KR950002773B1 - Method of extracting honey perfume - Google Patents

Abstract

The preparation method of honey flavor (I) consists of (1) heating honey at 42-50'C to water content 19% using a vacuum evaporator, (2) adsorbing (I) on activated carbon columns or (3) adsorbing (I) on U-shaped glass column jacketed in liquid nitrogen, (4) desorbing (I) from the columns by blowing nitrogen or helium gas at 40-60ml/min, (5) adding (I) to concentrated honey prepared in process (1).

Description

How to recover and re-add honey flavor components

1 is a graph of the weight of honey fragrance components that can be adsorbed on the unit weight of activated carbon.

2 is a graph of the relationship between moisture content and honey fragrance component loss rate.

3 is a view showing the adsorption process of the honey fragrance component according to the present invention.

The present invention relates to a method for recovering and re-injecting honey fragrance components, and more particularly, to recover the inherent fragrance of honey lost in a vacuum concentration process of lowering moisture content in order to improve the preservation of honey by using a selective adsorption method. The present invention relates to a method of improving the quality of honey by re-injection into the final concentrate.

Honey is obtained by collecting honey from flowers of various plants by bees and storing and ripening them in honeycombs. The honey obtained in this way has a unique fragrance according to the type of flower, and is favored not only as a health food but also in consumer preference. It is food to be received. However, the honey freshly collected by bees has a problem of low preservation because the moisture content is high and the possibility of destruction by microorganisms is high. Therefore, the preservation is improved by reducing the water content to about 19% by using a reduced pressure concentration method in order to increase the preservation.In this reduced pressure concentration method, the natural honey is preheated to about 50 ° C and then sent to a reduced pressure concentration tank. 700-740mmHg) The evaporated water and honey fragrance is discarded after condensation by heat exchanger. The content of the fragrance contained in such condensate was very low (about 60 ppm), so they could not be re-introduced into honey. Therefore, the present inventors have been studied for a long time to solve the above problems, a method of effectively collecting and re-injecting the water and the fragrance components contained in the condensate produced during the decompression concentration of the raw material honey and re-injected into the honey concentrate Was developed.

In the present invention, in view of the fact that the aquatic group in the volatile components produced during the vacuum concentration has a relatively large polarity, the fragrance component has a non-polar characteristic, the fragrance component using a material that selectively adsorbs only non-polar substances After adsorbing and concentrating, it was separated by heat desorption reaction and re-injected into the honey concentrate to develop a method of producing honey with a high aroma.

The method for recovering and re-adding the honey fragrance component according to the present invention comprises three steps of adsorption, desorption, and re-injection. The process first involves placing the raw honey in a vacuum concentrator, and then evacuating the vapor outlet and the vacuum of the concentrator. After installing the column filled with activated carbon between the pumps, adjust the temperature of the concentrator to around 42-50 ℃, maintain the pressure of the vacuum pump at about 700-740mmHg, concentrate it, and put the adsorption column into the heated heating jacket and inert While blowing the nitrogen gas or helium gas, which is a gas, and heating the temperature of the heating jacket to about 19 ° C., the fragrance is desorbed in an instant. Then, the inert gas is blown as a carrier gas to move the desorbed honey fragrance to vacuum. It is directly blown into the raw honey concentrate of the concentration tank or condensed in a U-shaped tube contained in liquid nitrogen and then inert as a mobile phase gas. By blowing move the honey flavor components will condense into the produced honey that holds the mixed honey sikimeuroseo unique fragrance raw honey concentrate.

Hereinafter, a method for recovering and re-adding a honey fragrance component according to the present invention will be described in detail by way of examples.

Example 1

(1) adsorption process; After weighing exactly 2.5 g of acacia raw material honey with a chemical balance, put it in a 50 ml round flask, install it in a Rotarap, a vacuum concentrator, and charge 0.4 g of activated carbon (18-35mesh, ASTM). Was connected between the outlet of the rotor and the vacuum pump.

After adjusting the temperature of hydrogen to 50 degreeC, the rotation speed of the round flask was adjusted to 50 times per minute, and the pressure gauge scale of the vacuum pump was adjusted so that it might be set to 740 mmHg. While concentrated for 10 minutes, the honey fragrance component disappeared in the increasing state during the concentration was selectively adsorbed on the activated carbon column. As a result of observing the moisture content of the honey concentrate, it was observed that the final moisture content is 20.0%.

