (M. deliciosa, ceriman) at three ripening stages, ripe, half-ripe and unripe, was established using headspace solid-phase microextraction (HS-SPME) combined with gas chromatography–quadrupole mass spectrometry detection (GC–qMS). To obtain the optimal HS-SPME conditions, the main experimental parameters that influence the extraction efficiency and experimental response were analyzed. The highest extraction efficiency was achieved with 1 g of ceriman sample, using a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber for 60 min at 40 °C with 15% NaCl (w/w). After optimization, all ceriman samples were analyzed with the best extraction conditions that allowed to identify 80 volatile metabolites (VOMs), belonging to different chemical groups namely ethyl esters (88.61–77.94%), terpenoids (18.08–9.83%), carbonyl compounds (3.41–1.05%), higher alcohols (1.41–0.51%) and lactones (0.14–0.03%). Thirty-eight of the identified volatile metabolites (47.50%) have not been reported in M. deliciosa, so far, providing a more complete characterization of its volatile composition. The predominant VOMs identified in M. deliciosa fruits were ethyl butanoate, linalool, ethyl hexanoate, ethyl 2-methyl butanoate, butanoic acid, ethyl benzoate and propyl butanoate. Remarkable differences were found in both the quantitative and qualitative composition of M. deliciosa fruits at different ripening stages.Principal component analysis (PCA) provided a suitable tool to differentiate the volatile profile of target fruits among three ripening stages.     

Improving fruity aroma production by fungi in SSF using citric pulp

Aromas produced by microorganisms can be recognized as natural and therefore have great economic potential. Ceratocystis fimbriata has the potential to produce a variety of aromas. The aim of the present work is to increase the fruity aroma production in citric pulp (CP), a waste from the citric juice production industry, using C. fimbriata in solid-state fermentation (SSF), testing other residues as carbon (sugarcane molasses, soya molasses) and nitrogen (soya bran or urea) sources. The studies were carried out in 250 mL Erlenmeyer flasks, pH 6.0, 75% initial moisture, 30 °C, inoculum rate 1 × 10⁷ spores/g of CP, during 120 h. Total volatile compounds were quantified by headspace analysis in a gas chromatograph. The best production of volatile compounds was detected when the citric pulp was supplemented with 50% of soya bran, 25% of sugarcane molasses, and mineral saline solution. The production of total volatile reached 99.60 μmol/L g.     

Generation of volatile compounds in Brazilian low-sodium dry fermented sausages containing blends of NaC1, KC1, and CaC12 during processing and storage

Brazilian dry fermented sausages with different salt contents were manufactured: control (2.5% NaCl), 50% salt reduced (1.25% NaCl, F1), 50% replaced by KCl (1.25% NaCl and 1.25% KCl, F2), 50% replaced by CaCl₂ (1.25% NaCl and 1.25% CaCl₂, F3), and 50% replaced by KCl and CaCl₂ (1.25% NaCl, 0.625% KCl and 0.625% CaCl₂, F4). Changes in the composition of volatile compounds were studied during processing (0, 7, and 19 days) and storage (30, 60, and 90 days). Neither reduction nor replacement of NaCl by KCI affected the volatile compounds produced during the manufacturing process, and both increased the volatile compounds from carbohydrate fermentation and amino acid degradation during storage. The addition of CaCl₂ improved the generation of hexanal and (E)-hept-2-enal and other volatiles from lipid oxidation during processing and storage. After 90 days of storage, the control sample showed an increase in the generation of volatile compounds from lipid oxidation.     

Development of potentially synbiotic fresh-cut apple slices

The aim of this study was, to develop potentially synbiotic fresh-cut apple wedges by applying probiotic bacteria (Lactobacillus rhamnosus GG) and prebiotics in the form of oligofructose and inulin. An assessment of the quality, sensory, polyphenol and volatile attributes of synbiotic and probiotic samples was also undertaken. Fructan analysis showed that all prebiotics remained stable over the 14 days storage period and an intake of 100 g of apple supplies 2–3 g of prebiotics. All samples sets contained ca. 10⁸ cfu/g over the test period, which is sufficient for a probiotic effect, and is comparable to counts of probiotic bacteria in commercially available dairy products. Browning index, firmness, acidity and dry matter remained stable throughout the 14 days compared to the control while applying prebiotic coatings resulted in an increase in soluble solids. Sensory assessment indicated acceptable quality of probiotic and synbiotic apple wedges. HPLC analysis showed levels of decrease in polyphenolic compounds. No difference was found between O₂ and CO₂ headspace concentration and volatile production of synbiotic samples and samples only treated with probiotics.     

