A solvent-free squeezing method for extraction of collected mass from aerosols of electronic cigarettes and heated tobacco products.

Previous in vitro toxicological assessments have demonstrated that almost no mutagenic and genotoxic activities in electronic cigarette (e-cigarette) and heated tobacco product (HTP) aerosols were detected even at the maximum recommended concentration. To accurately compare the toxicity levels between cigarette smoke and e-cigarette or HTP aerosols, higher exposure concentrations increasing the possibility to detect toxicity in in vitro tests are necessary, while avoiding solvent-induced toxicity. This study aimed to develop a solvent-free extraction method to obtain concentrated aerosol extracts for improved toxicological evaluation. Our novel approach involved squeezing several Cambridge filter pads, which collected aerosol constituents, in closed containers to achieve solvent-free extraction with comparable efficiency to the conventional method using organic solvents. The optimized squeezing method yielded extracts with concentrations approximately 10 times higher than those obtained in conventional extraction methods. Yield comparison of various constituents, such as flavoring compounds, in e-cigarette aerosol extracts revealed similar extraction efficiencies between the squeezing and conventional methods. However, the extraction efficiency for constituents with high log Pow values, predominantly found in HTP aerosol extracts, was unacceptably low using the squeezing method. In addition, solvent-free centrifuging, another type of extraction method, exhibited unsatisfactory results for even e-cigarette aerosols compared with the conventional method. Our findings suggest that the solvent-free squeezing method is suitable for extracting aerosol collected mass from e-cigarette aerosol but not from HTP aerosol. We anticipate that the solvent-free squeezing method will contribute to a deeper understanding of toxicological differences between e-cigarettes and conventional combustible cigarettes.

Heat treatment improves the sensory properties of the ultrafiltration by-product of honeybush (Cyclopia genistoides) extract.

BACKGROUND: Ultrafiltration of green honeybush (Cyclopia genistoides) extract results in a by-product (retentate). Application of further separation processes for recovery of polyphenols would entail creation of additional waste. Repurposing the retentate as a food flavour ingredient provides an alternative valorization approach. RESULTS: The retentate, suspended in water (270 g L-1 ), was heat-treated at 80 °C for 2, 4, 8 and 16 h, and at 90 °C for 2, 4, 6 and 8 h to change its sensory profile. The heat-treated retentate, diluted to beverage strength (2.15 g L-1 ), had prominent 'grape/Muscat-like' and 'marmalade/citrus' aroma and flavour notes. Overall, heating for ≤ 4 h increased the intensities of positive flavour and aroma notes, while reducing those of 'green/grass', 'hay' and bitterness, whereafter further heating only had a slight effect on the aroma profile at 80 °C (P < 0.05), but not at 90 °C (P ≥ 0.05). The heat treatments, 80 °C/4 h and 90 °C/4 h, were subsequently applied to different batches of retentate (n = 10) to accommodate the effect of natural product variation. Heating at 90 °C produced higher intensities of positive aroma attributes (P < 0.05), but was more detrimental to the phenolic stability, compared to 80 °C. CONCLUSION: After heat treatment, the phenolic content of C. genistoides retentate, reconstituted to beverage strength, still fell within the range of a typical 'fermented' (oxidized) honeybush leaf tea infusion. The change in phenolic composition will not diminish the benefit of an improved sensory profile for the retentate by-product through heating. © 2021 Society of Chemical Industry.

Reduction in flavor-intense components in fish protein hydrolysates by membrane filtration.

Enzymatic protein hydrolysates based on side stream materials from the fish-filleting industry are increasingly explored as food ingredients. However, intense sensory properties, and high salt contents, are often a limiting factor. Most of the sensory attributes, such as fish flavor and salty taste, can be ascribed to low-molecular-weight, water-soluble components, whereas bitterness is associated with small hydrophobic peptides. In this study, protein hydrolysates based on head and backbone residuals from Atlantic salmon (Salmo salar) and Atlantic cod (Gadus morhua) were produced using two different enzymes. The effects of micro- and nanofiltration on the chemical composition, protein recovery, and sensory properties of the final products were investigated. The choice of raw material and enzyme had negligible effects, whereas nanofiltration caused a considerable reduction in metabolites, ash, and the intensity of several sensory attributes. The intensity of bitterness increased after nanofiltration, indicating that small peptides associated with bitter taste were retained by the membrane. Total protein yield after microfiltration was 24%-29%, whereas 19%-24% were recovered in the nanofiltration retentate. PRACTICAL APPLICATION: Enzymatic protein hydrolysates can be included in food products to increase the protein content, and as a nutritional supplement and/or functional ingredient; however, unpalatable and intense flavors limit applications. This study investigated the use of membrane filtration to improve flavor quality and reduce salt content in fish protein hydrolysates. Although some protein loss is unavoidable in micro- and nanofiltration, this study demonstrates the production of fish protein hydrolysates with >90% protein and peptide content, which is suitable for inclusion in foods.

