KR102305182B1 - Method of preparing black platycodon concentrate enhanced saponin contents, platycodon extract and liquid stick comprising the same - Google Patents

Abstract

The present invention relates to a method for producing black bellflower in which the content of saponin, such as Platicodin, is remarkably increased through a number of times of steaming, aging and drying processes with a natural plant fermented fermented and dried bellflower, and a black bellflower extract including the same. And it relates to a liquid stick manufacturing method.
In the present invention, the content of absorbable saponin metabolites (saponin metabolites, saponin intermediate metabolites, specific saponins) is increased through immersion and penetration using natural plant fermented fermented liquid, steam steaming, hot air drying, maturation and low temperature drying steps. It is significantly higher than dried bellflower, significantly lowers the content of harmful substances (residual pesticides, heavy metals and benzopyrene, etc.) can

Description

Method of preparing black bellflower complex concentrate with increased saponin content and liquid stick manufacturing method including the same

The present invention relates to a method for producing black bellflower having an increased saponin content, and a method for producing a black bellflower extract and a liquid stick including the same, and more particularly, to a natural plant fermented fermented and matured bellflower, the process of steaming, aging, and It relates to a method for producing black bellflower in which the content of saponin, such as platicodin, which is a saponin component, significantly increased through a drying process, and a method for producing a black bellflower extract and liquid stick including the same.

Bellflower (Platycodi Radix) is a dicotyledonous perennial plant that grows widely in Korea, China, and Japan. Its roots are collected in spring and autumn, dried in sunlight, and the skins are peeled off or dried to be used for food or medicine. The roots are thick and fleshy. It is fleshy, and the stem grows straight and when cut, a white sap comes out.

In Korea, it was mainly used for food, but its cultivation area is expanding as the consumption for not only food but also for medicinal purposes is increasing in recognition of its pharmacological components and pharmacological functions.

Bellflower is an alkaline food rich in fiber and rich in calcium and iron, and contains triterpenoid-based saponin as its main pharmacological ingredient.

The saponins contained in bellflower are platycodin A, C, D, D2, D3, platycodigenic acid A1~A5, which uses platycodigenin as an aglycone. , C, polygalacin D, D2, polygalacic acid, platycodigenic, etc., accounting for about 2% of the roots.

The taste of bellflower is spicy and bitter, and the nature is flat. It works on the lungs to stop coughing and remove phlegm.

In oriental medicine, it has excellent antitussive, expectorant, analgesic and anti-inflammatory properties, and is widely used as an antitussive and expectorant for cough and bronchitis.

Bellflower stimulates gastric mucosa and promotes bronchial secretion, thereby exhibiting expectorant action by significantly increasing mucus secretion. When Platicodin D is administered to the spinal cord, sensitivity to pain is significantly reduced, thereby exhibiting analgesic and anti-inflammatory action.

Other actions of bellflower include hypoglycemic action, peripheral vasodilation action, hemolysis action, anti-ulcer action and cholesterol content lowering action.

In addition, as a steroid-based compound, bellflower contains phytosterol, alpha-spinasterol, alpha-spinasterol glucoside, inulin, apiose, platyconin, etc. as pharmacological ingredients. It contains components such as betulin, which is a lupine triterpenoid.

However, despite the excellent pharmacological efficacy, bellflower has a unique flavor and taste, such as bitter taste, etc., which has lowered consumer preference, so various attempts are being made to develop various products so that it can be easily consumed.

However, in the process of removing the bitter taste, bitter taste, and off-flavor, most of the major physiologically active substances are destroyed or reduced, and water-soluble components are eluted, destroying the unique texture and shape of bellflower, making it difficult to develop products with excellent efficacy.

In addition, the saponin contained in bellflower is rapidly reduced through repeated heating and drying processes, and the inherent flavor is rapidly lost, so there is a problem in that the marketability is deteriorated.

The present invention is to provide a black bellflower and an extract thereof with a significantly increased content of saponin components.

The present invention is to provide a black bellflower with an increased steroid component and an extract thereof.

