KR0184719B1 - Pinus koraiensis sieb powder - Google Patents

Abstract

The present invention extracts the leaves of Pinus Koraiensis Sieb. Et Zucc with water, ethanol or a mixture thereof at 60-70 ℃ to obtain an extract, the filtrate is continuously extracted with ethyl ether and ethyl agate to form an organic solvent layer After harvesting, the extract was concentrated under reduced pressure to prepare soft pine extract, and 20% to 40% by weight of 5% egg white was added thereto to remove tannins, and then concentrated under reduced pressure to dry by spray drying to produce pine cone extract.

The manufactured pine pine extract powder is convenient to take without astringent taste, and contains rutin and various amino acids, so it can be used as a health supplement in the treatment of circulatory diseases.

Description

Manufacturing method and its use of sea pine leaf extract

1 is a UV chart that tests the routine components of the pine pine extract powder.

2 is an amino acid analysis chart of the experiment of various amino acids in the pine pine extract.

3 is a GC-MS chart of essential oils in the pine leaf extract powder.

The present invention relates to a method for producing a pine pine extract and its use.

Haisong (Pinus Koraiensis Sieb. Et Zucc), also known as Hongsong, also known as Gwasong (Jangbaeksan), is a branch of the pine family (Pinaceae) about 30m high and about 1m wide. It is an evergreen tree growing in Changbai Mountain, Peninsula, Japan, Soviet Union, etc., and bark is gray reddish, split into pieces and reddish brown. The pine needles fall early, with 5 needles in the day, straight and slightly curved, 6-12cm long, with a triangular cross section and a pore line, and green without the pore line and narrow serrated around There are three kinds of local corridors but internal corridors.

It is known that sea pine leaves have a bitter taste and hot nature, and 30-60g is used in folk medicine for influenza, acupuncture, hypertension, and nervous breakdown (see Changbai Mountain Plant Book and Herb Herb).

Recently, the seaweed leaves contain essential oils and flavonoids, and essential oils include α-pinene, β-pinene, camphor, karen, terpinolone, limonene, bornyl acetate, sesquitelphen and diterpene. Flavonoid-based components, such as a lot of it has been found to have antipyretic, analgesic, anti-inflammatory and anti-convulsive action.

Until now, the method of taking sea pine leaves was taken by crushing finely, or by dipping them into water and then leaching them by filtration. Jill was coarse.

Therefore, the present invention solves the above drawbacks, as well as the existing antipyretic, analgesic, salt-containing and anti-convulsant action in addition to the effective treatment of circulating diseases that can be expected to contain the effective ingredient of the seaweed leaf pine powder extract The purpose is to provide.

Referring to the technical configuration of the present invention for achieving the above object of the present invention.

After extracting the pine pine leaves to prepare the pine pine extract, the effective amount of egg white is added to the mixture, and centrifuged to remove the precipitate by spray-drying to prepare a marine leaf extract powder.

To explain more specifically, the pine leaves are collected and dried in the shade, and then the powder is pulverized and extracted with filtrate at 60 to 70 ° C. with water or ethanol or a mixed solution thereof, and the filtrate is concentrated under reduced pressure. After the filtrate was shaken to obtain a filtrate, the filtrate was extracted with ethyl ether, and the organic solvent layer was partitioned. The remaining aqueous layer was removed with ethyl ether, cooled to room temperature, extracted with ethyl acetate, and then the organic solvent layer was fractionated. Collect the dried pineapple extract after drying under reduced pressure, and add 5% egg white 1-50% by weight, preferably 20-40% by weight, to homogenize at 60 ℃ for 30 minutes. After removing the tannin by centrifugation at high speed, concentrated under reduced pressure and spray-dried to prepare a pine leaf extract powder.

In carrying out the present invention, the extraction temperature during ethanol extraction is 60-70 ℃, repeated extraction 2-4 hours 2-3 times can maximize the extraction effect.

In the present invention is added to the egg white collected from the egg, to remove the tannin component of the astringent taste contained in the softening extract, the amount of use is 1-50% by weight, based on the softening extract based on 5% egg white, preferably Preferably, the amount corresponding to 20-40% by weight is used, and the removal mechanism of tannin is that a precipitate is formed by molecular bonding of tannin and egg white component, and the formed precipitate is easily separated from the soft extract by centrifugation. It can be removed.

