KR100900810B1 - Method for preparing of Korean citrus peel increased of aglycone flavnoid and mixture containing the powder - Google Patents

Abstract

The present invention relates to a dermis powder having an increased amount of a non-dodecyl compound of dermis, a method for producing the dermis powder, and a composition containing the powder,

More specifically, a citrus dermis consisting of a common glycoside compound is treated with a saccharolytic enzyme such as cellulase, betaglucarase, xylanase, etc., and reacted over a certain period of time to improve quality characteristics such as the elution yield of dermis, , Naringenin, and the like are increased and the content of the non-dodecyl compound is increased to produce a dermis having a high content of the non-dodecyl compound. The dermis powder, ≪ / RTI >

dermis

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dermis powder, a dermis composition containing a dermis compound,

       FIG. 1 is a graph showing changes in content of total phenolic compounds, electron donating ability, and nitrite scavenging ability of a flavonoid elution extract, a contour map

FIG. 2 is a graph showing the change of contour map of naringin, hesperidin, naringenin and hesperetin according to the present invention

FIG. 3 is a graph showing the relationship between the yield of flavonoid elution and the content of naringenin and hesperetin according to the present invention.

4 is a graph showing the results of comparing the yield of flavonoids eluted from the general dermis and the dermis according to the present invention

FIG. 5 is a graph showing the results of comparing the electron donating ability of the general dermis and the dermis according to the present invention,

6 is a graph showing the results of comparing nitrite scavenging ability of general dermis and dermis according to the present invention

7 is a graph showing the results of comparing ACE inhibitory activities of general dermis and dermis according to the present invention

8 is a graph showing the results of comparing the mechanical redness of a general dermis and the dermis according to the present invention

Figure 9 shows a preferred process step of the present invention

The present invention relates to a dermis powder in which the content of a non-dodecyl compound of the dermis is increased, a method for producing the dermis powder, and a composition containing the powder,

The dermis has been used as herbal medicine since ancient times and dried the skin of ripe orange. The pharmacological actions of the dermis are known to be increased activity of lipid digestive enzymes, antiallergic effect, suppression of uterine muscle contraction, sedative effect, inhibition of capillary permeability, arteriosclerosis by arteriosclerosis, and prevention of hypertension. In one room, the dermis promotes gastric secretion and helps digestion. It is used to cure cough and phlegm symptoms caused by bronchitis, etc. In Korea, it has been used for a long time because it has been boiled and dipped in dandruff when it was caught by cold. . The main physiologically active ingredient of the dermis is composed of glycoside compounds such as naringin and hesperidin. Naringin and hesperidin, which are glycoside forms, are known to have less antioxidative, anti-inflammatory and anti-cancer activities than naringenin and hessperin (chajaeyoung, physiology activity of Cho, Young - Su 2001 citrus flavonoids. Korean J Soc Agric Chem Biotechnol 44 (2) 122-128). These glycoside compounds are known to be poorly digested and absorbed in the human body.

  In addition, most of the dermis is being used for medicinal purposes, and is being used in the form of tea bags in the form of concern. In case of concern in the form of tea bag, the elution yield should be high, and it takes time to elute.

   Therefore, the present invention provides a dermis powder having an increased dissolution yield and an increased non-parasitic compound content, and a powder prepared thereby to provide beverage compositions, food additives and the like.

  It was also tried to make a composition in the form of fine granules by using it in combination with other excipients.

Accordingly, the present invention has been made to solve the above problems

It is an object of the present invention to provide a process for preparing a citrus fruit having a physiologically active substance in the form of a glycoside by the enzymatic treatment and the quality of the dermis itself such as flavonoid elution yield, total phenolic compound content, electron donating ability, nitrite scavenging activity, Which has an increased antioxidant, anti-inflammatory and anticancer activity, and which has a high elution yield. The produced dermis is mixed with various processed products and compositions to provide citrus dandelion powder which can be applied to beverage composition, food additive and the like.

Another object of the present invention is to provide a composition which can be taken intact in combination with other excipients so that the flesh of the mandarin dermis is formed.

The structure and operation of the present invention will be described.

As shown in FIG. 9, the method for producing dermal powder according to the present invention comprises a first step of washing citrus fruits, a second step of separating and shredding the shells, a step of adding enzyme to the chopped shells, 3, and lyophilization to form a dermis powder in the fourth step.

In addition, by treating with a saccharolytic enzyme such as cellulase, betaglucarase, xylanase and the like for a predetermined period of time, the quality of the dermis, especially the elution yield, is increased, and the production and content of the undecanoic compound are increased, Of the dermis of the present invention can be produced, and this will be demonstrated through an experiment according to the following examples.