The present invention provides a pre-treatment step of (1) putting a bellflower in a steamer, steaming it with steam, and drying the steamed bellflower;

(2) immersing the pre-treated bellflower in natural plant fermented fermented liquid;

(3) spraying and infiltrating the fermented and aged natural fruit sugar pickle into the bellflower that has undergone the immersion process;

(4) putting the bellflower in a steamer and steaming;

(5) heating the bellflower, which has undergone the steaming step, with hot air;

(6) aging the bellflower that has undergone the heating process; and

(7) A method for producing black bellflower comprising the step of drying the bellflower that has undergone the aging step with cold air, wherein the method relates to a method for producing black bellflower in which the cycle of steps (2) to (7) is repeated several times.

The method for producing black bellflower of the present invention can dramatically increase the content of platycodin, a component of bellflower saponin, through nine steaming, aging and drying processes of dried bellflower using natural plant fermented fermented liquid. have.

In the present invention, the content of absorbable saponin metabolites (saponin metabolites, saponin intermediate metabolites, specific saponins) is increased through immersion and penetration using natural plant fermented fermented liquid, steam steaming, hot air drying, maturation and low temperature drying steps. It is significantly higher than dried bellflower, significantly lowers the content of harmful substances (residual pesticides, heavy metals, benzopyrene, etc.) can

1 shows a method for producing black bellflower of the present invention, FIG. 2 shows a bellflower saponin platicodin D peak, FIG. 3 is a bellflower steroid atroposide H peak, and FIGS. 4 and 5 are black bellflower of the present invention. Bellflower and extract manufacturing process, Figure 6 is an ultra-high pressure liquid chromatography used for the analysis of the black bellflower of the present invention.

Hereinafter, a preferred embodiment of the present invention will be described with reference to the drawings. However, the scope of the present invention is not limited to the description or drawings of the following embodiments. That is, the terms used herein are used only to describe specific embodiments, and are not intended to limit the present invention. The singular expression includes the plural expression unless the context clearly dictates otherwise. In addition, terms such as "comprises" or "have" described in this specification are intended to designate that the features, numbers, steps, operations, components, parts, or combinations thereof described in the specification exist, but one or the It should be understood that the existence or addition of the above other features or numbers, steps, operations, components, parts or combinations thereof is not precluded in advance.

1 shows a method for manufacturing black bellflower of the present invention. Referring to FIG. 1 , the method for producing black bellflower of the present invention includes a pretreatment step, a immersion step, an infiltration step, a steaming step, a heating step, an aging step, and a drying step.

In the method for producing black bellflower of the present invention, the cycle from the immersion step (including the penetration step, the steaming step, the heating step, and the aging step) to the drying step can be repeated several times, and preferably, the cycle is repeated two or more times or about 10 times, More preferably, it can be repeated 9 times.

The pre-treatment step (1) is a step of putting the bellflower in a steamer, steaming, and drying the steamed bellflower.

For example, in the pretreatment step (1), the bellflower root is put in a washing machine, washed with hot water at 40 to 60° C., put in a hot air dryer, and dried at 60 to 80° C., dried bellflower is put in a steamer and passed through steam and steaming at 100 to 110° C. for 6 to 8 hours, and placing the steamed bellflower in a steamer and drying in a cold air dehumidifying dryer with cold air at 10 to 20° C. for 12 to 24 hours.

The immersion step is a step of immersing the pre-treated bellflower in a natural plant fermented fermented liquid.

The immersion step is a step of immersing the pre-treated bellflower at 35-45° C. for 20-24 hours by adding a fermented and aged natural fruit sugar pickle.

Natural plant fermented sugar syrup contains 4 or more types selected from walhash (persimmon), plum, gold, fresh ginseng, garlic, and ginger, but contains walhash, plum, and gold as essential.

First, take 8~12kg of moonshine, 4~6kg of plum, golden, fresh ginseng, garlic, ginger, etc., add 25~35kg of unrefined sugar and mix evenly, then put it in a traditional pottery and seal it, and keep it out of direct sunlight. It can be fermented for more than 3 months in a cool, well-ventilated place.

After filtering the mixed fermented liquid of natural plants fermented at room temperature for 3 months with cotton, the filtrate is transferred to a storage tank and aged for 9 months while stirring once a day at 25-30 ° C. A mature liquid can be obtained.

