JP6846947B2 - Evaluation method of contribution of fragrance compounds to retronasal aroma - Google Patents

Description

The present invention relates to a method for evaluating the degree of contribution of various perfume compounds that can be added to edible products such as beverages or foodstuffs to retronasal aroma.
The present invention also relates to a food and drink flavor whose expression of retronasal aroma is controlled based on the degree of contribution positioned based on the evaluation method, and a food and drink containing the food and drink flavor.

With the diversification of consumers' tastes for food and drink, it is required to develop food and drink that responds to the diversity. With the passage of time, diversity is also required for flavors, which are one of the raw materials for food and drink.
Generally, when a flavorist develops a blended fragrance, various fragrance compounds are mixed in a container so as to approach the target fragrance. Apply the mixed fragrance to the odor paper and check the fragrance (orthonasal aroma) that escapes through the anterior nares and into the nasal cavity. Furthermore, by adding the prepared flavor to water or foods and drinks close to the final product, the flavors (retronasal aroma) perceived when the flavors released from the foods and drinks pass through the back nostrils and into the nasal cavity during the food and drink process are produced. Confirm. At this time, since there is a difference between the orthonasal aroma and the retronasal aroma due to changes due to the reaction of the fragrance compound in the oral cavity, the amount to be mixed is finely adjusted. By repeating this work, we will develop a blended flavor that exerts the target fragrance when consumers eat food and drink.
In this way, it is an important issue in the perfume industry to evaluate how much each perfume compound of the blended perfume contributes to the sensation when eating and drinking, and to develop a blended perfume with high palatability. However, this method of evaluating the degree of contribution has to rely on the sensibilities of skilled flavorists, and it is difficult to quantify the degree of contribution for each fragrance compound.
Until now, the degree to which each fragrance compound of the fragrance compound contributes to the senses has been evaluated from the orthonasal aroma, and the fragrance compound having a high palatability has been developed.

For example, as a concept for estimating how much each flavor compound contributes to the aroma of food and drink, a value called Odor Activity Value (OAV) obtained by dividing the concentration of the flavor compound in food and drink by a threshold value may be used. Yes (see Non-Patent Document 1). However, it is not possible to evaluate the contribution of each flavor compound during eating and drinking, which changes with time, by the conventional method of obtaining OAV.

In addition, as a method for evaluating the degree of contribution using gas chromatography, qualitative analysis of odorous substances in the analysis target is performed, and Flavor Dilution Factor (FD factor: Fn) of each odorous substance is performed by Aroma Extract Dilution Analysis (AEDA). Is calculated, and these are multiplied by the intrinsic threshold (Tn) of each odorous substance to obtain the FD value (Fn × Tn), and the amount of each odorous component is calculated. (See) is also known, but this FD factor cannot evaluate the contribution of each flavor compound during eating and drinking.

In addition, regarding retronasal aroma during eating and drinking, a method for evaluating fragrances that have good aroma diffusivity at the start of eating and drinking as initial fragrances, and fragrances that exhibit appropriate sustainability as persistent fragrances (patent). (Refer to Reference 2) is also disclosed, but it is not possible to evaluate the contribution of each flavor compound during eating and drinking by this evaluation method.

In addition, although there are many methods for detecting retronasal aroma by device measurement, there is a detection limit for any device, and it is not possible to detect all of the flavor compounds contained in food and drink. It is difficult to evaluate the contribution of retronasal aroma to fragrance compounds that are below the detection limit in the measurement of time and cannot obtain actual measurement values.

Japanese Unexamined Patent Publication No. 2004-325116 Japanese Unexamined Patent Publication No. 2009-31138

Lebensm. -Wiss.u.-Technol. (1993), 26,347-356

The subject of the present invention is to solve the conventional problems, provide a method for evaluating the contribution of a flavor compound in the process of eating and drinking, and consider the contribution evaluated by the method to obtain retronasal aroma. An object of the present invention is to provide a food or drink compounded fragrance whose expression is controlled and a food or drink containing the food or drink compounded fragrance.

The present inventors have calculated the concentration accumulated value of retro nasal aroma in food and (C _R), Retoronezaru threshold concentration accumulated value when the threshold (C _T) were estimated at the time of eating, by using those A study was conducted to find _{a value (CR} / _CT ) indicating the degree of contribution.