Study of chemical changes in pasteurised orange juice during shelf-life: A fingerprinting-kinetics evaluation of the volatile fraction

The current work used fingerprinting-kinetics for the first time to monitor shelf-life changes in a low-pH, pasteurised, shelf-stable product, more particular in orange juice. Orange juice samples were stored as a function of time at four different storage temperatures (20, 28, 35 and 42 °C). To obtain insight into chemical changes in the volatile food fraction, samples were fingerprinted with headspace GC–MS. The objectives of this work were twofold: (i) to identify major chemical changes of pasteurised orange juice during shelf-life and (ii) to study the kinetics of selected shelf-life compounds in the context of accelerated shelf-life testing (ASLT). At 20 °C, changes in terpenes and a decrease in aldehydes were observed. Oxides and sulphur compounds increased and esters decreased at increased storage temperatures (at 28 °C and above). Concerning ASLT, four volatile compounds had clear temperature and time dependent kinetics within the investigated temperature range.     

Effect of temperature on growth and metabolism of probiotic bacteria in milk

The growth and metabolism of six probiotic strains with documented health effects were studied in ultra-high temperature (UHT) treated milk supplemented with 0.5% (w/v) tryptone or 0.75% (w/v) fructose at different temperatures. The probiotic strains were Lactobacillus acidophilus La5, Lb. acidophilus 1748, Lb. johnsonii LA1, Lb. rhamnosus GG, Lb. reuteri SD 2112 and Bifidobacterium animalis BB12. Fermentation was followed for 48 h at 20, 30, 37 and 45 °C and the samples were analysed for pH, log cfu mL⁻¹, volatile compounds, organic acids and carbon dioxide. All six probiotic strains showed very different profiles of metabolites during fermentation, however, the two Lb. acidophilus strains were the most alike. All strains, except Lb. reuteri SD 2112, showed viable cell numbers above 6.5 log cfu mL⁻¹ after 48 h fermentation at 30, 37 and 45 °C. The probiotic strains produced different amounts of metabolic products according to temperature and fermentation time illustrating the importance of controlling these parameters.     

Phenolic and aroma compositions of pitomba fruit (Talisia esculenta Radlk.) assessed by LC–MS/MS and HS-SPME/GC–MS

Pitomba (Talisia esculenta Radlk.) is a Brazilian exotic fruit consumed specially in the Amazonian region. Because of its large consumption and also due to the lack of knowledge regarding its chemical composition, pitomba fruit was studied in relation to its phenolic and aroma constitution. Using liquid chromatography tandem mass spectrometry (LC–MS/MS), 13 phenolic compounds (catechins, flavonoids and organic acids) were tentatively identified by comparison with standards and by fragmentation patterns. A validated method was applied to quantify common phenolic compounds of the pitomba pulp, for which quinic acid was the main compound (507.8 ± 7.4 μg g^− 1 DWP). Gas chromatography mass spectrometry (GC–MS) was employed along with headspace solid-phase microextraction (HS-SPME) to assess the aroma composition of pitomba fruit. A total of 27 volatile organic compounds (VOCs) were tentatively identified for pitomba fruit, for which 2-phenethyl acetate (17.89%) and isopentyl acetate (13.43%) esters were the main VOCs, contributing to the characteristic aroma of pitomba. The antioxidant capacity of the extract of pitomba fruit was evaluated by ABTS, DPPH and ORAC assays. We observed that pitomba has a moderate antioxidant activity.     

Method for the static headspace analysis of carrot volatiles

A static headspace analysis/gas chromatography/mass spectrometry (SHA/GC/MS) method was developed to analyse the volatile composition of raw (seven different varieties), stored and cooked carrot samples. A total of 35 different volatile compounds were identified in carrots. Of these, trans-ocimene, 2,5-dimethyl styrene, camphor, borneol, α-santalene, α-selinene, γ-elemene and α-zingiberene in raw carrots and propanol in stored carrots were identified for the first time. Major volatile compounds identified in raw carrots were α-pinene, sabinene, myrcene, limonene, γ-terpinene, terpinolene, β-caryophyllene and γ-bisabolene. Mono-and sesquiterpenes accounted for about 97% of the total volatiles identified. Sizeable varietal differences (p<0.01) were observed. Carrot volatiles did not change appreciably during the 28 day storage period at 5, 25 and 35°C, except propanol that showed exponential increases at higher temperatures. No propanol was detected in fresh raw carrots. Cooking resulted in 88.6, 93.0 and 95.5% loss in total volatiles after cooking times of 10, 20 and 30 min, respectively.     