The penetrating step is a step of injecting and infiltrating the fermented and aged natural fruit sugar pickle into the bellflower that has undergone the immersion process. More specifically, the penetrating step may be a step of spraying the fermented and aged natural fruit sugar pickled radish into the bellflower that has undergone the immersion process, and then infiltrating it at 35 to 45° C. for 10 to 12 hours.

The steaming step is a step of putting the bellflower in a steaming machine and steaming it with steam. More specifically, the (4) steaming step may be a step of putting the bellflower in a steaming machine and steaming it with steam at 100 to 110° C. for 4 to 6 hours.

The steaming step is a step of passing the bellflower with steam of 100 ~ 110 ℃, if the temperature range, the steam passing through is 14 ~ 20p.si, preferably 14.65 psi (100 ℃) ~ 20.76 psi (110 ℃) of pressure is required In the steaming step, if the temperature is lower than the temperature range, it is impossible to steam the bellflower, and if it is higher than the temperature, the active ingredient of the bellflower may be decomposed.

In the present invention, the bellflower that has undergone the steaming step is cooled while gradually lowering the temperature through the heating, ripening, and drying steps.

That is, in the warming step, the bellflower that has undergone the (4) steaming step is heated by passing hot air at 60 to 80° C. for 180 to 220 hours, and in the aging step, the bellflower that has undergone the heating process is placed in an incubator and 40 to 60° C. is aged for 90 to 110 hours, and in the drying step, the bellflower, which has undergone the aging step, is dried by passing cold air at 10 to 20° C. for 60 to 80 hours.

That is, in the method for producing black bellflower of the present invention, after heating the bellflower with steam at 100 to 110 ℃ in the steaming step, 180 to 220 hours (heating) at 60 to 80 ℃, 90 to 110 hours at 40 to 60 ℃ (aging) ), and cooled and dried at 10-20°C for 60-80 hours (drying).

In the present invention, heating, aging, and drying steps are performed while gradually lowering the temperature after the steaming step.

In the steaming step, after heating the bellflower with pressurized steam at 100~110℃, put it in a hot air dryer and go through the primary drying process at 60~80℃, then lower the temperature step by step and aged at 40~60℃ for a certain period of time, 10 The original shape of black bellflower can be maintained as it is by cooling it to ~20°C and drying it through cold air.

Unlike the present invention, when the steamed bellflower is quickly dried at a high temperature, the original shape of the black bellflower cannot be maintained and the shape may be distorted, as well as the saponin component may be decomposed.

The present invention repeats one cycle from the immersion step (including the permeation step, the steaming step, the warming step, and the aging step) to the drying step several times, more preferably 9 times (ie, excluding the pretreatment step, the steaming step is repeated 9 times) included) can be repeated.

In the present invention, the content of saponin is increased rapidly as the foaming process is increased through immersion, penetration, steaming, warming, aging, and drying steps repeated several times or 9 times. can If repeated 10 times or more, the saponin content does not increase any more, but rather decomposes.

In another aspect, the present invention provides a method for producing a black bellflower complex concentrate, including wild ginseng, red ginseng, deodeok, maekmundong, sambaekcho, and heating the black bellflower and purified water prepared above in an extraction container, filtering the solution in the extraction container, and Concentrating the filtrate into a vacuum concentrator.

For example, 10 to 30 kg of black bellflower, preferably 15 to 20 kg, is taken in an extraction container, and 1 to 6 kg of wild ginseng, preferably 2 to 4 kg, 6 to 15 kg of red ginseng, preferably 7 to 12 kg, 2 to 12 kg of deodeok. , preferably 4 to 8 kg, 4 to 24 kg of maekmundong, preferably 8 to 16 kg, and 4 to 24 kg of three hundred seconds, preferably 8 to 16 kg of purified water 60 to 240 kg, preferably 100 to 150 kg, and 90 to After heating at 100° C. for 4 to 6 hours, it can be filtered with cotton.

In addition, the filtered filtrate is placed in a vacuum concentrator and concentrated under reduced pressure at 65 to 75° C. for 4 to 6 hours to obtain a Gujeunggupo black bellflower complex concentrate (60 to 70 brix).

In addition, the present invention is a step of preparing a complex viscous liquid formulation of black bellflower by mixing the previously prepared complex concentrate with Sukhumidus concentrate, ginseng powder, bokryeong powder, antler powder, maca powder, acid medicine powder and honey, the black bellflower complex dot It relates to a method for manufacturing a black bellflower liquid stick, which includes the step of filling and sealing the composition liquid formulation to a stick using an automatic filling machine while heating it to 60-80°C.