The scent drifting from food and drink and the scent perceived during eating and drinking may have different sensory impressions. Therefore, if the perfume compound that escapes from the mouth to the nose during eating and drinking is measured, it is possible to perform an analysis that is highly relevant to the sensation when actually eating and drinking.
Specifically, by using PTR-MS (Proton Transfer Reaction-Mass Spectrometry), the concentration of each perfume compound of retronasal aroma excreted from the nose during eating and drinking can be measured over time. I was able to obtain it continuously.

When detecting retronasal aroma by instrument measurement (specifically, PTR-MS) and analyzing the concentration change of each fragrance compound obtained, the peak top concentration of the respiratory cycle can be used, but it is reproducible. The area value under the curve (concentration integrated value) for each respiration was used because the result was obtained and the variation among the subjects was suppressed.

After swallowing a certain amount of food and drink, the integrated concentration of retronasal aroma decreases over time, and the decay of the integrated concentration with respect to time or respiratory rate can be approximated by a power function. Among coefficients of the power function ^{_{(C R = a * t -b}} ), t is the number of breaths, a initial amount (1 respiratory th concentration accumulated value), b is the damping coefficient, the initial and the addition amount of perfume compounds The amounts are almost proportional, and the damping coefficient is almost independent of the amount added. By utilizing this relationship, it is possible to estimate the integrated value of the concentration of retronasal aroma during eating and drinking even if the amount of addition is the limit of detection by device measurement (specifically, PTR-MS). It became.

By evaluating the amount of addition (threshold concentration) that can be detected when a certain amount of food and drink is swallowed and applying the above relationship, the concentration of retronasal aroma discharged from the nostrils when the threshold sample is swallowed is integrated. The value can be calculated. In addition, since the concentration released immediately after swallowing (concentration of the first breath) is the maximum, the integrated concentration value of the first breath was used as the integrated value of the retronasal threshold concentration during eating and drinking.

Based on the above findings, the inventors have completed the present invention as follows.
[1]
It is a method to evaluate the contribution of flavor compounds that are felt after swallowing food and drink.
1) The threshold concentration of the aqueous solution is discharged from the mouth through the nose after swallowing and is discharged from the nose. 2) The food and drink is discharged from the mouth after swallowing through the nose through the nose. An evaluation method characterized in that the ratio of the concentration of the fragrance compound or the integrated value of the fragrance concentration is defined as the degree of contribution of the fragrance compound.
[2]
The evaluation method according to [1], wherein the concentration of the fragrance compound or the integrated value of the fragrance concentration according to [1] is based on the result measured by a real-time analyzer.
[3]
The evaluation method according to [1] to [2], wherein 2) described in [1] is an aroma concentration integrated value at each respiratory rate estimated by a power function that approximates the attenuation for each respiration.
[4]
The evaluation method according to [1] to [3], wherein 1) described in [1] is the concentration of the first breath or the integrated value of the aroma concentration.
[5]
A method of evaluating the degree of contribution by the method described in [1] to [4] and evaluating the fragrance balance.
[6]
A blended fragrance composition prepared based on the contribution or fragrance balance evaluated by the methods described in [1] to [5].
[7]
A food or drink to which the blended flavor composition described in [6] is added.

That is, in the present invention, the fragrance compound that passes through the mouth to the nose and is discharged from the nose during eating and drinking of food and drink containing the fragrance compound that emits fragrance is measured by a real-time analyzer, and the concentration integrated value of the fragrance compound is measured for each breath. calculates, by approximated by a power function, which varies over time retro nasal aroma concentration accumulated value of the (C _R) can be estimated for each breath, also be discharged in one respiratory th when the threshold concentration that Retoronezaru threshold concentration accumulated value when (C _T) was estimated to, C R _/ C _T represents the contribution of each fragrance compound, it can seek sensory contribution in the respiratory cycle for each respiratory rate, scent balance This is a method for evaluating the degree of contribution of retronasal aroma to a fragrance compound for food and drink, which is characterized by evaluating.

According to the evaluation method of the present invention, the contribution of various fragrance compounds in the nasal cavity can be objectively evaluated without relying on the experience of flavorists as in the past. In addition, it is possible to evaluate the degree of contribution that changes over time after eating and drinking. Furthermore, by using the contribution calculated based on the evaluation method, the balance of the aroma felt after eating and drinking can be predicted, so that the aroma intensity can be adjusted according to the purpose before developing the blended flavor composition. Can be examined, and a blended fragrance composition can be efficiently developed.