Effects of pre-rigor injection of sodium citrate or acetate,or post-rigor injection of phosphate plus salt on post-mortem glycolysis,pH, and pork quality attributes

Forty pork carcass sides were assigned to one of four treatments: pre-rigor citrate (CIT) or acetate injection (ACE); post-rigor phosphate and salt injection (PHOS); and non-injected control (CON). Loins in 20 sides were injected at 50 min post-mortem with 4% solutions of CIT or ACE to approximately 110% of projected loin weights, and 10 loins were injected at 24 h post-mortem to 106.6% with a solution of 4.4% PHOS and 2.2% salt. Although CIT increased pH (P < 0.05), neither CIT nor ACE altered (P > 0.05) glycolytic metabolite concentrations. The pH increase in muscles from the CIT treatment was most likely due to its buffering ability rather than to its glycolytic inhibition. Pre-rigor CIT injection improved tenderness without the detrimental effects on color or flavor found with PHOS, but neither CIT nor ACE altered glycolytic metabolites or improved firmness, wetness, or fresh visual color over CON. Poor flavor attributes of the ACE treatment will hinder its use as an ingredient for pork enhancement solutions.     

Temperature shows greater impact on bovine Longissimus dorsi muscle glycogen debranching enzyme activity than does salt concentration

The degradation of glycogen progresses by the co-operation of two enzymes: glycogen phosphorylase (phosphorylase) and glycogen debranching enzyme (GDE). We studied the effect of temperature (4–42 °C) and salt concentration (0–3% NaCl) on bovine M. longissimus dorsi GDE activity. GDE activity (n = 4) decreased significantly with decreasing temperature from about 40–4 °C. GDE exhibited 52% activity at 25 °C and 11% at 4 °C compared to its optimum activity measured at 39 °C. In rapidly chilled meat, the reduction in GDE activity may substantially delay the rate of glycolysis. However, residual GDE activity at 4 °C seems sufficient to enable the attainment of normal ultimate pH if the available time is long enough. An increase in salt concentration from 0% to 2% and to 3% induced a significant (P < 0.001) increase in the ultimate pH of ground bovine meat (n = 6), but showed no effect on GDE activity.     

Volatile compounds in Spanish dry-fermented sausage ‘salchichón’ subjected to high pressure processing. Effect of the packaging material

The effect of high pressure treatment (400 MPa, 10 min at 12 °C) on the volatile profile of Spanish dry-fermented sausage ‘salchichón’, packaged with or without aluminium foil in a multilayer polymeric bag, was investigated. The analysis of the volatile fraction was carried out by dynamic headspace extraction coupled to gas chromatography–mass spectrometry. Pressure-treated samples showed significantly higher levels of alcohols, aldehydes and alkanes and lower levels of two methylketones as compared with control samples. An intense migration was observed of compounds from the plastic material into the product, mainly linear and branched-chain alkanes, alkenes and benzene compounds. Most of these migrating compounds were significantly more abundant in pressurized samples than in untreated samples.     

Mitigation of acrylamide and hydroxymethyl furfural in instant coffee by yeast fermentation

Acrylamide being known as carcinogenic and hydroxymethyl furfural (HMF) being known as cytotoxic compounds are heat induced process contaminants found in instant coffee. Today's instant coffee production method involves roasting of coffee beans, grinding, flavor and aroma separation, extraction, concentration, and drying steps. During roasting, acrylamide and HMF are formed in varying amounts depending upon the degree of heat treatment as a result of the Maillard reaction. This study was conducted in order to reduce the concentrations of acrylamide and HMF in instant coffee. Instant coffee (20%, w/v) was mixed with sucrose (0–10, w/v) and baker's yeast (Saccharomyces cerevisiae, 1–2%, w/v) in a tightly closed glass vessel. The mixture was fermented at 30 °C for 48 h. The kinetics of acrylamide and HMF degradation was investigated. HMF and acrylamide contents were reduced exponentially at varying rates, depending upon fermentation medium and time. After 24 h, HMF concentration was decreased by 61.2%, 75.7%, 93.6% and 99.2% in the fermentation media containing none, 1%, 5%, and 10% of sucrose, respectively. After 48 h, acrylamide concentration was decreased by about 70%. These results revealed that yeast fermentation is promising for the mitigation of HMF and acrylamide in instant coffee.     