The method of the present invention is to take 5-15 kg of black bellflower complex concentrate from Gujeung-gupo and put it in a preparation tank, 5 to 15 kg of Sukhumang concentrate, 5 to 15 kg of ginseng powder, 5 to 12 kg of bokryeong powder, 1 to 5 kg of antler powder, 1 to 4 kg of maca powder, After mixing 1-5 kg of acid medicine powder and 50-60 kg of honey, it is heated at 60-80°C for 2-4 hours to prepare a complex viscous liquid formulation.

The prepared black bellflower complex viscous liquid formulation can be filled and sealed in a polyethylene liquid stick by 10 to 12 g using an automatic filling machine while maintaining a temperature of 60 to 80 ° C.

Hereinafter, the present invention will be described in more detail through examples, but the present invention is not limited to these examples.

Example 1

1. Preparation of natural plant fermented sugar syrup

First, take 8-12 kg of wolhashi, 4-6 kg of plum, golden, fresh ginseng, garlic, ginger, etc., add 25-35 kg of unrefined sugar, mix evenly, and ferment at room temperature for 3 months. After filtering the mixed fermented solution of natural plants fermented at room temperature for 3 months with cotton, the filtrate was transferred to a storage tank and aged for 9 months while stirring once a day at 25-30° C. for 30 minutes, and then filtered with cotton.

2. Bellflower pretreatment

Take 20~24kg of bellflower root, put it in a washing machine, wash it 3 times with warm water at 40~60℃, put it in a hot air dryer, and dry it at 60~80℃ for 4~6 hours. The dried bellflower was put in a steamer and passed through steam at 100~110℃ for 6~8 hours. Put the steamed bellflower in a steamer, put it in a cold-air dehumidifying dryer, and then dry it with cold air at 10-20°C for 12-24 hours.

3. Immersion and spraying of natural plant sugar fermented liquid

500 g each of the pretreated bellflower was taken on 12 bed plates, 400-600 mL of natural plant sugar fermented fermentation solution was added, and then immersed at 35-45° C. for 20-24 hours. After immersion, 200~300mL of natural plant fermented sugar pickled liquid was evenly sprayed, and then the process of infiltration at 35~45℃ for 10~12 hours was repeated twice.

4. Bellflower Gujeunggupo

The bellflower, which had been immersed and sprayed, was placed in a steamer, passed through steam, and then steamed at 100 to 110° C. for 4 to 6 hours. The bellflower, which had undergone the steaming process, was placed in a dryer and heated at 60-80° C. for 180-220 hours by passing hot air. It is desirable to carry out the hot air drying process while alternately performing the wet heating method and the convection heat circulation method, and maintaining the humidity at 40 to 60%. The bellflower, which had undergone the heating process, was placed in an incubator and aged at 40 to 60° C. for 90 to 110 hours. The dried bellflower, which had undergone the aging process, was put in a cold air dryer and passed through cold air at 10 to 20° C. for 60 to 80 hours and dried.

Steps 3 and 4 were repeated 9 times with dried bellflower to prepare black bellflower in Gujeunggupo.

5. Gujeunggupo Black Bellflower Complex Concentrate Manufacturing

18 kg of Gujeunggupo black bellflower prepared above was taken in an extraction container, and 3 kg of wild ginseng, 9 kg of red ginseng, 6 kg of deodeok, 12 kg of maekmundong and 12 kg of sambaekcho were added, 120 kg of purified water was added, heated at 90-100 ° C. for 4-6 hours, and then filtered with cotton. .

The filtrate was taken, put in a vacuum concentrator, and concentrated under reduced pressure at 65-75° C. for 4-6 hours to obtain a Gujeung-gupo black bellflower complex concentrate (60-70 brix).

6. Gujeunggupo complex viscous liquid formulation

Take 10 kg of Gujeung-gupo Black Bellflower Complex Concentrate, put it in a preparation tank, and mix 10 kg of Sukji Hwangseok concentrate, 10 kg of ginseng powder, 7 kg of Bokryeong powder, 3 kg of deer antler powder, 2 kg of maca powder, 2 kg of acid medicine powder and 56 kg of honey at 60~80℃. By heating for ~4 hours, Gujeunggupo black bellflower complex viscous liquid formulation was prepared.