In order to know the amount of the honey fragrance ingredient contained in the raw honey sample before condensation and the concentrated honey concentrate, the honey sample was purged with nitrogen gas for 2 minutes and then Yunacon, a purging & trapping device. After mounting on (UNACON), the fragrance components were analyzed by gas chromatography under the following analytical conditions.

* Injection bulb degree; 230 ° C. * gas flow rate; 20ml / min

Detector temperature; 250 ° C. * detector; Flame Ionization Detector (FID)

Mobile gas; Helium * initial temperature; 40 ℃

* Temperature program; 5 ° C./min * final temperature; 200 ℃

As a result of quantitative determination of the area of the detection peak in the chromatogram based on 4-methylthiazole as a standard, it was observed that 8,5943 μg and 5.5078 μg, respectively.

(2) desorption step; In order to recover the honey fragrance component bonded to the activated carbon column in the adsorption process, an adsorption column in which the honey fragrance component is adsorbed is put in a heated heating jacket and nitrogen gas, which is an inert gas, is blown into the adsorption column at a rate of 50 ml per minute. Simultaneously with the zooming, the temperature of the heating jacket was heated to 190 ° C. to desorption immediately.

As a result of measuring the amount of honey fragrance component separated by desorption by gas chromatography under the same analytical conditions as in the above adsorption process, it was observed that about 2.9270 μg of aerobic component was adsorbed and that the adsorption efficiency was about 94.8%. .

(3) re-insertion process; Nitrogen gas, which is an inert gas, was blown as a carrier gas and the desorbed honey fragrance component was transferred to the raw honey concentrate of the vacuum concentration tank and mixed. In order to measure the efficiency of re-injection of the recovered honey fragrance components into the honey concentrate, it was analyzed by quantitative analysis of the honey fragrance components of the final honey concentrate under the same analytical conditions as in the above adsorption process. It was found that this oil is oil-resistant, and the re-feeding efficiency of 89% was observed.

Example 2

(1) adsorption process; Accurately weigh about 2.5g of acacia honey with chemical balance and place it in a 50ml round flask, install in a vacuum concentrator Rotarap, and fill with 0.4g activated carbon (18-35mesh, ASTM). Was connected between the outlet of the rotor and the vacuum pump.

The temperature of the water bath was adjusted to 45 DEG C, the rotation speed of the round flask was adjusted to 55 times per minute, and the pressure gauge scale of the vacuum pump was adjusted to 720 mmHg. While concentrated for 15 minutes, the honey fragrance component disappeared in the vapor phase of the concentration was selectively adsorbed on the activated carbon column. As a result of observing the moisture content of the honey concentrate, it was observed that the final moisture content is 19.2%.

In order to know the amount of honey flavor components contained in the raw honey sample before concentration and the honey concentrate after concentration, the honey flavor components were analyzed by gas chromatography under the same analytical conditions as in Example (1). It was observed that 8.5943 μg and 5.1469 μg.

(2) desorption step; In order to recover the honey fragrance components bonded to the activated carbon column in the adsorption process, the adsorption column in which the honey fragrance components are adsorbed is put in a heated heating jacket and the inert gas Hellum gas is blown into the adsorption column at a rate of 50 ml per minute. At the same time, the temperature of the heating jacket was heated up to 190 ° C. and quickly desorbed.

As a result of measuring the amount of honey fragrance components separated by desorption by gas chromatography under the same analytical conditions as in the above adsorption process, it was observed that about 3.5120 μg of the fragrance components were adsorbed and that the adsorption efficiency was about 101.8%. It was.

(3) re-insertion process; The honey fragrance component obtained by desorption from the activated carbon column is condensed in a U-shaped tube contained in liquid nitrogen, and then blown with nitrogen gas as a carrier gas to transfer the condensed honey fragrance component. Mix with concentrate. 8.80 μg of fragrance components as a result of measuring the amount of honey fragrance components in the final honey concentrate by gas chromatography under the same analytical conditions as in Example 1 to determine the efficiency of re-injection of the recovered honey fragrance components into the honey concentrate. It was observed that it contained and there was 83% re-feed efficiency.

In the above embodiment, the amount of activated carbon used is the adsorption when the amount of activated carbon is packed into the column by dividing the amount of activated carbon into 10 steps from 0.04 g to 0.4 g in order to know the adsorption capacity of the honey fragrance component according to the amount of activated carbon used. As a result of measuring the amount of honey fragrance components, a standard graph as shown in FIG. 1 was obtained, and it was observed that the honey fragrance component adsorption capacity of 6.9 ± 0 57 μg per 1g of activated carbon was observed. Based on these results, the amount of activated carbon to be used was determined.