The present experiment compares the quality characteristics such as flavonoid extraction yield, total phenolic compound content, electron donating ability, nitrite scavenging activity and ACE inhibitory activity of the general dermis and the dermis according to the embodiment of the present invention.

In addition, this experiment compares the composition of flavonoids by changing contents of hesperetin and naringenin, which are undecodomeric compounds of general dermis and dermis according to the embodiment of the present invention.

The optimal enzyme concentration and reaction time are identified through the above experimental results.

<Examples>

 In 2006, Jeju organic citrus fruits, which do not contain pesticides, waxes, etc., were used.

Enzyme treatment

  A mixture of cellulase, betaglucarase and xylan lase active ingredient Viscozyme L (Viscozyme, Novozyme Co. Denmark) was added to the whole volume at a constant concentration at a ratio of 1: 3, Lt; / RTI &gt; In order to produce high-quality dermis, enzymatic treatment with the enzyme concentration (0, 0.5, 1, 1.5, 2%) and enzyme treatment time (0, 6, 12, 18, 24 hr) And then lyophilized (lyophilized by enzymatic treatment, liquefied and liquefied, so all of the enzymes treated were lyophilized), and some large particles were pulverized to examine the quality characteristics of dermis and the composition of the planovoids.

Table 1

Flavonoid extraction

The extraction of flavonoids from citrus fruits was carried out as follows with reference to the Perfetti method. 1 g of the powdered sample was mixed with 20% DMF methanol (n, n-di-methylformamide) and methanol in a volume ratio of 20:80) and the mixture was refluxed at 90 ° C for 4 hours.

yield

The extracts of flavonoids were added to a handful of water, and the solids content was measured by heating at 105 ° C under atmospheric pressure.

Flavonoid analysis

The extract was cooled, filtered and diluted to 25 ml with 20% DMF methanol. This solution was filtered with a 0.45 mu m filter to prepare a sample for HPLC analysis.

Flavonoid analysis

Determination of total phenolic compound content

The total phenolic compound content of each extract was colorimetrically determined according to the Folin-Denis method (17). That is, 5 ml of Folin-Ciocalteu reagent was added to 5 ml of the sample solution diluted 100 times with the extract, and after 3 minutes, 5 ml of 10% Na ₂ CO ₃ was added and the mixture was shaken and left at room temperature for 1 hour to measure the absorbance at 700 nm. The control was treated in the same way with distilled water instead of the test solution. At this time, tannic acid was prepared as a standard substance at a concentration of 5 ~ 50 μg / ml and used to prepare a calibration curve.

Electron donating ability (EDA)

The electron donating ability (EDA) of the test solution was measured by the method using α, α-diphenyl-β-picrylhydrazyl (DPPH). That is, 12 mg of DPPH reagent is dissolved in 100 ml of absolute ethanol, 100 ml of distilled water is added, 50% ethanol solution is blanked, the absorbance of the DPPH solution is adjusted to 1.0 at 517 nm, 5 ml of the solution is mixed with 0.5 ml of the sample solution After incubation at room temperature for 30 seconds, the absorbance at 517 nm was measured, and the difference in absorbance between the sample added and the non-added sample was expressed as a percentage (%) to be the electron donating ability.

Nitrite scavenging ability

Colorimetric determination was made at 520 nm by Kato et al. That is, a sample of a predetermined concentration was added to 1 ml of a 1 mM NaCO ₃ solution, and the pH of the reaction solution was adjusted to 1.2, 0.1, and 1, respectively, using 0.1 N HCl (pH 1.2) and 0.2 M citric acid buffer (pH 3.0, 3.0, 4.2 and 6.0, and each reaction solution was adjusted to 10 ml. Each reaction solution was incubated at 37 ° C for 1 hour, and then 1 ml of 2% acetic acid solution (5 ml) was added, and 1% sulfanilic acid and 1% naphthylamine (1: (Shimadzu UV-1601PC, Japan) was used to measure the absorbance at 520 nm, and the nitrite scavenging rate was measured according to the following equation. The absorbance was measured using a spectrophotometer (Shimadzu UV-1601PC, Japan) Respectively.

    N: nitrite scavenging rate

A: Absorbance after left standing for 1 hour by adding sample to 1 mM NaNO ₂ solution

B: Absorbance of NaNO ₂ solution

    C: Absorbance of the sample itself

ACE inhibitory activity

 Angiotensin converting enzyme inhibitory effect was measured by Cushman and Ondetti method. The reaction solution was prepared by dissolving 2.5 mM of hippuryl-L-histidyl-L-leucine (HHL, Sigma, H1635) in 0.1 M potassium phosphate buffer (pH 8.3) containing 0.3 M NaCl and 0.15 mL of ACE A6778, 0.2 unit / mL) and 0.1 mL of each sample solution were mixed. For the control, 0.1 mL of distilled water was added to the control sample, and the reaction was carried out at 37 ° C. for 30 minutes. The reaction was stopped by addition of 0.25 mL of 1N HCl 1.5 mL of ethyl aacetate was added. Ethyl acetate was distilled from the solvent and 1 mL of distilled water was added to the residue. The absorbance of hippuric acid was measured at 228 nm using a spectrophotometer.