Gujeunggupo black bellflower complex viscous liquid formulation was filled and sealed in a polyethylene liquid stick by 10 to 12 g using an automatic filling machine while maintaining a temperature of 60 to 80 ° C.

bellflower analysis

1) Sample pretreatment process

After pulverizing gujeunggupo bellflower, 1 g of powder was put into a 15 mL test tube, 10 mL of methanol (99.99%) was added, and then placed in a sonicator and passed through ultrasonic waves for 10 minutes.

5 mL of the sample passed through ultrasonic waves was taken in a centrifuge tube, centrifuged at 13,000 rpm for 10 minutes, and then 1 mL of the supernatant was taken to obtain a stomatocyst sample solution.

Separately, dried bellflower (Comparative Example 1), which was not subjected to gujeunggupo, was operated in the same manner as a control solution.

2) Analysis device

Device name: 　 Ultra-performance liquid chromatograph (UPLC, Waters, Milford, USA)

Column: ACQUITY UPLC HSS T3 column (100mm x 2.1mm, 1.8um, Waters)

3) Analysis conditions

Sample injection volume: 5uL

Column temperature: 40℃

Mobile phase: A solvent (water + 0.1% formic acid)

Solvent B (acetonitrile + 0.1% formic acid)

Solvent gradient: normal phase solvent A 97% (0-5 min), 3-100% (5-16 min), 100% (16-17 min), reverse phase B solvent 100-3% (17-18 min), 97% (19-25 min)

Positive ion method: capillary voltage 2kV, cone voltage 40V

Anion method: capillary voltage 1kV, cone voltage 40V

Data Analysis: Waters UNIFI V1.71 Software

MS/MS scan range: 50~1200m/z

4) Analysis result

Pulverize the sample obtained by gujeunggupo of dried bellflower, 1g of powder was added to 10mL of methanol, passed ultrasonic waves, centrifuged, and 1mL of the supernatant was used as the sample solution of bellflower, 5ul of which was injected into the ultra-high pressure liquid chromatography apparatus. Next, the normal phase A solvent and the reverse phase B solvent were programmed at an appropriate ratio for 25 minutes, and the area of the peak was compared to compare the contents before and after gujeunggupo.

Table 1 is the area ratio of bellflower saponin components of Examples (Gujeunggupo black bellflower) and Comparative Example (general dried bellflower), and Table 2 is the area ratio of steroid components.

Ingredient name Unexpanded 9 packs 9 packs One Platycodin D 556 287089 2 Lobatoside I 610 849 3 Dehydrocorydaline 2525 4 2″-O-Acetylpoly-galacin D2 121173 5 Deapioplatycodin D 352433 6 Esculentoside K 260596 7 Julibroside C1 985802 8 Kajichigoside F1 248015 9 Mimengoside B 397 10 Platycodin C 274720 11 Polygalacin D 90464 12 Trachelosperoside B-1 508475 13 Trachelosperoside D-1 602198 14 Vaccaroside C 16672 3,691 3,748,883

Ingredient name Unexpanded 9 packs 9 packs One 14-Hydroxy sprengerinin C 1183 2 Astragaloside II 3380 3 Dioscoreside B 557 4 Marstenacigenin A 280 5 Neohecogenin-3-O-β-D-glucopyanosyl(1 2)-β-D-glucopyanosyl(1 4)-galactopy-ranoside 4327 6 Terrestrosin F 29080 7 Yesanchinoside J 381 8 Timosaponin F 270033 236816 9 Atroposide H 472401 10 Marstenacisside C 416 309,221 709,633

Figure 2 shows the bellflower saponin platicodin D peak, Figure 3 is the bellflower steroid atroposide H peak, Figures 4 and 5 are the black bellflower and extract production process of the present invention, Figure 6 is the black bellflower of the present invention This is an ultra-high pressure liquid chromatograph used for the analysis of bellflower.