Comparison of volatile trapping techniques for the comprehensive analysis of food flavourings by Gas Chromatography-Mass Spectrometry.

Trapping volatiles is a convenient way to study aroma compounds but it is important to determine which volatile trapping method is most comprehensive in extracting the most relevant aroma components when investigating complex food products. Awareness of their limitations is also crucial. (Un)targeted metabolomic approaches were used to determine the volatile profiles of two commercial flavourings. Four trapping techniques were tested as was the addition of salt to the mixture. Comprehensiveness and repeatability were compared and SBSE proved particularly suitable for extracting components such as polysulfides, pyrazines and terpene alcohols, and provided an overall broader chemical spectrum. SPME proved to be more suitable in extracting sesquiterpenes and DHS in extracting monoterpenes. Adding salt to the sample had only quantitative effects on volatiles as detected by SPME. These results help clarify the advantages and limitations of different trapping techniques and hence deliver a valuable decision tool for food matrix analysis.

Impact of Lactobacillus plantarum 423 fermentation on the antioxidant activity and flavor properties of rice bran and wheat bran.

Rice bran (RB) and wheat bran (WB) fermented with L. plantarum 423 had enhanced odor intensity, especially for sulfides and aromatics. The hydroxyl radical-scavenging activity (73.28 ± 3.18%) and oxygen radical-scavenging activity (2.12 ± 0.08 mmol·TE/g) of RB fermentation broth were better than those of WB fermentation broth. Even at 2 µg/ml, the purified antioxidant fractions from the WB fermentation broth showed strong intracellular ROS-scavenging activity in human umbilical vein endothelial cells (HUVECs), and the purified antioxidant fractions (200 µg/ml) from the RB fermentation broth had a good antiaging effect. The dominant antioxidant components in the RB and WB fermentation broths were acids (70.21%) and ketones (10.64%), these components jointly give the RB and WB fermentation broths a variety of antioxidant properties. These results are beneficial for developing RB and WB deep-processing technology and laid the foundation for the preparation of antioxidant fractions with L. plantarum 423.

Umami fractions obtained from water-soluble extracts of red oncom and black oncom-Indonesian fermented soybean and peanut products.

Red oncom, a fermented product from solid waste of soybean curd process, and black oncom, a similar fermented product but made from defatted peanut cake, have been known to have umami taste. Umami fractions of red oncom and black oncom that are responsible for umami taste have not been investigated yet. The objective of this research was to characterize umami fractions obtained by ultrafiltration and chromatography of both oncoms. The first step, water-soluble extracts of oncoms were ultrafiltered using a membrane with cutoff 3,000 Da and followed by gel filtration chromatography (Sephadex G-25) to obtain umami fractions. Ultrafiltration fractions of red oncom (molecular weight [MW] less than 3,000 Da) and black oncom (MW more than 3,000 Da) had an intense umami taste. The further fractionation by gel filtration chromatography linked to taste dilution analysis yielded umami fractions. Chemical characterization revealed that free glutamic acid, free phenylalanine, and peptides containing their residual amino acids were present in the fractions. PRACTICAL APPLICATION: Umami fractions of red and black oncoms can be used as a source of umami compounds for food industries and food services. The information from this paper can be used by other researchers who will explore umami peptides.

Determination of optimal sample preparation for aldehyde extraction from pale malts and their quantification via headspace solid-phase microextraction followed by gas chromatography and mass spectrometry.

Aldehydes originating from malt play an important role in beer flavour deterioration. In order to better understand the influence of malting process on beer staling, it is necessary to acquire a reliable analytical methodology for determination of beer staling aldehydes in malt. Therefore, the aim of this study was to evaluate extraction parameters, which allow quantification of beer staling aldehydes present in pale malts. The method was validated with respect to linearity (R > 0.9988), limit of detection (0.28 - 0.99 µg/L), limit of quantification (0.92 - 3.31 µg/L), accuracy (± 5%), repeatability (1.3 - 5.3%) and intermediate precision (>20%). The following parameters of sample preparation were evaluated: sample amount, extraction time and temperature, ultrasonication time and oxygen level. Consequently, the best extraction conditions were successfully applied on pale malts. After extraction, the samples were analysed by headspace solid-phase microextraction (HS-SPME) with on fibre carbonyl derivatisation followed by gas chromatography and mass spectrometry (GC-MS). In addition, the salting-out effect during HS-SPME was studied. The method application allowed to identify significant differences (p ≤ 0.05) in the levels of aldehydes among various industrial scale, pale malts. The optimised method could give the information on the aldehyde content introduced into the brewing process and its potential contribution to the overall beer quality.

