Development of a 3D Printer for the Manufacture of Functional Food Protein Gels.

The use of additive manufacturing is growing in multiple sectors, including food, and its scientific and technological challenges form the subject of much ongoing research. One current hurdle is the implementation of the 3D printing process for meat protein matrices. This article gives an overview of the various 3D printers used to study the printability properties of foods and presents the development of a 3D printer designed to print food protein gels. Printhead development (flow rate and temperature control) and the modifications made to the printing plate (temperature control) are described and discussed in relation to the constraints highlighted in a first prototype. A second, developed prototype was characterized and validated. This last phase showed perfect control of the prototype in the purging of the extrusion system, the flow rate, the calibration and the displacement of the printhead, along with the temperatures at both printhead and plate. A study of the printed gels also revealed good repeatability of the printed gel geometry and pointed to new ways to improve the process. In the near future, the protein gels that will be printed from this prototype will serve as a base for texturizer-free functional foods for people with chewing difficulties.

Relevance of two-dimensional gas chromatography and high resolution olfactometry for the parallel determination of heat-induced toxicants and odorants in cooked food.

The assessment of the dual impact of heating treatments on food safety and aroma is a major issue for the food sector. The aim of the present study was to demonstrate the relevance of multidimensional GC techniques, olfactometry and mass spectrometry for the parallel determination of process-induced toxicants and odorants in food starting with cooked meat as a food model. PAHs were analyzed by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry after extraction by accelerated solvent extraction (ASE-GC × GC-TOF/MS). Odour-active compounds were determined by dynamic headspace-GC hyphenated with eight booth olfactometry and mass spectrometry (DH-GC-MS/8O) and DH-heart-cutting multidimensional GC hyphenated with olfactometry and mass spectrometry (DH-GC-GC-MS/O). For PAH determination, the GC × GC conditions consisted of a combination of a primary non-polar BPX-5 column and a secondary polar BPX-50 column, and a modulation period of 5s. In terms of linearity (R(2) ranging from 0.985 to 0.997), recovery rate (84-111%) and limit of detection (5-65 ng/kg of cooked meat), the ASE-GC × GC-TOF/MS method was found consistent with the multiresidue determination of 16 PAHs including benzo[a]pyrene in cooked meat. For aroma compounds, DH-GC-MS/8O and DH-GC-MS/O revealed 53 major meat odour-active compounds. A customized heart-cutting GC-GC-MS/O enabled the coeluting odour zones with high odour-activity to be resolved and revealed 15 additional odour-active compounds. Finally, these developments of multidimensional approaches were used to investigate the balance between 16 PAHs and 68 odour-active compounds generated with different cooking techniques.

Effect of added thiamine on the key odorant compounds and aroma of cooked ham.

This study shows that thiamine plays a major role in the formation of three key odorants of cooked ham: 2-methyl-3-furanthiol, 2-methyl-3-methyldithiofuran, and bis(2-methyl-3-furyl)disulphide. Analyses revealed that under identical cooking conditions, the productions of these three aroma compounds increase in a closely intercorrelated way when the dose of thiamine increases. Using a specific 2-methyl-3-furanthiol extraction-quantification method, it was possible to relate the amounts of thiamine added in model cooked hams to the amounts of 2-methyl-3-furanthiol produced in the cooking process. Sensory analyses highlighted the role of thiamine as a precursor of cooked ham aroma.

Volatile compounds of Viola odorata absolutes: identification of odorant active markers to distinguish plants originating from France and Egypt.