Referring to Tables 1, 2, and FIGS. 2 to 3, the unexpanded sample (as a comparative example) showed a total of 401 peaks, and the total area was 540,039, whereas the gujeunggupo sample (Example 1) showed a total of 846 peaks. and the total area increased to 4,529,697, indicating an 8.3-fold increase in soluble components compared to the unexpanded sample.

Among them, there were 3 main saponin peaks in unpoed bellflowers and the area was very low as 3,691, but 13 saponin peaks in gujeunggupo bellflowers and an area of 3,748,883 were found, with an area ratio of more than 1,000 times through the gujeunggupo process. appeared to be increased.

On the other hand, the area of Platycodin D, a key component of bellflower, was 556 in the unexpanded sample, but 287,089 in the Gujeunggupo sample, which was confirmed to be increased 516 times compared to the unexpanded sample.

Comparing the content of soluble saponin in bellflower seeds, the saponin content of unpoulted bellflower was only 0.68%, but the saponin content of bellflower in gujeunggupo rose to 82.7%.

In particular, the content of Platicodin D, an active ingredient in bellflower, was 6.33%. On the other hand, there were 8 main steroid peaks in the unexpanded bellflower, and the area was 309,221, and the steroid peaks in the gujeunggupo bellflower were 3, and the area was relatively high with 709,663.

The steroid area of the old grapevine was 2.2 times higher than that of the unentrained grapevine, and among them, the peak of atroposide H was newly generated in the process of the old grapevine, and it was found that the area occupied 472,401.

Comparing the soluble steroid content, the unexpanded bellflower was relatively high at 57.2% of the soluble steroid, and the steroid content of the old bellflower was relatively low at 15.6%. appeared to be

In the above description, various embodiments of the present invention have been presented and described, but the present invention is not necessarily limited thereto. It will be readily appreciated that branch substitutions, transformations and alterations are possible.

Claims (6)

A step of heating wild ginseng, red ginseng, deodeok, maekmundong, sambaekcho, black bellflower and purified water into an extraction container;
filtering the solution in the extraction vessel; and
As a method for producing a black bellflower complex concentrate comprising the step of placing the filtrate in a vacuum concentrator and concentrating,
The black bellflower
(1) a pre-treatment step of putting the bellflower in a steamer, steaming, and drying the steamed bellflower;
(2) immersing the pre-treated bellflower in a natural plant fermented fermented liquid;
(3) spraying and infiltrating the fermented and aged natural fruit sugar pickle into the bellflower that has undergone the immersion process;
(4) putting the bellflower in a steamer and steaming;
(5) heating the bellflower, which has undergone the steaming step, with hot air;
(6) aging the bellflower that has undergone the heating process; and
(7) A method for producing a black bellflower complex concentrate comprising the step of drying the bellflower, which has undergone the aging step, with cold air, and is manufactured by repeating the cycle of steps (2) to (7) several times. The method of claim 1, wherein the immersion step is a step of immersing the pre-treated bellflower oil at 35-45° C. for 20-24 hours by adding a natural fruit sugar pickled fermented and aged solution,
The penetrating step is a method for producing black bellflower complex concentrate, characterized in that after spraying the fermented and ripening liquid of natural fruit sugar pickles on the bellflower that has been immersed, and then infiltrating it at 35 to 45° C. for 10 to 12 hours. The method according to claim 1, wherein the (4) steaming step is a step of putting the bellflower in a steamer and steaming the bellflower at 100 to 110° C. for 4 to 6 hours. The method according to claim 1, wherein the heating step heats the bellflower, which has undergone the (4) steaming step, at 60-80° C. for 180-220 hours by passing hot air,
In the aging step, the bellflower, which has undergone the heating process, is placed in an incubator and aged at 40 to 60° C. for 90 to 110 hours,
The drying step is a method for producing a black bellflower complex concentrate, characterized in that the dried bellflower, which has undergone the aging step, is passed through cold air at 10 to 20° C. for 60 to 80 hours. delete Preparing a complex viscous liquid formulation of black bellflower by mixing the black bellflower complex concentrate prepared according to claim 1 with Sukhumidus concentrate, ginseng powder, bokryeong powder, antler powder, maca powder, acid medicine powder and honey;
A method for producing a black bellflower liquid stick, comprising the step of charging and sealing the black bellflower complex viscous liquid formulation to the stick using an automatic charger while heating the liquid formulation to 60-80°C.

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