Optimization of solid phase microextraction combined with gas chromatography-mass spectrometry (GC-MS) to analyze aromatic compounds in fresh tomatoes.

In this study, conditions for solid-phase microextraction coupled to gas chromatography-mass spectrometry to extract and analyze volatile compounds from fresh tomatoes (Solanum lycopersicum cv. Fendi) were optimized. Four main experimental parameters were optimized, including internal standard, fiber material coating, extraction temperature, and salt concentration. The optimal extraction conditions were 85 µm Carboxen/Polydimethylsiloxane fiber, 60°C extraction temperature, 1-heptanol as an internal standard, and without adding sodium chloride in the tomato sample. Analysis of tomato fruit samples using these optimized conditions allowed us to identify 37 volatile compounds that could be grouped into seven categories: aldehydes (11), hydrocarbons (7), alcohols (7), ketones (5), oxygen-containing heterocyclic compounds (3), esters (3), sulfur-and nitrogen-containing heterocyclic compounds (1). PRACTICAL APPLICATIONS: In this study, we optimized a method to extract tomato flavor compounds. In recent years, many consumers complained that tomatoes have poor flavor. A method to extract flavor compounds will assist in characterizing the compounds that contribute to tomato flavor and could be used in the development of tomatoes that have enhanced flavor.

Identification of key aroma-active compounds in sesame oil from microwaved seeds using E-nose and HS-SPME-GC×GC-TOF/MS.

The study investigated the volatile compounds of sesame oil and the effects of microwave processing (0-8 min with 1-min intervals), mainly focusing on the integral flavor characteristics and individual aroma-active compounds. A total of 82 characteristic odors were identified using GC×GC-TOF/MS. Fifteen volatile compounds with the highest odor activity values (OAV > 100) were selected as the key odors contributing to the flavor profile of microwaved sesame oil, including 2-methyl-propanal (pungent, malt, green), 2-methyl-butanal (cocoa, almond), furaneol (caramel), 1-octen-3-one (mushroom), 4-methyl-3-penten-2-one (sweet), 1-nonanol (fat, citrus, green), 2-methyl-phenol (phenol), 2-methoxy-phenol (smoke, sweet), 2-methoxy-4-vinylphenol (clove, curry), 2,5-dimethyl-pyrazine (cocoa, roasted nut, roast beef), 2-furfurylthiol (coffee, roast), 2-thiophenemethanethiol (sulfur), methanethiol (gasoline, garlic), methional (cooked potato), and dimethyl trisulfide (fish, cabbage). The OAVs significantly increased with a longer microwave process. Meanwhile, PCA results based on E-nose and cluster analysis results based on GC×GC-TOF/MS were similar to distinguish flavor formation during the microwave process. PRACTICAL APPLICATIONS: Sesame oils were prepared by a microwave process. Aroma-active compounds with the highest OAVs in sesame oils were not clear. Identification of key aroma compounds of sesame oils could adopt a comprehensive assessment method in combination with E-nose and individual odors detection. Microwave pretreatment as a new processing technology for sesame oil extraction could reduce the time consumption and produce a unique fragrant flavor compared to the traditional roasting process.

Aroma Investigation of Chios Mastic Gum (Pistacia lentiscus Variety Chia) Using Headspace Gas Chromatography Combined with Olfactory Detection and Chiral Analysis.

Chios mastic gum (Pistacia lentiscus var. Chia) exhibits intensely sourish, green, resinous, and woody odor notes with hints of citrus and pine. Despite its attractive flavor, no description of its aroma properties by molecular sensory techniques has been published thus far. A total of 25 odor-active compounds with flavor dilution (FD) factors of 1-512 were identified by gas chromatography-mass spectrometry-olfactometry (GC-MS-O) combined with headspace solid-phase microextraction (HS-SPME) and stir bar sorptive extraction (HS-SBSE). Quantitative analyses performed by multiple HS-SPME and calculation of odor activity values of 10 odorants with high FD factors revealed an essential role of several minor components (e.g., ß-myrcene, limonene, ß-linalool, and perillene) for the overall aroma of mastic gum, besides the dominating compound α-pinene. The indispensable contribution of the minor odorants to mastic gum was further confirmed by aroma recombination and omission tests. Varying enantiomeric excess values of the key odorants were observed by multidimensional GC-MS.