A: The amount of hippuric acid produced in the reaction mixture

B: hippuric acid production in the control

1. Quality Characteristics

Table 2 shows the yield, total phenolic compound content, electron donating ability, and nitrite scavenging ability of the enzyme-treated citrus peel in combination with the levels shown in Table 1 as quality characteristics for the lyophilized powder.

Table 2.

As shown in Table 2, the elution yield was 48.49% for the general dermis and 63.03 ~ 72.97% for the enzyme treatment. In addition, when the citrus peel was compared with the freeze-dried one, the freeze-dried amount was 50.36%, which is slightly higher than the general dryness, but not significantly different. The contents of total phenolic compounds were 7.87 mg% in the general dermis and 8.24 ~ 10.94 mg% in the enzyme treatment, but it was not much different from the general dermis. In the case of electron donating ability, 7.54% in the case of general dermis, but 13.56 ~ 18.38% in case of enzyme treatment, showed that enzyme treatment of the general dermis has higher activity than general dermis. In the case of nitrite scavenging ability, general dermis was 1.50%, but it was 17.79 ~ 23.43% when treated with enzyme.

Based on these results, the second-order regression equation for the response surface analysis is shown in Table 3, and overall significance was recognized at the significance level of R2 0.9 or higher and within 5%.

Table 3

1) X1: enzyme concentration (%), X2: time (hr)

Based on the regression equations in Table 3, contour maps and optimal values are predicted as shown in FIGS. 1 and 4. FIG.

Table 4.

As shown in Table 4 and FIG. 1, the elution yield was a graph showing the maximum value when the enzyme concentration was 1.41% and the reaction time was 15.38 hr. The contents of total phenolic compounds showed higher contents of enzyme and higher reaction time, and it was predicted that the enzyme treatment concentration was 1.55% and the reaction time was 22.00 hr. The electron donating ability was predicted to be high when the enzyme treatment concentration was 1.32% and the reaction time was 16.57 hr, and the graph showed a maximum point. The nitrite scavenging activity was predicted to have the maximum value at the enzyme treatment concentration of 1.165% and the reaction time of 17.67 hr. Overall, the total phenolic compound content, electron donating ability and nitrite scavenging activity were affected by the enzyme reaction time rather than the enzyme concentration as shown in Table 5.

Table 5

*** Significant at 1% level,

** Significant at 5% level,

* Significant at 10% level

2. Flavonoid Composition

The major flavonoid compounds that are harmful to citrus are the glycoside forms of naringin and hesperidin and their undecomposed forms of naringenin and hesperetin, as well as rutin, deosmine, nobiletin and tangeretin.

Among the citrus flavonoids, the antioxidant activity was highest in the hessperin, and the aglycone forms hessperine and naringenin were reported to be higher than their glycoside forms, naringin and hesperidin. Thus, in this example, the flavonoid composition of the citrus peel when subjected to the enzyme treatment, namely the levels of naringin, hesperidin, hesperetin and naringenin,

Table 6

As shown in Table 6, the content of hesperidin was 58.85 mg / g in the general dermis and no other flavonoids were detected. When hesperidin was reacted for about 12 hr without enzyme addition, 54.17 mg / g of hesperidine, 0.20 mg / g of naringenin, 0.13 mg / g of hesperetin and naringin were not detected, and hesperidin 54.30 mg / g, and others were not detected. However, the amount of hesperidin decreased with enzymatic treatment, while that of naringenin and hesperetin increased.

Based on these results, the second-order regression equation was obtained from the response surface analysis through SAS program. As shown in Table 7, the significance level of hesperidin to R2 0.8693 was found to be within 10% of the significance level. Naringin, And in case of hesperetin, significance was recognized at significance level within R2 0.9 and 5%.

Table 7

1) X1: enzyme concentration (%), X2: time (hr)

Based on the regression equations in Table 7, the contour map and the optimum value prediction condition are shown in FIG. 2 and Table 8.

Table 8

As shown in Table 8 and FIG. 2, the maximum value was predicted at the enzyme concentration of 1.20% and the reaction time of 11.88 hr in case of Naringin. In the case of hesperidin, the enzyme concentration decreased by 0.32% The maximum value was predicted at 3.25 hr. In the case of naringinin, the content increased with increasing enzyme reaction time. The maximum value was predicted when enzyme treatment concentration was 1.34% and reaction time was 23.27 hr. In the case of hesperetin, the enzyme concentration increased and the reaction time increased. The maximum value was estimated at the enzyme treatment concentration of 1.69% and the reaction time of 20.74 hr. As a result of examining the influences of flavonoid components on the enzyme treatment conditions, it was found that the overall reaction time was affected as shown in Table 9.

