KR100463381B1 - shikonin contain pigment constituent extract method from a lithospermum erythrorizon - Google Patents

Abstract

The present invention relates to a method for extracting pigment components containing siconin from the ground, the present invention is milled and kneaded wheat, fermented for 3 weeks at 32 ℃-38 ℃ and dried to produce yeast, and barley, The yeast and cooked barley were mixed 1: 7 and fermented at 32 ° C.-38 ° C. and 60% relative humidity for 2 days to prepare granules. The fermented granules and water were mixed at 1: 5 for 10-15 days. Preparing dried rice flour, and using the distilled stock solution having an alcohol content of 65% to 75% by distilling the fermented rice flour as an extraction material, adding dry grass and the extraction material to a tank to which a stirrer is attached; Extracting the pigment component of the grass by operating the rotational speed of the stirring tank in which the grass and the extraction material were added at 130 RPM, extracting the pigment component by stirring for 12-15 hours under the conditions of 40 ℃-45 ℃; It is composed of the step of adding 0.15%-0.25% citric acid to the herbal extract obtained in the pigment component extraction step. According to the present invention, it is possible to maximize the extraction of pigment components containing siconin from the ground, and to prepare an extract in which the pigment of the extract can be stabilized unchanged even after light or storage. The effect of easily producing red wine having an alcohol content is provided.

Description

Shikonin contain pigment constituent extract method from a lithospermum erythrorizon}

The present invention relates to a method for extracting a pigment component containing siconin from the ground, and more particularly, to a method for extracting a pigment component which can maximize the extraction yield when extracting a pigment containing siconin from the ground.

In general, lipospermum erythorhizon Shiebold et. It is a representative plant.

Such siconin derivatives are already used in prescriptions for anti-inflammatory, detoxification and antipyretic purposes. They have bactericidal and anti-inflammatory properties and are used externally as ointments for swelling, burns, frostbite, eczema and hemorrhoids. It is used for the promotion and prevention of constipation. It is also used as a natural colorant and is used to make red wine of red wine by eluting it with grain alcohol during the manufacture of Hongju, a traditional liquor of Jindo province, Jeollanam-do.

Various methods for producing red wine, as described above, using components of the grass having the above characteristics are also introduced. That is, since the pigment of the grass containing siconin is fat-soluble, the method of extracting the pigment component from the grass with alcohol solvent using the property of eluting reddish purple at the alcohol content of 40% or more.

Representatively, the primary method of eluting the pigment by flowing a solvent with an alcohol content of 40% or more to the surface layer of the ground, and the method of distilling the ground again by putting the extract in a tank to correct the pigment of the eluted extract and secondary extraction will be.

However, this method of extracting the pigment of the grass according to the prior art, it was difficult to extract the entire amount of the pigment present in the ground skin because it was not able to grasp the elution characteristics of the pigment, non-hygienic, such as using the grass once extracted once again There was a problem.

In addition, as described above, since the pigment of the ground was eluted by a solvent having an alcohol content of 40% or more, it was difficult to prepare a red wine having an alcohol content of 40% or less. In order to prepare a proper amount of water added to the alcohol content of more than 40% Hongju, in this case, there was a problem that the red-red color unique to Hongju due to the increase in the water content is changed to yellow. Particularly, when water is added, most of the lipoproteins eluted and the fat-soluble substances produced during the distillation due to the lower alcohol content become suspended and cause the problem of losing the transparency of the red wine.

The present invention was invented to solve the problems of the prior art as described above, the technical problem of the present invention can maximize the extraction of pigment components containing siconin from the ground, can stabilize the pigment of the extracted extract solution And, to provide a lipo pigment extract manufacturing method that can be produced red wine having a low alcohol content and various alcohol content.

1 is a graph showing the siconin content and the pigment extraction yield when weed extraction in alcohol content 10-90V / W% solution.

2 is a chromatogram of 50 ppm of standard foam for quantifying siconin

Figure 3 is a graph showing the spectrum by the initial vitamin seed addition of lichen extract according to the present invention.

Figure 4 is a graph showing a change pattern by the addition of vitamin seed during storage of the extract of the present invention.

Figure 5 is a graph showing the spectrum by the addition of the initial citric acid of the lichen extract according to the present invention.

Figure 6 is a graph showing a change pattern by the addition of citric acid during storage of lichen extract according to the present invention.

7 is a schematic process diagram for explaining the present invention.

