JPS6018760A - Discrimination of young liquor and urn aged one of millet brandy (awamori) - Google Patents

Abstract

PURPOSE:To make it possible to accurately discriminate young liquor and urn aged one of millet brandy (AWAMORI) by utilizing such a fact that the association degree of the urn aged liquor is larger than that of the young one, by measuring the association degree of water and alcohol by using a differential scanning calorimeter. CONSTITUTION:A definite amount of a millet brandy (AWAMORI) specimen is conc. under vacuum while special grade liquor is added to the conc. specimen so as to adjust the alcohol conc. thereof to 60% and deionized water is subsequently added to the specimen mixture to bring the same to a constant volume. In the next step, the conditioned specimen is rapidly cooled to -160 deg.C by liquid N2 to be frozen and a thermogram is measured at a temp. rising speed of 10 deg.C/min in a range from -160 deg.C to +10 deg.C. In the thermogram, a frozen aqueous alcohol solution peak 5 in the vicinity of -100 deg.C, an endothermic peak 4 in the vicinity of -65 deg.C, a peak 3 wherein alcohol and water shift to high temp. -low temp. and together melted appear in a range of -56--60 deg.C and the recrystallization peak 2 of water appears in a range of -51--54 deg.C while the melting exothermic peak 1 of water appears at last. The shift degree due to the association of water and alcohol is different in young liquor and aged one. Hereupon, the discrimination of both of them can be accurately discriminated with accuracy not inferior to the sensory test of an expert by using a peak transfer peak shown by the drawing as an index.

Description

[Detailed Description of the Invention] As a result of conducting research on the aging of awamori from the physicochemical side, the present invention discovered that there is a difference in the degree of association between water and alcohol between new awamori sake and old sake aged by turtles. The purpose is to provide a method for distinguishing between the two using this.

When awamori is aged for a long period of time, it acquires a rounder taste, a pleasant texture, and a rich aroma, and has been prized and prized since ancient times as koosu (old sake), and was used to entertain wealthy guests.

Generally, awamori that has been distilled for less than a year is sold as new sake, and awamori that has been aged for more than three years is sold as old sake. However, some consumers have raised questions about the distinction between the two, such as whether the aged sake they have purchased does not seem to be good after drinking it, or whether there is a way to check if there is a difference between new and old sake. These issues are also being raised by the Fair Trade Commission, or the awamori industry has not been able to provide sufficient answers to this situation, and the method for distinguishing between new and old sake has not yet been resolved. Establishment has long been a dream of those involved.

The inventors of the present invention have conducted extensive research and development to solve this problem, and have discovered that when awamori is aged in a turtle, the association of water and spirit progresses, leading to the completion of the present invention.

Research on the aging of distilled spirits has mainly focused on elucidating the trace components related to their flavor, and there seem to be very few studies focusing on water and spirit, which are the main components of group 'a', but there are still some studies. There are valuable reports. For example, NA
KAMURA has reported that as alcoholic aqueous solutions are stored and aged, the degree of light scattering polarization decreases and the lumen vector changes (SOl.

Rep, TOhOku Univ, 1,35.200
(1952)).

On the other hand, Akahoshi shows that during the aging of distilled spirits and aqueous alcohol solutions stored in barrels, the formation of aggregates between water molecules and alcohol molecules progresses and the dielectric constant decreases. (Journal of the Japanese Society of Agricultural Chemistry, 3'7
, (8), 443 (1q63).

In addition, there are studies using NMR (1981 Japanese Society of Agricultural Chemistry Lecture Abstracts, p. 495).

The present inventors used DSO to investigate how non-volatile components, mainly metal components, eluted during awamori aging affect the alcoholic spirit-water interaction, and how they relate to sensory perception. There is no other example of research from the physicochemical side of aged sake stored in turtles.It was discovered that the association between water and alcohol progresses with storage, and by measuring the degree of association, new and old teeth were investigated. This is the first time in the 500-year long history of awamori that a method for determining the difference has been found, and its practical application is thought to be significant for the awamori industry.

When awamori is aged 5.2 times in a turtle, the interaction between water and alcohol is promoted, and as a result, the amount of water and sake lees that melt individually decreases, and the amount of water-alcohol melt increases. This is thought to be due to non-volatile components, mainly metal salts, which increase during the aging of awamori, or to promoting the association between alcoholic spirit and water.

Figure 1 shows the degree of association between water and alcohol measured for awamori new sake and Kame-aged old sake. Thermogram A shows the melting process of new sake and Kekame-aged old sake. A total of five absorption/exothermic peaks were observed. An exothermic peak (beak 5) due to recrystallization of the frozen sake lees aqueous solution appears at around -100°C, and then an endothermic peak (beak 4) mainly due to melting of alcoholic spirit appears around -65°C. Beak 3 is thought to be the result of alcoholic spirit and water, which were strongly influenced by each other, shifting from high to low temperatures and melting together, and is found at -56°C to -60°C.

Next, an exothermic peak (beak 2) of water recrystallization appears at -51°C to -54°C, and finally an endothermic peak (beak 1) of water melting appears at around -40°C.

The first surface pressure shows the calorific value of beak 1 to beak 5 of new sake and old sake.