Hae pine leaf extract powder prepared according to the present invention is convenient to take because it has no astringent taste, and is not inferior as a food additive, and contains a routine such as a flavonoid-based ingredient, which can be used alone or in other ingredients when treating circulatory diseases. In addition, there is a feature that can be used as a main ingredient or supplement of health foods, health drinks, carbonated drinks, tea and pharmaceutical drinks.

Hereinafter, examples and experimental examples of the present invention will be described.

Example 1

The pine needles are dried in a shade for a certain time, and 100 g of finely crushed red pine leaves are put in 2 liters of ethanol, and extracted by filtration twice at 60 ° C. for 2 hours.

The filtrate is then concentrated under reduced pressure at 60 ° C. or lower, and thereafter, 1 liter of hot water is added thereto, followed by shaking.

The filtrate was cooled to room temperature, 1 liter of ether was added, the mixture was stirred, and the organic solvent layer was fractionated by extracting three times at 20-30 DEG C for 1 hour until the organic solvent layer became clear.

The remaining aqueous layer is warmed in a water bath to completely remove the ether and left to cool to room temperature. Add 1 liter of ethyl acetate, stir and mix, and extract the organic solvent layer three times until the organic solvent layer is clear. The organic solvent layer is concentrated to dryness and 5% egg white (25 g) collected from eggs. After dissolving in water and mixing egg white water with Haesong extract at a certain temperature, after a certain time, egg white sediment is removed by centrifugation. The separated solution is concentrated under reduced pressure, spray-dried and dried. Got.

The sea pine leaf extract powder prepared according to Example 1 of the present invention showed the following experimental values.

(next)

1) Appearance: Brown dry extract powder with unusual odor.

2) Identification test: Take 1g of pine leaf extract powder, add 100ml of water, shake to dissolve, and add 50ml of 0.5% gelatin solution. No white precipitate is formed.

3) Moisture: 10% or less (Kalfitshire method)

4) Heavy metal: 30ppm or less

5) Arsenic: 4ppm or less

6) Ash: Less than 10.0%

7) Acid insoluble ash: 1.0% or less

8) Foreign body test: suitable

9) Tar Color: Not detected

10) Escherichia coli: negative

Furthermore, the UV chart of the rutin ingredient contained in the powder prepared according to Example 1 is shown in FIG. 1.

* Experimental Condition: SHT = 2 × 2 SCAN WIDTH = 8

λ = 267 DRIFT = 25

MIN AREA = 10, 000

*Calculation :

Therefore, it was confirmed that the routine ingredient, which is the active ingredient of the pharmaceutical agent for the circulatory machine, contained about 0.03% of the pine needle extract powder of the present invention.

On the other hand, the analysis results of the various amino acids contained in 100g of pine needle extract powder prepared according to Example 1 are based on Table 1 (Experimental Equipment: Hitachi company amino acid analyzer), the analysis chart is shown in FIG.

In addition, various essential oil components contained in 100 g of pine needle extract powder prepared according to Example 1 were identified and analyzed using a gas chromatograph mass spectrometer.

1) Equipment used: PYE-204 gas chromatograpy.

Column: SE-54 Capillary Columm (23m × 0.25mm)

Temperature program: 50 ~ 200 ℃ (raising temperature)

Carrier gas: He

Injection volume: 0.2μl

2) Equipment: VGMM 7070H mass spectrometer

resolution 600, ionization method (EI ion source)

Temperature 200 ℃

NG 2035 Recorder

The experimental results are shown in Table 2 below. As the essential oil components of sea pine leaf extract powder, 10 components could be separated and evaluated. Among them, α-pinene, camphene, β-pinene, limonene, and bornyl Acetate (bornyl acetate), α-terpinolene (α-terpinolene), δ-3-karen (caren) and mycene (myrcene) containing 10 essential oils were identified and separated. The analysis chart is shown in FIG.

Example 2-8

The same procedure as in Example 1, except that 5% egg white no addition and 5% egg white by weight of 10% by weight to prepare the pine leaf extract powder, the results of performing a panel test for astringent taste for each Example in Table 3 As shown in Table 3, it can be seen that the addition amount of egg white is most preferably 20-40% by weight.