Impact of polyphenols on the headspace concentration of aroma compounds in apple cider.

BACKGROUND: To study the effect of polyphenols on the release of aroma compounds in apple cider, the impact of (-)-epicatechin, hydrocaffeic acid and phloridzin on volatility of 12 typical aroma compounds was investigated by headspace solid phase microextraction and gas chromatography-mass spectrometry. RESULTS: Analysis of variance results showed that increased concentrations of the phenolic compounds significantly affected the headspace concentration of most aroma compounds. The three polyphenols induced a volatility decrease for the majority of hydrophobic aroma compounds, while they exhibited an opposite behavior by salting out some hydrophilic alcohols. (-)-Epicatechin and hydrocaffeic acid showed a higher retention effect on most hydrophobic aroma compounds than phloridzin did. CONCLUSION: This study showed that the polyphenols had varying effects on aroma compound volatility in apple cider. The physicochemical characteristics and spatial conformation of polyphenols and aroma compounds influenced the magnitude of aroma-polyphenol interaction in apple cider. Understanding the effects of polyphenols on aroma release can improve the prediction of aroma profiles through chemical analysis, which assists cidermakers in improving the aroma quality of apple cider. © 2018 Society of Chemical Industry.

Use of odorant series for extra virgin olive oil aroma characterisation.

BACKGROUND: Extra virgin olive oil (EVOO) volatile composition is mainly used as a means of characterisation and authentication, especially for protected denomination of origin (PDO) products. This work investigated the volatile compounds from 25 EVOOs from four Spanish (Cornicabra, Manzanilla Castellana, Picual and Manzanilla Cacereña) and four Italian (Ortice, Ravece, Nocellara del Belice and Itrana) cultivars in terms of odour activity value (OAV). Forty-seven volatile compounds were analysed by solid phase microextraction gas chromatography/mass spectrometry (SPME-GC/MS). OAVs of volatile compounds with similar descriptors were grouped in order to establish eight odorant series: fruity, grass, apple, tomato, floral, woody-spicy, fatty and mushroom. RESULTS: No differences in sensory descriptors were observed among the EVOOs analysed by official VOO sensory analysis. The method of odorant series applied herein was demonstrated to successfully characterise EVOO odour as expected from a sensory panel but using only instrumental analysis of volatile compounds, and giving additional reliable quantitative information. The results can be presented as a 'barcode', providing a visual and effective graphical representation allowing an easy and rapid description of EVOO sensory attributes using instrumental data. CONCLUSION: The odorant series have the potential to better differentiate the aroma of food products, opening new possibilities allowing a schematic and effective visual representation to be used for EVOO quality control and consumer information, especially in new olive oil consuming countries. © 2018 Society of Chemical Industry.

Characteristic antioxidant activity and comprehensive flavor compound profile of scallop (Chlamys farreri) mantle hydrolysates-ribose Maillard reaction products.

The objective of the present study was to improve the utilization of scallop (Chlamys farreri) byproducts by using Maillard reaction. Scallop mantle hydrolysates (SMHs) were prepared using neutrase then reacted with ribose. Thirty-four peptides were identified from SMHs by UPLC-Q-TOF-MS, and the abundance of Asp and Lys suggested the strong Maillard reactivity. The formation of Schiff's base as well as modification of amide I, II and III bands in Maillard reaction products (MRPs) was confirmed by ultraviolet-visible, fluorescence, and Fourier transform infrared spectroscopy. Thirty volatile compounds were produced by the reaction of SMHs with ribose. Moreover, MRPs with enhanced radical scavenging and anti-linoleic acid peroxidation activities over SMHs promoted the survival and reduced the DNA damage of HepG2 cells treated with hydrogen peroxide. These results suggest that SMHs-ribose MRPs can be potentially used as food antioxidant for suppressing of lipid oxidation or protecting of cell from oxidative damage.

Identification of key aromatic compounds in Congou black tea by partial least-square regression with variable importance of projection scores and gas chromatography-mass spectrometry/gas chromatography-olfactometry.