Table 1 Calorific value of each beak New sake Old sake Beak 1 41.5 mcal/V 14. Omm/f Peak 2 6.5 8.0 Peak 3 10.5 30.0 Peak 4 56.5 50.0 Peak 5 36.0 32.5 Shifts to Beak 1.4 or Beak 3 during ripening Using 9go as the beak transfer rate, which is an indicator of the alcoholic spirit-water interaction in awamori, the values for new sake and old sake are 9, respectively, using the following formula.
．． 7 and 31.9 clearly show the difference between the two.

+ [Calorific value of Beak 4] From this, it was found that it is possible to distinguish between new sake and Kame-aged old sake by using the peak shift rate of the measured thermogram as an index.

Next, DS for 12 new sake items and 10 turtle aged old sake items.
The results of measuring the degree of water-alcohol association by O measurement are shown as examples.

Example (Pretreatment of 11 samples) Take 20 samples of each sample into test tubes, concentrate under reduced pressure using a four-tally evaporator, add 1.2 ml of ethanol (special grade 99.51) to give an alcohol concentration of 601, and deionize. The volume was made up to 2 ml with water.

(2) Using a DSO meter made by DSO Usouri Denki Co., Ltd., first, 20 μt of the sample was placed in a small aluminum container and rapidly heated to -160°C using liquid nitrogen (using 15~b da as a control, -160°C to +10℃
Heat change song 1i as awamori melts by increasing the temperature at a rate of 10℃ per minute! ; [(thermogram) was measured.

(3) Sensory test The venue is Okinawa National Tax Office Appraiser's Office. There were five judges: a rustic official and a manufacturing brewer.

In the judging process, three items each with the characteristics of Kamame-aged old sake and three items with the characteristics of new sake were lined up, and the judges asked them in advance to determine the score. The 20% diluted product was evaluated on the following scale.

(4) Measurement Results Figure 2 shows the peak shift rates obtained as a result of DSC measurements of 12 new sakes and 10 turtle-aged old sakes.

The peak transition rate for new sake is 7% to 15%, and for old sake it is 24%.
There was a clear difference between the two, and it was found that the water and spirit of old sake were in a more advanced state than new sake.

FIG. 3 shows the relationship between the age of aging and the peak shift rate obtained by performing DSC measurements on aged sake that has been stored for 3 to 13 years.

The peak transition rate increases as it ages, and the peak transition rate Ir! i return formula is Y-0,37
It is given by X −5,09.

(However, Y: Age of aging, X: Peak transition rate.) The correlation coefficient r between the two is 0.754, which is significant at a risk rate of 2. In addition, in order to check the regression equation, we performed a new DSC measurement on four old sakes with a certain age, and found that they were almost on the regression line.

FIG. 4 and FIG. 5 show test results of peak transfer rate and sensory value.

Various factors are involved in the level of sensory ripeness, and the degree of association between water and spirit is considered to be one of them.

We do not know how much this contributes to the level of sensual ripeness, and there are few reports linking factors related to ripening to sensuality.

As shown in Figure 4, the peak shift rate is higher for awamori that has the aroma of turtle-aged old sake than for awamori that has the aroma of new sake. The correlation coefficient T between the two is 0902, and the risk rate is 1.
It is significant in both cases.

(5) Relationship between peak shift rate and taste As shown in Figure 5, taste is also closely related to peak shift rate. That is, the rounder the awamori, the higher the peak shift rate compared to the rougher awamori. The correlation coefficient r between the two is α858, which is significant at a criticality rate of 1.

As mentioned above, it is easy to judge whether it belongs to new sake or old turtle-aged sake by using the peak shift rate of the thermogram obtained by measuring the degree of association between water and spirit as an indicator. became clear.

Furthermore, regarding turtle-aged aged sake with different ages, D.
As a result of measuring the SO and examining the consistency between the age of maturity calculated from the regression equation and the actual age of maturity, it was found that there is a correlation between the two, so the present invention can also be used as a method for estimating the age of turtle maturity. I understand.

[Brief explanation of drawings]

Figure 1 is a thermogram of new sake and Kame-aged old sake.
In the figure, A indicates new sake and B indicates old sake. Figure 2 shows the DSO peak migration rates of new and aged sake, where ○ indicates aged sake and . indicates new sake. Figure 3 shows the relationship between the age of aged sake and the DSO peak transfer rate, where ◯ indicates a sample for the regression equation, and ◯ indicates a check sample. Figure 4 shows the relationship between the DSC peak shift rate and the sensory value (aroma), and Figure 5 shows the relationship between the DSC peak shift rate and the sensory value (taste), where ○ indicates old sake, and 0 indicates new sake. People Patent Attorney Shun Tatsuyama - Fig. 1 wr row (“Keeping the fusion angle of old sake - Seven Guuu, Mu, Fig. 2 ○ Old sake - Toshikaban type (?) J$1 Jhongdan (middle)

Claims (1)

[Claims] A differential scanning calorimeter (
A method for distinguishing between new awamori sake and turtle-aged old sake, characterized in that the peak shift rate of a thermogram obtained by measuring the association degree of water 7 and alcohol using DSC) is used as an index.