Mathematical modeling of mass transfer in osmotic dehydration of onion slices

The study on osmotic dehydration of onion slices was carried out in order to remove the moisture prior to the further mechanical drying. Three salt concentration levels (5%, 12.5% and 20%), three temperature levels of osmotic solution (28 °C, 43 °C and 58 °C) and the observations on weight loss and solid gain were taken at an interval of 5 min up to first half an hour followed by interval of 10 min for next 1 h. The sample to solution ratio of 1:5, agitation of 100 shakes per minute, sample thickness of 4 mm and 0.2% potassium metabisulphite mixed with osmotic solution were used for the study. A two-parameter mathematical model developed by Azuara et al. was used for describing the mass transfer in osmotic dehydration of onions slices. The effect of time on mass transfer kinetics was investigated and the constants of two-parameter model and final equilibrium points for moisture loss as well as solid gain were found. The effect of solution concentration and solution temperature was also studied and it was found that equilibrium moisture loss and solid gain are related to solution concentration and solution temperature logarithmically. The optimum conditions of osmotic dehydration for further drying were found to be 20% salt concentration, 28 °C solution temperature and 1-h of osmosis.     

Dynamics of the loss and emergence of volatile compounds during the concentration of cashew apple juice (Anacardium occidentale L.) and the impact on juice sensory quality

Concentrating cashew apple juice alters the beverage aroma and flavor, compromising consumer acceptability of the concentrated beverage. To understand the mechanisms involved in these changes, this research characterized the dynamics of the loss and emergence of volatile compounds during cashew apple juice concentration, reporting their impact on beverage sensory quality. Fresh cashew apple juice (10.3°Brix) was concentrated in a thermal-siphon type evaporator operating in a closed system. Five samples were taken throughout the concentration process with the following soluble solids contents: 11.8°Brix, 14.9°Brix, 20.2°Brix, 29.6°Brix and 42.1°Brix. Trained judges rated the aroma note intensities, described as “fresh cashew apple” and “cooked” as perceived in the fresh and concentrated beverages. The headspace volatiles of the six samples were identified and quantified by GC–MS. The results indicated the esters as the major component in the fresh juice (226.46 μg kg^− 1) representing 45.0% of the total mass of volatiles, followed by the terpenes (118.98 μg kg^− 1), acids (45.23 μg kg^− 1), aldehydes (39.10 μg kg^− 1), alcohols (18.91 μg kg^− 1), lactones (19.15 μg kg^− 1), hydrocarbons (18.02 μg kg^− 1) and ketones (11.05 μg kg^− 1). Predictive statistical models (R² > 0.956, p ≤ 0.002) revealed that on reaching 14.9°Brix, the ester concentration declined more than 90%, the terpene content almost 100%, alcohols 85%, aldehydes 80% and hydrocarbons 90%. At 14.9°Brix, the intensity of “fresh cashew apple” aroma still predominated in the juice, but the panelists detected the presence of a weak “cooked” aroma. Concentration of the beverage to 20.2°Brix or above expressively increased the cooked aroma intensity and the concentration of hydrocarbons, alcohols and some aldehydes usually associated with off-flavors such as pentanal and decanal. This raises the possibility that some of these compounds might have been formed during juice processing. Juice with better sensory quality could possibly be obtained by concentrating the beverage to levels below 20.2°Brix, recovering the esters that evaporated off the juice until ~ 15°Brix is reached, and re-adding them to the juice concentrated.     

Effects of a black rice extract (Oryza sativa L. indica) on cholesterol levels and plasma lipid parameters in Wistar Kyoto rats

This study was designed to evaluate the efficacy of an anthocyanin pigmented rice (e.g. black rice) to mitigate the onset of hypercholesterolemia in rats-fed atherogenic diets. Male Wistar (n = 10/group) rats were fed with atherogenic diets containing 0.5% cholesterol in the presence and in the absence of bile salt (e.g. 0.05% cholic acid) along with a standardized black rice extract (BRE) (e.g. 3%, w/w). All animals were individually housed in stainless steel cages and fed with the experimental diets during a 12-h period for 10 weeks. Body weights of rats were measured every week of the experiment. After 10 weeks fed on experimental diets, rats were sacrificed and plasma total cholesterol, HDL and LDL cholesterol and triacylglycerols were measured immediately. The total cholesterol (TC) content in the liver, heart and aorta, and the concentration of triacylglycerol (TAG) were measured after lipid extraction using Folch method. Rats fed with 0.5% cholesterol containing diets which also included bile salt exhibited a considerably more severe hypercholesterolemia than counterparts fed diets containing only 0.5% cholesterol. The inclusion of the BRE in diets significantly (p < 0.05) decreased the level of TC, LDL–TC and TAG in plasma of rats-fed control diets that either contained or were absent in bile salt (p < 0.05). There were no differences in HDL-level. Liver crude lipids and total cholesterol levels were also significantly (p < 0.05) decreased in experimental groups relative to the control group in both experiments. Thus, supplementation of atherogenic experimental diets with BRE effectively decreased lipid levels in hypercholesterolemic rats. In lieu of the mixture of bioactive components present in BRE, it is possible that more than one mechanism underlying this reduction in lipids is involved.     