Absolutes isolated from Viola odorata leaves, valuable materials for the flavor and fragrance industry, were studied. Violets are mainly cultivated in France and Egypt and extracted locally. The absolutes of the two origins showed different olfactory profiles both in top and heart notes, as evidenced by sensory analysis. The aims of this study were i) to characterize the volatile compounds, ii) to determine the odorant-active ones, and iii) to identify some markers of the plant origin. Two complementary analytical methods were used for these purposes, i.e., headspace solid-phase microextraction (HS-SPME) using different fiber coatings followed by GC/MS analysis and gas chromatography - olfactometry/mass spectrometry (GC-O/MS) applied to violet leaf extracts. From a total of 70 identified compounds, 61 have never been reported so far for this species, 17 compounds were characterized by both techniques (with seven among them known from the literature), 23 compounds were solely identified by HS-SPME GC/MS (among them only two being already mentioned as components of violet absolutes in the literature), and, finally, 30 compounds were only identified by GC-O/MS. According to the HS-SPME GC/MS analyses, ethyl hexanoate and (2E,6Z)-nona-2,6-dienol were specific volatile compounds of the sample with French origin, while (E,E)-hepta-2,4-dienal, hexanoic acid, limonene, tridecane, and eugenol were specific of the samples with Egyptian origin. Additional compounds that were not detected by HS-SPME GC/MS analysis were revealed by GC-O analyses, some of them being markers of origin. Pent-1-en-3-ol, 3-methylbut-2-enal, 2-methoxy-3-(1-methylethyl)pyrazine, 4-ethylbenzaldehyde, ß-phenethyl formate, and 2-methoxy-3-(2-methylpropyl)pyrazine revealed to be odorant markers of the French sample, whereas cis-rose oxide, trans-rose oxide, and 3,5,5-trimethylcyclohex-2-enone were odorant markers of the Egyptian samples.

Identification and origin of odorous sulfur compounds in cooked ham.

The aim of this work was to identify and gain further knowledge on the origin of sulfur compounds present in the volatile fraction of cooked ham, and on their role in the aroma of this product. To this end, we performed analyses by one- and two-dimensional gas chromatography coupled with mass spectrometry, and olfactometry. Among the odorant sulfur compounds identified, three furans present in trace amounts proved to have very intense odours responsible for the "meaty, cooked ham" notes of this pork product. They were 2-methyl-3-furanthiol, 2-methyl-3-(methyldithio)furan and bis(2-methyl-3-furyl) disulphide. Addition of thiamine or cysteine also enabled us to study the effect of these odour precursors on the formation of odorant furans during the cooking of ham. The results revealed a direct link between the thermal degradation of thiamine and the formation of these compounds. By contrast, addition of cysteine in the presence of fructose or xylose did not appreciably increase their production.

Effect of nitrite on the odourant volatile fraction of cooked ham.

The aim of this work was to reliably identify the key odour compounds in cooked ham and acquire new knowledge on the role of sodium nitrite on the formation of its aroma. Gas chromatography coupled with mass spectrometry and (or) olfactometry was used. In all, 24 odourants were identified in the volatile fraction of cooked ham. Their main origins are discussed. Orthonasal sniffing of the hams was used to study how these substances contributed to the overall aroma of the product. The aroma of cooked ham is a balance between that of certain sulfur compounds produced during cooking and that of oxidation compounds commonly found in cooked meats. In the absence of nitrite, this balance is disturbed by extensive formation of oxidation compounds that mask the meaty notes induced by the sulfur compounds.

Analysis of the volatile profile and identification of odour-active compounds in Bayonne ham.

The aim of this work was to reliably identify odour-active compounds in dry-cured ham using powerful analysis methods for the volatile fraction. For this purpose, dynamic headspace gas chromatography combined with eight-way olfactometry using a panel of eight sniffers was used. One- and two-dimensional gas chromatography coupled with mass spectrometry and (or) olfactometry were also used. More than 600 compounds from the volatile fraction of dry-cured ham were identified and their biochemical origins are discussed. They covered a wide diversity of structures and chemical functions. Only 29 of them proved odour-active. Comparison of the results of GC-O analysis with those obtained by orthonasal sniffing of the dry-cured ham helped to gain a better understanding of how these substances contributed to the overall aroma of the product. Thus, "Fruity-Floral", "Green-Vegetable" or "Plastic-Chemical" odours intensively perceived by GC-O have been poorly perceived by orthonasal sniffing. By contrast, "Animal-Meat products" or "Butter-Lactic-Cheesy" odours have been much better perceived by orthonasal sniffing. These results indicate that to understand the interactions between odour-active compounds, experimental doping with carefully selected odour-active compounds will be necessary.

Characterization of volatile compounds of Indian cress absolute by GC-olfactometry/VIDEO-sniff and comprehensive two-dimensional gas chromatography.