BACKGROUND: Gas chromatography-olfactometry (GC-O) is the most frequently used method to estimate the sensory contribution of single odorant, but disregards the interactions between volatiles. In order to select the key volatiles responsible for the aroma attributes of Congou black tea (Camellia sinensis), instrumental, sensory and multivariate statistical approaches were applied. RESULTS: Using sensory analysis, nine panellists developed eight descriptors: floral, sweet, fruity, green, roasted, oil, spicy, and off-odour. Linalool, (E)-furan linalool oxide, (Z)-pyran linalool oxide, methyl salicylate, ß-myrcene, and phenylethyl alcohol, which were identified from the most representative samples by the GC-O procedure, were the essential aroma-active compounds in the formation of basic Congou black tea aroma. In addition, 136 volatiles were identified by gas chromatography-mass spectrometry (GC-MS), among which 55 compounds were determined as the key factors for six sensory attributes by partial least-square regression (PLSR) with variable importance of projection scores. CONCLUSION: Our results demonstrated that headspace solid-phase microextraction/GC-MS/GC-O was a fast approach for isolation and quantification aroma-active compounds. The PLSR method was also considered to be a useful tool in selecting important variables for sensory attributes. These two strategies, which allowed us to comprehensively evaluate the sensorial contribution of a single volatile from different perspectives, can be applied to related products for comprehensive quality control. © 2018 Society of Chemical Industry.

Effect of Temperature on Flavor Compounds and Sensory Characteristics of Maillard Reaction Products Derived from Mushroom Hydrolysate.

Maillard reaction products (MRPs) were prepared from mushroom hydrolysate (MH) by heating with d-xylose and l-cysteine at various temperatures (100 °C-140 °C) for 2 h at a pH of 7.4. The sensory characteristics of MH and MRPs were evaluated by panelists and volatile compounds were analyzed by GC/MS. Additionally, partial least squares regression (PLSR) was performed to analyze the correlation between quantitative sensory characteristics and GC/MS data. GC/MS results revealed that higher reaction temperature resulted in more nitrogen and sulfur containing compounds in MRPs while alcohols, ketones and aldehydes were the major flavor compounds obtained in MH. PLSR results showed that 3-phenylfuran and 2-octylfuran were the compounds responsible for the caramel-like flavor; 1-octen-3-ol, (E)-2-octen-1-ol and geranyl acetone were significantly and positively correlated to mushroom-like flavor, whereas, 2-thiophene-carboxaldehyde, 2,5-thiophenedicarboxaldehyde and 3-methylbutanal positively affected MRPs meat-like attribute. Overall, 125 °C was identified as the optimal temperature for preparing MRPs with abundant volatile compounds and favorable sensory characteristics; the concentration of free amino acids and 5'-GMP, which are associated with the umami taste, in MRPs derived under 125 °C were 3 to 4 times higher than those in MH.

Effects of radio frequency and high pressure steam sterilisation on the colour and flavour of prepared Nostoc sphaeroides.

BACKGROUND: Nostoc sphaeroides has been used as a highly effective herbal medicine and dietary supplement for thousands of years. The desired dark green colour of fresh N. sphaeroides is converted into an undesirable dark brown during conventional high pressure (HP) steam sterilisation. Radio frequency (RF) sterilisation technology was used in this study to determine its effectiveness in sterilising N. sphaeroides and to achieve better preservation of natural colour and desirable flavour. Sterilisation was carried out using a 6 kW, 27 MHz RF instrument for 10, 20 and 30 min. The degree of microbial kill and the effects of RF sterilisation on colour and flavour were determined and compared with those obtained from HP steam (121 °C, 30 min) sterilisation. RESULTS: The effects of RF sterilisation on colour and flavour (measured using electronic nose) parameters were significantly lower than that in HP steam sterilisation. The RF sterilisation carried out for 20 min achieved logarithmic reduction of bacterial population and met China's national standard while preserving the colour and flavour better. CONCLUSION: Results of the present study indicated that application of RF sterilisation would improve the quality of sterilised N. sphaeroides and broaden its application in the food and health food industries. © 2017 Society of Chemical Industry.

Italian and Spanish commercial tomato sauces for pasta dressing: study of sensory and head-space profiles by Flash Profiling and solid-phase microextraction-gas chomatography-mass spectrometry.