The present invention for solving the above technical problem is a step of adding dry extract obtained by the grain and the alcohol content is 65%-75% after putting dry grass into a stirring tank equipped with a stirrer; Extracting the pigment component of the grass by operating the stirring speed of the stirring tank in which the grass and the extraction material were added at 130 RPM, extracting the pigment component by stirring for 12-15 hours under the conditions of 40 ℃-45 ℃; In order to stabilize the pigment of the extract of the pigment component obtained in the pigment component extraction step, adding citric acid to the extract 0.15%-0.25% and then filtering using a 0.7-1.0 ㎛ filter medium Provided are a method for extracting a pigment component containing nin.

At this time, the extraction material was pulverized into 30-40 mesh to kneading the water content of 5% by weight to 8% by weight, then molded into a diameter of 15cm, thickness 5cm and fermented for 3 weeks at 32 ℃-38 ℃ and dried at room temperature To make yeast, and the washed barley was immersed in purified water for 1-3 hours and then cooled to prepare cooked barley, and the yeast and the cooked barley were mixed 1: 7, and then 32 ℃-38 ℃, relative Fermented granules were prepared by fermentation at 60% humidity for 2 days to prepare granules, and fermented granules and water were fermented for 10 to 15 days by mixing 1: 5. It features.

According to the present invention, it is possible to maximize the extraction of pigment components containing siconin from the ground based on data obtained through several trials and errors. That is, by extracting the extraction material with an alcohol content of 65% to 75% or more and extracting it with a stirrer, it is possible to maximize the extraction of the pigment component, and to stabilize the pigment of the extracted extract with citric acid, using these extracts Hongju can be prepared.

Referring to the preferred embodiment of the present invention based on the accompanying drawings as follows.

First, in order to extract the pigment component from the ground, an extraction material having an alcohol content of 65% or more is prepared.

The extraction material is pulverized into 30-40 mesh to add water, kneading, kneading so that the moisture content is approximately 5% to 8% by weight and is molded into a diameter of 15cm and a thickness of 5cm.

The dough thus formed is fermented at 32 ° C.-38 ° C. for 3 weeks, and then dried at room temperature to produce yeast.

Subsequently, the barley is washed with water, immersed in purified water for 1 to 3 hours, and then steamed. The cooked barley is cooled to prepare steamed barley.

The yeast and the barley prepared as described above was mixed at 1: 7, and then fermented at 32 ° C.-38 ° C. and 60% relative humidity for 2 days to prepare granules, and the fermented granules and water were mixed at 1: 5. Fermentation is prepared for 10 to 15 days.

Subsequently, the fermented rice flour is distilled by a single distillation, and at this time, the distillation stock solution of the initial distillation is collected and used as a solvent for extracting the ground pigment. The alcohol content (alcohol frequency) of the initial distillation stock solution is approximately 65%-75%.

In this embodiment, the extraction material is manufactured using grains such as wheat and barley as described above, but industrial alcohols and spirits may be used. However, since the value of the extract or the value of the red sake to be prepared with the extract is lowered, it is preferable to prepare with grains.

When the extraction material is obtained by this process, the dry grass is placed in a tank with an agitator and the extraction material is added. At this time, the ratio of the extraction material and dry grass shall be 3-5.5: 1 (V / W%).

When the extractant and the dry grass is added to the stirrer, the pigment component is extracted by stirring for 12-15 hours under the conditions of 40 ℃-45 ℃.

Hereinafter, the effects of the mixing ratio of the extractant and the dry grass and the alcohol content of the extractant on the extraction of the pigment component and the effects of the temperature and the extraction time on the extraction of the pigment component through the test will be described in more detail. .

First, the method was performed to determine the optimum ratio of the content of the extractant to the dry grass to prepare a high concentration of the pigment extract by adding an excess of the grass to the extraction material (65 ~ 75% alcohol content) as follows. .

The extracting material: prepared by the dry ground content of 3: 1, 4: 1, 5: 1 (V / W%) and extracted with stirring for 12-15 hours under conditions of 35 ℃-45 ℃ at 130RPM, 70 Diluted 10 times in% ethanol solution and the changes in extraction yield, sikonin content and chromaticity are shown in Table 1.

The chromaticity measurement was repeated three times with a color difference meter (JS555, colo techno system co, LTD). The measured values were expressed as L value (Lightness), a value (red / green), and b value (yellow / blue) which are Hunter color values.

TABLE 1

White wine: Grassland content (V / W%) Extraction yield (%) Siconin Content (ppm) Chromaticity L value a value b value 3.5: 1 32.4 610.4 68.24 48.20 11.74 4.5: 1 28.6 583 71.91 39.03 15.09 5.5: 1 23.8 438 77.38 32.41 19.21

As shown in Table 1, it was difficult to extract because it was not completely deposited on the extract when the ratio was less than 3.5: 1, and elution of 5.5: 1 or more was diluted with the meaning of high concentration pigment elution. When comparing the eggplants, the extraction ratio was found to be the most suitable at a ratio of 4.5: 1 (V / W%).