In addition to the embodiments described above, the inventors of the present invention, on the premise that the amount of adsorbent is sufficient, to find out how much the adsorption efficiency of activated carbon, i.e., the amount of honey fragrance components lost without being adsorbed by activated carbon, is reduced. The mass balance was calculated from the amount of honey fragrance components contained in, the amount of honey fragrance components remaining in the honey concentrate after concentration, and the amount of honey fragrance components adsorbed on activated carbon, which is a nonpolar adsorbent. The same result as 1 was obtained.

TABLE 1

As shown in Table 1, it has been observed that as the concentration time is longer, the efficiency of adsorbing the fragrance component on the activated carbon column is increased, and the average adsorption efficiency is 98 ± 15.6% (the adsorption efficiency exceeds 100%). In other words, the more adsorbed scents than the evaporated scents, the raw honey is analyzed by the Purge & Trapmethod method, and some of the scents are lost during the analysis. In this case, the adsorption efficiency is relatively high because there is less fragrance component lost by analyzing the adsorption column directly on the gas chromatography, and the adsorption efficiency is somewhat different due to the difference in the analysis method in both cases).

In addition, the fragrance loss when the water content was lowered to 19% at a pressure of 740 mmHg and a concentration temperature of 50 ° C. in the raw honey having an initial moisture of 21.2% was reduced to <100 × Figure 2 shows the relationship between water content> and water content. In other words, it can be seen that the higher the moisture content, the higher the loss loss.

In addition, the present inventors analyzed and compared the fragrance content of the raw honey and the commercial honey sample in order to examine the fragrance loss rate of the acacia honey in the market. The analytical method is to dilute 1g honey sample 100 times with ultrapure water, purge 5ml of diluent for 15 minutes and dry for 6 minutes, and measure the content of honey fragrance components by gas chromatography under the same analytical conditions as in Example 1). As a result, it was observed that about 32-62% of honey scent was lost in the commercially available honey.

The honey obtained through the process described in the above embodiment had about 40% higher content of honey fragrance than the commercially available honey, and sensory tests by five-point symbol scale method on 20 professional panelists (Sniff). As a result of examining the degree of preference by the test), it was confirmed that the product according to the present invention is superior quality to the existing product at the level of 95%.

Therefore, in the present invention, the honey fragrance component lost in the vacuum concentration process of the raw honey is adsorbed and re-desorbed using the activated carbon which is a nonpolar adsorbent, and efficiently re-introduced into the final honey concentrate to prepare honey retaining the original fragrance of the honey as it is. Could.

Claims (7)

The temperature of the vacuum concentrator equipped with a column filled with activated carbon as a non-polar adsorbent between the steam outlet and the vacuum pump is adjusted to around 42 ° C to 50 ° C, and the pressure of the vacuum pump is about 700 to 740 mmHg. And a step of separating and adsorbing the concentrate and a step of desorbing the honey fragrance component from the activated carbon to which the honey fragrance component is adsorbed. The method of claim 1, wherein the adsorption column in which the honey fragrance component is adsorbed is placed in a heated heating jacket, and the inert gas is blown, and at the same time, the temperature of the heating jacket is heated to 180 deg. C to 190 deg. Method for recovering honey fragrance components, characterized in that. The method for recovering honey fragrance component according to claim 2, wherein nitrogen gas is used as the inert gas. The method for recovering honey fragrance component according to claim 2, wherein helium gas is used as the inert gas. The method of claim 2, wherein the flow rate of the inert gas is 40 to 60 ml per minute. Characterized in that the honey fragrance component is moved by blowing nitrogen or helium gas into the honey fragrance component recovered in the honey vacuum concentration process, and the honey fragrance component thus transferred is directly added to the raw honey concentrate of the vacuum concentration tank and mixed. Re-injection of honey fragrance components. The honey fragrance component recovered in the honey vacuum concentration process is condensed in the U-shaped liver contained in liquefied nitrogen (llquid nltrogen), and then moved by blowing nitrogen or helium gas into the condensed honey fragrance component, and thus moved. The condensed honey fragrance component of the re-feeding method of the honey fragrance component, characterized in that by mixing the raw material concentrated honey concentrate in a vacuum concentration tank.