Aroma extraction

Aroma compounds, 11 517 Aroma extract dilution analysis (AEDA), 11 519-520... 

Blank I, Grosch W, Evaluation of potent odorants in dill seed and dill herb Anethum graveolens L.) by aroma extract dilution analysis,Sci 56 63-67, 1991. 

Nishimura, O. Identification of the characteristic odorants in fresh rhizomes of ginger (Zingiber officinale Roscoe) using aroma extract dilution analysis and modified multidimensional gas chromatography-mass spectroscopy. J Agr Food Chem 1995 43(11) 2941-2945. 

The impact of MOX upon reductive odors was included in the study of McCord (2003) for MOX at 5-10 mL/L/month over 5 months on a Cabernet Sauvignon wine in commercial scale tanks. Lower concentrations of methyl mercaptan and ethyl mercaptan were observed in the oxygenated wines, but no impact was seen upon disulfides, in spite of the suggestion that concentrations of the disulfides could increase due to direct oxidation of sulfides. Dimethyl sulfide concentrations were not affected, except that lower concentrations were seen in wines with added toasted oak staves or segments, with or without MOX. The concentrations of various oak extracted compounds were also measured in this study, with similar levels seen with and without MOX alongside appreciable increases due to the presence of the oak staves or segments in some cases (e.g., lactones and vanillin), oxygenation appeared to enhance aroma extraction. 

For estimating the contribution of volatile compounds to bread aroma Rothe and coworkers (S) defined "aroma value" as the ratio of the concentration of some volatile compounds to the taste threshold value of the aroma. This concept was further developed by Weurman and coworkers (9) by introducing "odor value", in which aroma solutions were replaced by synthetic mixtures of volatile compounds in water. These mixtures showed the complexity of the volatile fractions of wheat bread, because none of them resembled the aroma of bread. Recently two variations of GC-sniffing were presented (10-11), in which the aroma extract is stepwise diluted with a solvent until no odor is perceived for each volatile compound separately in the GC effluent. The dilution factors obtained indicate the potency of a compound as a contributor to the total aroma. 

Twenty-nine odour-active compounds were detected by using aroma extract dilution analysis (AEDA) [60]. The results of AEDA together with GC-MS analysis showed ethyl 2-methylbutanoate (described as fruity flavour), followed by methyl 2-methylbutanoate and 3-methylbutanoate (fruity, apple-like), 4-hydroxy-2,5-dimethyl-3(2H)-furanone (sweet, pineapple-like, caramel-like), d-decalactone (sweet, coconut-like), l-( ,Z)-3,5-undecatriene (fresh, pineapple-like), and a unknown compound (fruity, pineapple-like) as the most odour-active compounds. 

However, a single GC-O run only is usually insufficient to distinguish between the potent odorants that most likely contribute strongly to an aroma and those odorants that are only components of the background aroma. Therefore, to improve the results, two methods, combined hedonic aroma response measurements (CHARM) analysis [4] and aroma extract dilution analysis (AEDA) [5, 6] have been developed. As discussed in Sect. 16.4 in both methods serial dilutions of food extract are analysed by GC-O. 

Fig. 16.2 Flavour dilution (FD) chromatogram obtained by application of aroma extract dilution analysis on an extract prepared from parsley leaves. The odorants were identified as 1 methyl 2-methylbutanoate, 2 myrcene, 3 l-octen-3-one, 4 (2)-l,5-octadien-3-one, 5 2-isopropyl-3-me-thoxypyrazine, 6p-mentha-l,3,8-triene, 71inalool, 8 2-sec-butyl-3-methoxypyrazine, 9 (.Z)-6-dece-nal, 10 / -citronellol, 11 ( , )-2,4-decadienal, 12 / -ionone, 13 myristicin, 14 unknown. RI retention index. [30, 31]...

As reported in the previous section, AEDA is performed with a concentrated aroma extract. However, concentration of the volatile fraction might lead to losses of odorants, e.g. by evaporation and by enhanced side reactions in the concentrated extract. Consequently, the odour potency of these odorants can be underestimated in comparison to those whose levels are not reduced during concentration. To clarify this point, aroma extract concentration analysis (AECA) [56] should check the results of AEDA. AECA starts with GC-O of the original extract from which the non-volatile components have been removed. The extract is then concentrated stepwise by distilling olf the solvent, and after each step an aliquot is analysed by GC-O [56]. 

Table 16.4 Potent odorants of boiled beef—comparison (AECA) with AEDA [56] of aroma extract concentration analysis...

The highly volatile odorants are not detected or are underestimated when the screening method is applied to an aroma extract. These compounds are lost when the extract is concentrated or they are masked in the gas chromatogram by the solvent peak. To overcome this limitation, the screening has to be completed by GC-O of static headspace samples (GCOH Fig. 16.3) [59-61]. 