In addition, the change in chromaticity is the tradition that the chromaticity of the law of average L value (70 ~ 58), a value (50 ~ 30), and b value (20 ~ 10) is currently marketed as a result of measuring the chromaticity value of Jindo Hongju coming out of the current product. As the chromaticity of the Hongju, all three were appropriate.

On the other hand, Figure 1 of the accompanying drawings shows the results of measuring the sikonin content of the extract extracted by the process as described above using high performance liquid chromatography (HPLC). That is, it shows the sikonin content and pigment extraction yield analysis results in the grass using alcohol.

As shown in Fig. 1, almost no colorant elution was observed in the alcohol content of 10% to 30%, and the content of siconin was less than 5ppm, which did not show the red color and light yellow color.

In particular, the extraction yield was the highest in the alcohol solution of 70% content and the sikonin content increased with higher concentration. In view of these characteristics, it was determined that the complete dissolution of the lichen pigment should be extracted for a long time in an alcohol solution containing more than 70%.

On the other hand, the analysis conditions of high performance liquid chromatography to quantify the sikonin in the above test is shown in Table 2 below.

TABLE 2

Instrument Injector; AT 3000, Futecs Pump; NS 2001P Colum μ Bondapak C18 (8mm × 10cm) solvent system CH 3 CN-H 2 O- (C 2 H 5) 3 N-AcOH (70: 30: 0.3: 0.3, v / v) Flow rate 1.5ml / min Detector UV, NS 2100S, 520nm

In addition, the chromatogram shown when 20ppm injection of 50ppm standard foam is shown in FIG.

As confirmed, the standard foam for each concentration was analyzed to prepare a calibration curve, and then a sample was injected to calculate the sikonin content of the lichen extract for each alcohol concentration.

On the other hand, the extraction characteristics test according to the extraction time was added to 500ml of the alcohol solution (the extraction solution) of 70% content in 5 g of Guernsey, irradiated for only 12 hours at 130PRM and the results extracted up to 48 hours are shown in Table 3.

TABLE 3

Analysis item 1 hour later 12 hours later 24 hours later 36 hours later 48 hours later Extraction yield (%) 1.4 18.7 19.2 19.4 19.5 Siconin Content (ppm) 2.4 35.4 36.1 36.4 36.5

As confirmed in Table 3, the relationship between the extraction time and the extraction yield did not change significantly after 12 hours, and as the time was invested, the dissolution of the pigment was not so large that the dissolution of the pigment was 12 to 15 hours. .

In addition, in order to measure the relationship between the extraction temperature and the extraction yield and the sikonin content, 500 ml of 70% alcohol solution was added to 5 g of Guernsey and extracted at 130 ° C. at 25 ° C., 40 ° C., and 50 ° C. for 12 hours. Extraction yield and siconin content by solid content by these tests were shown in Table 4 below.

TABLE 4

Analysis item 25 ℃ 40 ℃ 50 ℃ Extraction yield (%) 18.4 21.8 24.3 Siconin (ppm) 35.2 35.7 35.6

As shown in Table 4, the extraction yield of the pigment increased most at 55 ° C, but the change in siconin content was not so large that the dissolution of the water-soluble component inside the epidermis was greater than that of the pigment, thus extracting near 40 ° C-45 ° C. It was found that the method was the most suitable extraction temperature.

As confirmed above, the mixing ratio of the extraction material and the grass was 4.5: 1 (V / W%), and the alcohol content of the extraction material was 65%-75%, and the alcohol content was 65 ~. It is expected to extract the optimal extraction yield and siconin content when extracting 12-15 hours under 40 ℃ -45 ℃ at 130RPM in 75% of extraction material.

On the other hand, in order to stabilize the pigment of the herbal extract obtained by the above process, citric acid is added 0.15%-0.25% (V / W%) to the herbal extract. In this way, the addition of citric acid stabilizes the pigment of the extract, it is possible to minimize the changes under light conditions.

In order to explain this in more detail below, citric acid, which is an acidulant for stabilizing pigments, and the effect of acidulants other than citric acid on the extract will be described in detail.

Diluted licorice extract 10 times with 70% ethanol solution, and 0.05%, 0.1%, 0.15% and citric acid 0.1%, 0.2%, 0.3 Percentages were added in weight percent to volume, respectively, to determine the pattern of change in the claimed spectra under conditions of 25 ° C, 2,500 Lux incandescent lights, and in the dark without light sources.