Evaluation of pre-rigor injection of beef with proteases on cooked meat volatile profile after 1 day and 21 days post-mortem storage

This research was carried out to determine the effects of pre-rigor injection of beef semimembranosus muscle with nine proteases from plant and microbial sources, on the volatile profile of cooked beef after 1 day and 21 days post-mortem (PM) storage using Solid-phase microextraction gas chromatography mass spectrometry analysis. A total of 23 aldehydes, 5 ketones, 3 furans, 8 nitrogen and sulphur compounds, 4 alkanes, 7 alcohols and 6 terpenes were detected. Eleven volatile compounds characteristic of ginger flavour were detected in zingibain-treated meat. Benzaldehyde significantly increased (p < 0.05) only in kiwifruit juice (KJ), fungal 31 protease and Asparagus protease (ASP) treated samples from 1 day to 21 days PM storage. A significant increase (p < 0.05) in 3-methylbutanal was observed in KJ, bacterial and fungal protease treated samples at 21 days PM storage. Treatments with bromelain, papain, ASP, actinidin, and KJ (except KJ 21 days) proteases resulted in flavour profiles closer to that of the control beef sample.     

Temperature-dependent kinetics of grape seed phenolic compounds extraction: Experiment and model

The kinetics of a batch solid–liquid extraction of total phenolic compounds (PC) from milled grape seed (Vitis vinifera L. cv. “Frankovka”) using 50% ethanol at different extraction temperatures (25–80 °C) was studied. The maximum yield of PC was 0.13 kg_GAE/kg_db after 200 min of extraction in agitated vessel at 80 °C. A new model based on the assumptions of a first order kinetics mechanism for the solid–liquid extraction and a linear equilibrium at the solid–liquid interface was developed. The model involves the concept of broken and intact cells in order to describe two successive extraction periods: a very fast surface washing process followed by slow diffusion of phenolic compounds from grape seeds to the solvent.The proposed model is suited to fit experimental data and to simulate the extraction of phenolic compounds, which was confirmed by the correlation coefficient (r ? 0.965), the root mean square error (RMSE ? 0.003 kg_GAE/kg_db) and the mean relative deviation modulus (E ? 2.149%). The temperature influenced both equilibrium partition coefficients of phenolic compounds and transport properties, which is manifested by a relatively high value of activation energy (23–24) kJ/mol and by values of effective diffusivity in seed particles.     

Effects of ethanol,tannin and fructose on the headspace concentration and potential sensory significance of odorants in a model wine

The effects of ethanol (8, 10, 12, 14, and 16% v/v), tannin (500, 1000, and 1500 mg/L) and fructose (200 and 2000 mg/L) concentrations on the headspace of eight selected odorants were investigated using headspace solid phase microextraction (HS-SPME) and gas chromatography–mass spectrometry (GC–MS). Analysis of variance results (ANOVA) showed significant interaction effects for the majority of odorants (P < 0.05). In general, higher tannin concentration enhanced the release of odorants while fructose induced a retention effect, both of which were largely dependent upon ethanol concentration. The net magnitude effect was a substantial reduction in the headspace concentration of odorants with the dominant contribution from ethanol concentration. The percent reduction in extracted odorant was more pronounced on larger molecular weight compounds. Further multivariate analysis discriminated model wines with different ethanol concentrations and, to a lesser extent, separated model wines with different fructose and tannin concentrations. Subsequent gas chromatography–olfactometry (GC–O) analysis revealed differences in the estimated odor thresholds of odorants in the model wines. Threshold values increased between 2 and 10,000-fold for 2-methoxyphenol and eugenol, respectively, at higher ethanol, tannin and fructose concentrations. Consequently, odor unit values (OUV) of odorants decreased indicating a reduction in the potential contribution of the odorants to the aroma of model wine. These results highlighted the significant impact that wine matrix interactions can have on wine aroma quality.