FIG. 1 shows a sensory evaluation and a contribution evaluation of each incense tone immediately after swallowing with respect to water in which 0.1% of the basic blended flavor composition for coffee (reference product 3) was perfume in Example 3. It is a scatter diagram showing the relationship between the average value of the sensory evaluation and the value obtained by logarithmizing the contribution degree (fragrance balance prediction). FIG. 2 shows a sensory evaluation and a contribution evaluation of each incense tone 30 seconds after swallowing with respect to water in which 0.1% of the basic blended flavor composition for coffee (reference product 3) was perfume in Example 3. It is a scatter diagram showing the relationship between the average value of the sensory evaluation and the value obtained by logarithmizing the contribution degree (fragrance balance prediction) at that time.

Among the foods and drinks in the present invention, the beverage is not particularly limited, but is a tea beverage such as green tea, matcha or tea, a soft beverage such as coffee, cocoa, carbonated beverage, fruit juice beverage, sports drink and flavored water (near water). Examples include alcoholic beverages such as water, gin, vodka, whiskey, wine, chuhai, sour, shochu and Japanese liquor, and beverages such as beer, sparkling liquor, low alcohol beer and non-alcoholic beer.
Beverages to which fragrances can be added are particularly preferable, specifically coffee, fruit juice beverages, sports drinks, flavored water, sour, chu-hi, beer and the like, and coffee is particularly preferable.
Foods include frozen desserts such as ice cream, sherbets, and ice candy; Japanese / Western confectionery, jams, candy, jelly, gums, bread, curry, stew, Japanese-style soup, Western-style soup, and Chinese soup. Examples include soups such as, flavor seasonings, various instant beverages and foods, various snack foods, and nursing care foods. Preferred examples include frozen desserts, soups and jellies.

The flavor compound in the present invention is not particularly limited, but may be any flavor compound contained in animals and plants as a raw material for foods and drinks, and a flavor that can be added as a food additive. For example, it is described in the JPO Gazette Public Information and Conventional Techniques (Fragrances) Part II Food Flavors (Japan Patent Office), Natural Fragrance Base Materials (Japan Flavor Industry Association) and Synthetic Fragrances (Chemical Industry Daily). Examples include fragrances.

By associating the degree of contribution with the incense tone, it is possible to evaluate various scents that are felt all at once after swallowing food and drink by dividing them into each incense tone, and it is also possible to predict the balance of incense. The balance can be used especially when evaluating the feeling of throat and aftertaste, and when evaluating the masking effect. It is also possible to visualize the balance using a graph or the like.

Hereinafter, the present invention will be described in detail according to the embodiment.
In the present invention, the threshold concentration indicates a lower limit concentration that can be recognized when drinking water in which a single perfume compound is perfume in water is prepared at multiple levels and the perfumed drinking water is swallowed.
In the present invention, Retoronezaru threshold concentration accumulated value (C _T) is a beverage containing perfume compounds of the threshold concentration to 1 breath after swallowing, is estimated to be discharged from the nose missing from the mouth to the nose Indicates the integrated concentration value.
In the present invention, the term "after swallowing" may be any respiratory rate after the first breath.
In the present invention, in order to obtain the power function, it is preferable to measure between the 1st to 100th breaths continuously, and more preferably between the 1st to 20th breaths, and between the 1st to 10th breaths. Is most preferable to measure.

Swallow foods and drinks to which multiple flavor compounds are added, measure each flavor compound released from the nostrils in real time using PTR-MS, and integrate the retronasal aroma concentration for each breath of each flavor compound (C). ) Is calculated. Then, the attenuation of the retronasal aroma concentration integrated value that changes with each respiration (t) ^{is approximated by a power function (C = a * t -b} ), and the initial amount (a) (concentration integrated value of the first respiration) is used. Obtain the damping coefficient (b). The same measurement is performed a plurality of times, and the initial amount (a) and the attenuation coefficient (b) are averaged by the number of measurements.

Since the amount of the fragrance compound added and the initial amount are almost proportional to each other, the initial amount (a) is calculated according to the amount of the fragrance compound added. Since the attenuation coefficient (b) is almost independent of the addition amount, the value obtained above is used as it is. In this way, it is possible to obtain a power function equation corresponding to the amount added, calculated retro nasal aroma concentration accumulated value for each breath of the perfume compound (C _R).
The initial amount of the threshold level of perfume compounds were estimated from the relationship described above, to the initial amount Retoronezaru threshold concentration accumulated value (C _T).

The ratio of the integrated values of the two retronasal aroma concentrations ( _CR / _CT ) can indicate the contribution of each fragrance compound to any respiratory rate.
Hereinafter, the present invention will be described in more detail with reference to Examples.