Indian cress (Tropaeolum majus L.) has been consumed in salad or soup for decades, but its odor's detailed molecular composition is still unknown. Here we report on the study of the odorant profile and odor-impact compounds of Indian cress absolute by GC-olfactometry/vocabulary-intensity-duration of elementary odors by sniffing (GC-O/VIDEO-Sniff) on an eight-way multiport system, combined with GCxGC-MS analyses for the identification of odorant trace constituents. Odor impact compounds of Indian cress absolute were determined by GC-O, and the overall influence of sulfury and fruity notes stood out. Forty-four odorant compounds were identified among which 22 (50% of the identified odorant molecules) were identified by using comprehensive two-dimensional GC coupled to a time-of-flight-mass spectrometer (TOFMS). These trace compounds were not detected by 1D-qMS or could only be found with specific searches once they were detected by comprehensive 2D-GC, although they were well perceived by the judges in GC-O. This was amongst others the case for the two molecules having the highest odor impact, (E)-hex-2-enal (fruity) and diethyl trisulfide (alliaceous, sulfury, cabbage). A powerful sulfur-containing odor compound whose first identification in cress was recently reported by the authors was detected by GC-O: O,S-diethyl thiocarbonate (fruity/red fruit and sulfury odor).

Identification of odor impact compounds of Tagetes minuta L. essential oil: comparison of two GC-olfactometry methods.

Odor impact compounds of Tagetes minuta L. essential oil were studied by gas chromatography (GC)-olfactometry using aroma extract dilution analysis (AEDA) and vocabulary-intensity-duration of elementary odors by sniffing (VIDEO-Sniff). AEDA was conducted by direct injection and revealed the presence of 43 odorant zones. Highest flavor dilution (FD) values were obtained for ethyl 2-methylpropanoate, ethyl 3-methylbutanoate, (E)-ocimenone, two tentatively identified thiols, and two yet unknown compounds. VIDEO-Sniff was realized by dynamic headspace sampling (D-HS) combined with 8W-GC-olfactometry where eight sniffers simultaneously detect volatile compounds obtained from a single chromatographic separation and revealed the presence of 42 odorant zones. Odorant trace compounds detected by GC-O that were present in quantities inferior to the GC-qMS system's detection limit and those subject to coelutions were identified by GC x GC-time-of-flight mass spectrometry (TOFMS). A total amount of 37 odorant components could be identified by VIDEO-Sniff, and the strong influence of the fruity notes of numerous esters stood out. Highest olfactory signals were obtained for ethyl 2-methylpropanoate, ethyl 2- and 3-methylbutanoate, and oct-1-en-3-one. Both methods hence come to the conclusion that ethyl 2-methylpropanoate and ethyl 2- and 3-methylbutanoate are among the main odorants in Tagetes minuta L. essential oil. Differences, advantages, and drawbacks of both GC-O methods are discussed.

First identification of O,S-diethyl Thiocarbonate in Indian Cress absolute and odor evaluation of its synthesized homologues by GC-sniffing.

Indian cress (Tropaeolum majus L.) absolute was studied by GC-olfactometry (VIDEO-Sniff method) in order to identify odor-active aroma compounds. Because of its fruity-sulfury odor note, a compound that has never been identified in plant extracts before stood out: O,S-diethyl thiocarbonate, present at 0.1% (percentage of the total GC/FID area) in the extract. GCxGC-TOFMS allowed for a clean mass spectrum to be obtained, and isolation by preparative GC followed by NMR studies allowed its identification. Here, we report on the first detection of O,S-diethyl thiocarbonate in Indian cress absolute by GC-olfactometry/VIDEO-Sniff and on its isolation and identification. The synthesis and odor evaluation of its homologues are presented.

Fast characterization of cheeses by dynamic headspace-mass spectrometry.

This study describes a rapid method to characterize cheeses by analysis of their volatile fraction using dynamic headspace-mass spectrometry. Major factors governing the extraction and concentration of the volatile components were first studied. These components were extracted from the headspace of the cheeses in a stream of helium and concentrated on a Tenax TA trap. They were then desorbed by heating and injected directly into the source of a mass spectrometer via a short deactivated silica transfer line. The mass spectra of the mixture of volatile components were considered as fingerprints of the analyzed substances. Forward stepwise factorial discriminant analysis afforded a limited number of characteristic mass fragments that allowed a good classification of the batches of cheeses studied.