BACKGROUND: The sensory and head-space profiles of Italian and Spanish commercial tomato sauces were investigated. The Flash Profiling method was used to evaluate sensory characteristics. Samples within each set were ranked according to selected descriptors. One hundred volatile compounds were identified by solid-phase microextraction-gas chomatography-mass spectrometry. RESULTS: For Italian samples, the sensory notes of basil/aromatic herbs, acid and cooked tomato were among those perceived most by the assessors, whereas, in Spanish samples, the sensory attributes of garlic/onion and onion/sweet pepper and, in Italian samples, cooked tomato were among those found most frequently. Data were elaborated using multivariate statistical approaches and interesting correlations were observed among the different sensory attributes and related volatile compounds. CONCLUSION: Spanish samples were characterized by the highest content of volatiles linked to the thermal treatment of tomatoes and to raw and sautéed garlic and onion, whereas the Italian samples were characterized by terpenic compounds typical of basil and volatile molecules derived from fresh tomato. These results confirm the influence of both formulation and production processes on the aromatic profile (sensory attributes and volatile compounds) of tomato products, which is probably related to the different eating habits and culinary traditions in Italy and Spain. © 2016 Society of Chemical Industry.

Determination of four flavorings in infant formula by solid-phase extraction and gas chromatography-tandem mass spectrometry.

Increasing attention has been focused on the artificial flavorings added in foods, especially those for infants and children. For the first time, a sensitive and efficient analytical method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the simultaneous identification and quantification of four flavoring agents (vanillin, methylvanillin, ethylvanillin, and coumarin) in infant formula samples. The flavorings in samples were extracted with methanol/water (v/v, 1:1), cleaned up by solid-phase extraction, and determined by GC-MS/MS in selected reaction monitoring (SRM) mode. Both isotope-labeled internal standards and matrix-matched calibration solutions were used to correct the matrix effects. The limit of quantification (LOQ) was calculated as 10 times the standard deviation, and it was 10.0 µg kg (-1) for vanillin, methylvanillin, ethylvanillin, and coumarin. The average recoveries were in the range of 82.8-107.5% with relative standard deviations (RSDs) below 8.9% measured at three concentration levels (10, 50, and 100 µg kg(-1)). The proposed method is suitable for the sensitive and accurate simultaneous determination of four flavoring agents in infant formula samples and also provided potential use for reference in terms of real analysis of other foods.

Centrifugal partition chromatography applied to the isolation of oak wood aroma precursors.

Flavours extracted from oak wood during barrel ageing contribute to the organoleptic character of wines and spirits. The aim of this work was to identify the glycosidic precursors of the key volatile compounds responsible for oak wood aroma. Oak extract is a very complex matrix and, furthermore, precursors are present in very small quantities. Preparative centrifugal partition chromatography (CPC) is a promising solution for purifying the oak extract. The solvent system was selected on the basis of the partition coefficient of glycosidase enzyme activity (Kca). Thanks to the efficacy of CPC separation, three glucoside gallates were subsequently isolated by HPLC chromatography. Vanillin-(6'-O-galloyl)-O-ß-D-glucopyranoside, 3,4,5-trimethoxyphenyl-(6'-O-galloyl)-O-ß-D-glucopyranoside, and (6R,9R)-3-oxo-α-ionol-9-O-(6'-O-galloyl)-ß-glucopyranoside (macarangioside E) were isolated and identified. This was the first time that vanillin-(6'-O-galloyl)-O-ß-D-glucopyranoside was identified and the first time that macarangioside E was isolated from oak wood. Heating macarangioside E resulted in the formation of megastigmatrienone, which has an aroma reminiscent of tobacco.

Development of a solid phase microextraction protocol for the GC-MS determination of volatile off-flavour compounds from citral degradation in oil-in-water emulsions.

The conditions for headspace solid phase microextraction (HS-SPME) analysis of volatile off-flavour compounds in citral emulsion were determined. Type of SPME phase (65 µm PDMS/DVB, 100 µm PDMS and 75µm CAR/PDMS), adsorption temperature and salt concentration were significant factors affecting total peak area in the gas chromatogram and optimised in one factor experiments. Then, adsorption temperature (30-50°C), adsorption time (20-40 min), and salt concentration (0-6M) were studied to develop HS-SPME condition for obtaining the highest extraction efficiency. PDMS/DVB in 65 µm was the optimum fiber because of high adsorption efficiency and good reproducibility. The optimal condition was adsorption at 50°C for 40 min and 6M salt added to sample. Good Linearity, high recovery, good reproducibility and low limit of detection (LOD) for all off-odour compounds according to the optimised SPME conditions indicated that the SPME procedure was applicable for the analysis of the degraded citral products in headspace volatile of emulsion.