Next, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to these Examples.

The exhaled breath discharged from the nostrils after swallowing food and drink was introduced into a proton transfer-reaction mass spectrometer PTR-MS (IONICON Analytic) capable of detecting volatile organic compounds to obtain an absolute concentration of specified ions. Table 1 shows the PTR-MS parameters for the reaction chamber and introduction.

[Example 1]
A basic blended flavor composition for coffee (reference product 1) was prepared based on a model blending formulation composed of a flavor compound contained in coffee. Table 2 shows the formulation of Reference Product 1.

参考品１を水に０．１％添加し、試料とした。この試料を５℃に冷却し、試料を１０ｍｌ飲んだ後の鼻孔から放出される香料化合物をＰＴＲ−ＭＳによって測定した。測定時間は喫飲後およそ１分間とした。

Reference product 1 was added to water at 0.1% to prepare a sample. The sample was cooled to 5 ° C., and the perfume compound released from the nostrils after drinking 10 ml of the sample was measured by PTR-MS. The measurement time was about 1 minute after drinking.

The continuously changing concentration obtained as a measurement result was analyzed as a concentration integrated value for each respiration, and the value was approximated by ^{a power function (C = a * t-b).} The same measurement was performed a plurality of times, and the coefficients (a, b) were averaged by the number of measurements. Table 3 shows the coefficients (a, b) of the exponentiation function that derive the relationship of the integrated value of retronasal aroma concentration (C) with respect to the respiratory rate (t) for the constituent fragrance compounds of Reference Product 1.

Each of the 7 components of each fragrance compound constituting Reference Product 1 was added to water to prepare a sample. The addition concentration was diluted in 1% to 10-fold increments to prepare in multiple stages. Evaluation was performed in order from a sample having a low concentration that could not be detected, and the addition concentration that could be detected when 10 ml was swallowed was defined as the threshold concentration. Initial amount considered as being released from the nostrils when the amount to be the threshold concentration, that is calculated Retoronezaru threshold concentration integrated value (C _T). Threshold concentration and Retoronezaru threshold concentration accumulated value of the configuration perfume compounds of Reference product 1 a (C _T) are shown in Table 4.

Regard reference materials 1, obtained by calculating respiration th and 10 breaths th retro nasal aroma concentration accumulated value from the function shown in Table 3 (C _R), divided by Retoronezaru threshold concentration accumulated value (C _T) Table 5 shows the values of the degree of contribution to be made.

If the contribution is greater than 1.0, i.e. _CR / _CT > 1.0, it indicates that a concentration above the threshold is being released from the nostrils and the person can perceive the perfume compound. It is considered that there is, and the larger the value, the higher the degree of contribution. Contribution is smaller than 1.0, that is, when the C _{R /} C T _<1.0, show that a concentration of less than the threshold is emitted from the nostrils, when the person is not able to perceive the fragrance compounds positioned Be done. This contribution can be changed by adjusting the blending amount of the flavor composition in the formulation and the concentration added to the beverage.

[Example 2]
A basic compounded fragrance composition for grapes (reference product 2) was prepared based on a model compounding formulation composed of a fragrance compound contained in grapes. Table 6 shows the formulation of Reference Product 2.

A 100 ml aqueous solution containing 15 g of granulated sugar, 8 g of high fructose corn syrup, 2 g of gelatin, and 0.25 g of citric acid is heated to 80 ° C., 0.2% of reference product 2 is added to the jelly dough, and the sample jelly is cooled. And said. This sample was cooled to 5 ° C., and the perfume compound released from the nostrils after chewing and swallowing 10 g of the sample was measured by PTR-MS. The measurement time was about 1 minute after eating.

The continuously changing concentration obtained as a measurement result was analyzed as a concentration integrated value for each respiration, and the value was approximated by ^{a power function (C = a * t-b).} The same measurement was performed a plurality of times, and the coefficients (a, b) were averaged by the number of measurements. Table 7 shows the coefficients (a, b) of the exponentiation function that derive the relationship of the integrated value of retronasal aroma concentration (C) with respect to the respiratory rate (t) for the constituent fragrance compounds of Reference Product 2.