It is very common to combine methods in obtaining aroma isolates. The simultaneous distillation/extraction method previously described is an example. Another popular combination method initially involves the solvent extraction of volatiles from a food and then high-vacuum distillation of the solvent/aroma extract to provide a fat-free aroma isolate. This technique is broadly used today to provide high-quality aroma extracts for numerous purposes. The apparatus used in solvent removal has been improved upon to reduce analysis time and efficiency the modified method is termed solvent-assisted flavour extraction (SAFE) [16]. 

As mentioned in the introduction to this section, there is the opportunity to recover aroma compounds from baking or roasting exhaust gases. The patent literature contains numerous references to the recovery of aroma compounds using this approach, most commonly from cocoa, coffee, or tea processing. Aroma compounds from the roaster exhaust gases are either condensed in cryogenic traps [29-32] or collected on absorbents (e.g. charcoal [33]) and then solvent-extracted to obtain a concentrated aroma extract. The concentrated extract may be used to aromatise a similar product (e.g. soluble coffee) or may be used to flavour other products (e.g. coffee-flavoured ice creams). 

Flavorzyme is a commercially available proteolytic enzyme preparation by Novo Nordisk Bioindustrials. It can be used to obtain a meat-like process flavouring from defatted soybean meal. With the help of aroma extract dilution analysis, Wu and Cadwallader [61] showed in their study of 2002 the presence of key aroma compounds of roasty, meat-like aroma in the enzymatically hydrolysed and heated hydrolysed protein, e.g. maltol, furaneol, methanethiol and furanthiol derivatives. 

Giri, A., Osako, K., Okamoto, A., Okazaki, E., and Ohshima, T. (2011a). Antioxidative properties of aqueous and aroma extracts of squid miso prepared with Aspergillus ori/zae-inoculated koji. Food Res. Int. 44, 317-325. 

In contrast to the decaffeination of coffee, which is primarily executed with green coffee, black tea has to be extracted from the fermented aromatic material. Vitzthum and Hubert have described a procedure for the production of caffeine-free tea in the German patent application, 2127642 [11]. The decaffeination runs in multi-stages. First, the tea will be clarified of aroma by dried supercritical carbon dioxide at 250 bar and 50°C. After decaffeination with wet CO2 the moist leaf-material will be dried in vacuum at 50°C and finally re-aromatized with the aroma extract, removed in the first step. Therefore, the aroma-loaded supercritical CO2 of 300 bar and 40°C will be expanded into the extractor filled with decaffeinated tea. The procedure also suits the production of caffeine-free instant tea, in which the freeze-dried watery extract of decaffeinated tea will be impregnated with the aromas extracted before. 

For aroma extracts, the blank sample is a mixture of the solvents used in the extraction, and are concentrated in the same way as the aroma isolate. Some volatiles in aroma extracts may derive from trace impurities of the solvents. For headspace techniques, a blank run is also recommended to check impurities coming from the tubings and/or adsorbents used. 

Figure G1.3.1 Determination of the retention index (Rl) of an unknown compound C in an aroma extract (A) by comparing with a series on n-alkanes (B) analyzed under the same GC-conditions. 

Inject the aroma extract/sample spiked with the standard, prepared in steps 4 to 6. 

Grosch, W. 1993. Detection of potent odorants in foods by aroma extract dilution analysis. Trends Food Sci. Technol. 4 68-73. 

Gas chromatography/olfactometry (GC/O) based on dilution analysis (e.g., CharmAna-lysis or Aroma Extraction Dilution Analysis) gives an indication of what compounds are most potent in the aroma of foods. The application of SPME to GC/O dilution analysis can be achieved by varying the thickness of the fiber phase and the length of exposure, resulting in various absorbant volumes. 

Grosch, W. 1994. Determination of potent odourants in foods by aroma extraction dilution analysis (AEDA) and calculation of odour activity values (OAVs). Flavour Fragrance J. 9 147-158. 

At a meeting in Germany in 1983, the idea of using repeated sniffs of sequentially diluted samples, now generally called dilution analysis, was proposed (Acree and Barnard, 1984). This led to the publication of CharmAnalysis in 1984 and Aroma Extract Dilution Analysis (AEDA) in 1987, both of which were based on the idea of quantifying potency by dilution to threshold. Potency here is similar to the concept of titer or the amount of dilution necessary to... 

ACS American Chemical Society AED atomic emission detection AEDA aroma extract dilution analysis AMC 7-amido-4-methylcoumarin ANS anilinonapththalene sulfonate AOAC Association of Official Analytical Chemists... 

A first approach to distinguish between the odor-active compounds and the many odorless volatiles present in such aroma extracts is the application of gas chromatography/olfactometry (GCO, formerly called "sniffing-technique" [13-17]). 

Figure 6. Illustration of the static headspace/aroma extract dilution analysis (SHA) [adapted from Guth and Grosch, Annual report of the Deutsche Forschungsanstalt fur Lebensmittelchemie 1993, p. 27],...

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