※ Slight taste evaluation: ++ very strong

+ Can feel

-Can't feel it at all

Example 9-19

The same procedure as in Example 1 was carried out, but the egg white content was fixed to 30% by weight, and the following results were obtained when the main extraction solvent and the temperature conditions were different (see Table 4).

As can be seen in Examples 1 and 2-8, the astringent taste was completely removed, and as shown in Examples 9-19, the extract was maintained at 60-70 ° C. using ethanol as the extraction solvent to maintain the active ingredient. It can be seen that the most preferable in terms of yield of the amount of powder.

The recovery capacity of the pine pine extract powder prepared according to the present invention is 50-2000 mg, preferably 100-500 mg, and the powder is added to the tea and sausage of soft drinks, health supplements, and other foods. It is preferable to include in the range of 0.1-10w / v%, preferably 0.1-5w / v%.

Sea pine leaf extract powder prepared according to the present invention may add a preservative or preservative within the pharmaceutically acceptable range of food and medicine.

Hereinafter, the formulation example of the formulation containing the sea pine leaf extract powder according to the present invention is as follows.

[Example 1]

Haesong Leaf Extract Powder 500.0mg

───────────────

1cap.

[Example 2]

Haesong Leaf Extract Powder 500.0mg

Honey 150.0mg

3000.0mg per bag

Sodium benzoate 50.0 mg

Citric Acid 100.0mg

Purified water

───────────────

Total (pH 4.0) 120ml

[Example 3]

Haesong Leaf Extract Powder 500.0mg

Prickly Pear Dry Extract 50.0mg

Aminoethylsulfonic acid 1000.0mg

Nicotinic Acid Amide 20.0mg

Nitric acid nitrate 5.0mg

Pyridoxine Hydrochloride 5.0mg

Riboflavin Phosphate 5.0mg

5.0g high fructose

5.0 g of sugar

Citric Acid 150.0mg

Purified water

─────────────────

120 ml total

[Example 4]

Haesong Leaf Extract Powder 500mg

Palm oil 350mg

Soybean Oil 150mg

15 mg of lead

Gelatin 250mg

Concentrated glycerin 60 mg

D-sorbitol solution 40mg

Paraoxybenzoic Acid Methyl 1mg

10.2mg of paraoxybenzoate

150mg purified water

Ethanol 0.3mg

Echivanillin Correction

Titanium oxide 1.5mg

Yellow No. 5

Red No. 40

Blue No. 1

──────────────────

Total (soft capsule) 1600 mg

Next, the acute toxicity test of the pine leaf extract powder was performed and the results were described.

1. Experimental materials

(1) Material: The pine cone extract powder prepared according to Example 1 was prepared in an aqueous solution having a concentration of 25% during the experiment. (0.25 g / ml)

(2) Animal: 1CR rat of 20-22 g in weight

2.Experimental Method

Twenty rats are divided into two groups, female and male, each with a concentration of 0.25 g / ml powder and the maximum amount applicable to the rats is administered twice daily to the rat's stomach for 7 days. It was.

After the experiment was continued, the weight of the rats was measured, and the change status of the mice's defoliated leaf powder was recorded daily.

3. Experimental results

The rats were observed for 7 days, and the weight gained 0.9 0.2g on average daily.

The maximum dose of sea pine leaf extract powder in rats was 25g / Kg.

4. Experimental findings

The maximum capacity of the white pine cypress leaves is 25g / Kg, which is equivalent to 635g / Kg.

Therefore, the experimental results showed that the pine leaf extract powder was non-toxic.

As described above, the sea pine leaf extract powder of the present invention is non-toxic and has no astringent taste, which is convenient to take and can be used as a health supplement food for patients with circulatory diseases.

Claims (2)

After grinding the leaves of Pinus Koraiensis Sieb. Et Zucc, the extracts were repeatedly extracted 2-3 times at 60-70 ° C for 2-3 hours with water or ethanol, or a mixture thereof, and the filtrate was extracted and fractionated with ethyl ether. After preparing the pine leaf soft extract extract, add 20% to 40% by weight of 5% egg white to the pine leaf extract. Method for producing a pine pine extract powder, characterized in that. According to claim 1, 20% to 40% by weight of 5% egg whites are added to the extract extract of Pinus Koraiensis Sieb. Use.