Each of the five components of each fragrance compound constituting Reference Product 2 was added to water to prepare a sample. The addition concentration was diluted in 1% to 10-fold increments to prepare in multiple stages. Evaluation was performed in order from a sample having a low concentration that could not be detected, and the addition concentration that could be detected when 10 ml was swallowed was defined as the threshold concentration. Initial amount considered as being released from the nostrils when the amount to be the threshold concentration, that is calculated Retoronezaru threshold concentration integrated value (C _T). Threshold concentration and Retoronezaru threshold concentration accumulated value of the configuration perfume compounds of Reference product 2 (C _T) are shown in Table 8.

Regard reference product 2, obtained by respiration and tenth respiratory th retro nasal aroma concentration accumulated value from the function shown in Table 7 was calculated (C _R), divided by Retoronezaru threshold concentration accumulated value (C _T) Table 9 shows the values of the degree of contribution to be made.

[Example 3]
The following tests were conducted to verify the effectiveness of the retronasal aroma contribution.
A basic blended flavor composition for coffee (reference product 3) was prepared based on a model blending formulation composed of a flavor compound contained in coffee. Table 10 shows the formulation and typical incense tone expressions of Reference Product 3.

For the 11 components having a high degree of fragrance contribution in each fragrance compound constituting the reference product 3, typical fragrance tone expressions indicating the quality of the fragrance are also described. Fragrance compounds other than the above 11 components are collectively shown as flavor base A.

[Reference example 1]
(Prediction of fragrance balance over time)
The basic blended aroma composition for coffee was adjusted, and the aroma balance of the first and tenth breaths, which was presumed to be felt by the subject after drinking water containing 0.1% of the aroma, was predicted. Here, it is assumed that the first breath is immediately after swallowing and the tenth breath is about 30 seconds after swallowing. Perfuming the respiration th and 10 breaths th retro nasal aroma concentration accumulated value that is expected to come out of the nose when drinking water (C _R) is derived from the power function and the addition amount of each fragrance compound .. Even more Retoronezaru threshold concentration integrated value _{(C T)} of each flavor compound was calculated Retoronezaru aroma contribution of _(C R / C _T). Table 11 shows the value of the retronasal aroma contribution of each fragrance compound and the value obtained by adding the numerical values for each fragrance tone.

(sensory evaluation)
A sensory evaluation was performed to clarify the relationship between the above prediction results and sensations.
Seven skilled panelists performed a sensory evaluation of the aroma after drinking water containing 0.1% of the above basic coffee flavor composition (reference product 3). The evaluation items were fermentation-like, butter-like, nut-like, roasted, raw beans-like, brown sugar-like, and smoky, and the strength of each item was evaluated on a 7-point scale. The evaluation criteria are shown below.

Evaluation criteria 6 points: Feel very strong 5 points: Feel strong 4 points: Feel slightly strong 3 points: Feel slightly weak 2 points: Feel weak 1 point: Feel very weak 0 points: Do not feel at all

The timing of evaluation was immediately after swallowing and 30 seconds later, and a method was adopted in which 0 to 6 points were entered on the prepared evaluation form. Table 12 shows the simple average values of the seven evaluators.

(Comparison between fragrance balance prediction and sensory evaluation)
Since the value of the retronasal aroma contribution degree of each incense tone shown in Table 11 has a wide range of numerical values, the value obtained by logarithmic processing was used. When the contribution prediction for each incense tone and the results of the sensory evaluation were compared, a high correlation was found in the scatter plot (Fig. 1) showing the relationship immediately after swallowing. A correlation was also found in the scatter plot (FIG. 2) showing the relationship after 30 seconds. From this, it was shown that the degree of contribution in the retronasal aroma obtained by this evaluation method is useful as a method for predicting the fragrance balance.

Claims (5)

It is a method to evaluate the contribution of flavor compounds that are felt after swallowing food and drink.
1) The threshold concentration of the aqueous solution is discharged from the mouth through the nose after swallowing and is discharged from the nose. 2) The food and drink is discharged from the mouth after swallowing through the nose through the nose. An evaluation method characterized in that the ratio of the concentration of the fragrance compound or the integrated value of the fragrance concentration is defined as the degree of contribution of the fragrance compound. The evaluation method according to claim 1, wherein the concentration of the fragrance compound or the integrated value of the fragrance concentration according to claim 1 is based on the result measured by a real-time analyzer. 2. The evaluation method according to claim 1, wherein 2) is an aroma concentration integrated value at each respiratory rate estimated by a power function that approximates the attenuation for each respiration. The evaluation method according to claim 1 to 3, wherein 1) according to claim 1 is an integrated value of the concentration or aroma concentration of the first breath. A method for evaluating the degree of contribution and evaluating the fragrance balance by the method according to claims 1 to 4.

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