First, Figures 3 and 4 in the accompanying drawings shows the change in the spectrum of the initial state of the vitamin C added to the seed extract and the spectrum during storage, Table 5 shows the measurement results.

As shown in FIG. 3, the change in chromaticity at the time of initial storage is not large, but the change in chromaticity during storage is visible in the visible light main absorption bands varying from 680 to 800 mm after 80 hours, and the pattern changes to dark purple. Therefore, the addition of vitamin seed was judged to have a rather adverse effect on the pigment stability of the herbaceous extract.

TABLE 5

Save time processing content After dispensing Storage after 80 hours Control Vitamin Seed 0.05% Vitamin Seed 0.1% Vitamin Seed 0.15% Control Vitamin Seed 0.05% Vitamin Seed 0.1% Vitamin Seed 0.15% L value 82.807 79.639 77.819 76.461 83.219 77.57 69.844 68.878 a value 33.993 32.821 32.89 32.763 23.835 25.497 27.327 27.344 b value 10.385 5.921 4.092 2.861 12.098 5.883 -0.339 -2.658

In addition, the measurement results for the stability of the lichen extract upon the addition of citric acid are shown in Figures 5 and 6, are shown in Table 6.

TABLE 6

Save time processing content After dispensing Storage after 80 hours Control Citric Acid0.1% Citric Acid0.2% Citric Acid0.3% Control Citric Acid0.1% Citric Acid0.2% Citric Acid0.3% L value 82.807 82.685 82.807 81.775 83.219 81.709 82.846 84.433 a value 33.993 34.156 34.163 33.623 23.835 27.383 27.203 27.45 b value 10.385 9.271 10.188 10.097 12.098 12.144 11.969 12.156

As shown in FIGS. 5 and 6 or Table 6, the visible light main absorption band is 540-580 mm, which has a characteristic of showing brighter red color than the herb extract control, and stabilizes the pigment in a state in which there is no change in light (light). It can be seen that.

The change in chromaticity also increases a value toward red when stored, and b value of yellow increases to give vivid red color.

Therefore, the addition of 0.15%-0.25% citric acid to the lichen extract can enhance the stability of the pigment, it is possible to minimize the changes under the light conditions.

On the other hand, after adding citric acid to stabilize the pigment of the extract as described above, the extract is filtered using a filter body. At this time, it is preferable to use the filter medium which has an eye of 0.7-1.0 micrometer. The extract passed through the filter medium is obtained as the final material.

In this way, while extracting a mixture of dry grass with an alcohol content of 65% -75% extract while stirring, extract the pigment component containing the siconin for 40-45 ℃, 12-15 hours, and the citric acid in the extracted extract 0.15% Stabilize the pigment by adding 0.25% and then filter it to maximize the extraction of pigment components containing siconin from the ground, and extracts whose pigments do not change or the changes are minimized even when the extract is exposed to light. Could get

According to the method for extracting a pigment component containing siconin from the ground according to the present invention, it is possible to maximize the extraction of the pigment component containing siconin from the ground, and the pigment of the extract can be stabilized unchanged even after light or storage. Not only can the extract be prepared, but the effect of using the extract is that it can be easily produced with a low alcohol water, that is, having a variety of alcohol content.

Claims (2)

Adding a dry grass to the stirring tank to which the stirrer is attached, and then adding the extraction material obtained by the grain and having an alcohol content of 65% to 75%; Extracting the pigment component by operating the stirrer and the stirrer to which the grass and the extractant were added at 130 RPM for 12 to 15 hours under the conditions of 40 ° C.-45 ° C. to extract the pigment component; Adding stabilized citric acid (0.15%-0.25%) to the extract to stabilize the pigment of the extract obtained in the pigment component extracting step, and then filtration using a 0.7-1.0 μm filter medium; Pigment component extraction method containing siconin from the grass, characterized in that it comprises a. According to claim 1, The extracting material is milled by adding water, kneading the mill and then molded to a predetermined size and then fermented for 3 weeks at 32 ℃-38 ℃ and dried at room temperature to produce a leaven, Washed barley is immersed in purified water for 1 to 3 hours and then cooled to prepare cooked barley, The yeast and steamed barley are mixed 1: 7, and then fermented at 32 ° C.-38 ° C. and 60% relative humidity for 2 days to prepare granules. Fermented granules and water were fermented for 10 to 15 days in a mixture of 1: 5 to prepare drunk, A method for extracting pigment components containing siconin from the ground, comprising a distilled stock solution obtained by distilling the fermented rice flour with a distiller.