Table 9

*** Significant at 1% level,

 ** Significant at 5% level,

  * Significant at 10% level

In order to set the optimum conditions for enzyme treatment for producing the high-quality dermis, it was attempted to establish conditions of excellent elution yield and content of non-dividing compounds hesperetin and naringenin. As a result, the result of overlapping each contour map was as shown in Fig. 3. As a result of setting the optimum enzyme treatment conditions, the enzyme treatment concentration was 1.1 ~ 1.8% and the reaction time was 15 ~ 20 hr. Therefore, the optimum conditions for enzyme treatment were set as 1.5% enzyme reaction time and 18 hr reaction time.

Table 10

In the conventional dermis production method, the dermal powder (CC) dried at 40 ° C and the enzyme treatment concentration set at 1.5% and the reaction time set for the reaction time of 18 hr, Quality characteristics were compared.

1) Elution yield and Flavonoid content

1 g of each sample was eluted in 100 ml of distilled water at 95 ° C for 1 hour, and the soluble solid content was measured and calculated as a yield. As a result, as shown in FIG. 4, the enzyme-treated dermis powder showed a higher dissolution rate.

As a result of comparing the composition of flavonoids, only hesperidin was detected in the general dermis, but in the case of the dermis powder treated with the enzyme as shown in Table 11, the non-dividing compounds hesperetin and naringenin were high contents

Table 11

2) Electron donating ability, nitrite scavenging activity, ACE inhibitory activity

The activities of electron donating ability, nitrite scavenging ability and ACE inhibitory activity were controlled by controlling the concentration of crude flavonoid extract at a constant concentration (10000, 5000, 2500 ppm) by the functional properties of general dermis powder and enzyme - treated dermis powder.

  In the case of electron donating ability, nitrite scavenging ability and ACE inhibiting activity, as shown in FIGS. 5, 6 and 7, the enzyme treated dermal powder (CE) showed higher activity than the common dermal CC, The activity was found to be high. Overall, the enzyme-treated dermis (CE) was twice as high as the normal dermis (CC).

3) Mechanical color

As a result of comparing the mechanical chromaticity of the general dermis (CC) with that of the enzyme-treated dermis (CE), the whiteness (L value) and the yellow value (b value) And a value of enzyme treated dermis was higher than that of general dermis. It is believed that as the enzyme treatment, the browning of the citrus peel itself occurs somewhat and has a slight red color.

According to the above example, the saccharide bark was reacted with a saccharolase, beta-glucacase, xylanase, or the like, for a predetermined period of time, thereby yielding the total phenolic compound content, electron donating ability, nitrite scavenging ability, ACE degradation activity, and the production and content of non-parasitic compounds such as naringenin and hesperetin, which are excellent in antioxidation, anti-inflammation and anticancer activity among the flavonoid compositions, are increased. The enzymatic treatment conditions are that the enzyme treatment concentration is 1.1 to 1.8%, the reaction time is 15 to 20 hours, more preferably the enzyme treatment concentration is 1.5%, and the reaction time is 18 hours.

The dermis powder treated with the enzyme under the optimum conditions can be prepared as an active ingredient in foods or food additives, and can be prepared as an active ingredient according to the purpose of use without any specific restriction on the food.

For example, a composition comprising 49.10% of dandruff powder, 16.37% of lactose, 16.37% of starch, 16.37% of glucose, 1.63% of mannitol, 0.08% of vitamin C and 0.08% of malic acid was mixed and a small amount of water The mixture is then filtered through an 18 mesh sieve and dried at 50 ° C for about 2 hours to form a powdery dermal composition which can be taken in powder form or in water to be ingested in the form of tea.

      As described above, according to the present invention, by optimizing enzyme concentration and reaction time, it can be applied to the dermis to improve quality in comparison with general dermis. In particular, the dermis, which has a high elution yield and an increased non- Powder is constituted so that the dermis powder is composed of an effective ingredient, and the effect of contributing to the health promotion of a consumer by providing a food additive is a multi-purpose invention.

Claims (3)

The first step of washing the citrus fruits, the second step of separating and shredding the shells, the weight of the chopped shells and water were mixed at a ratio of 1: 3, and the cellulase, beta-glucanase, Wherein the enzyme treatment concentration of the dermis is 1.1 to 1.8% based on the total volume of the mixture and the reaction time is from 15 to 20 hours; and a fourth step of lyophilizing the powder after lyophilization. Production of dermis powder with improved quality and increased content of non-dodecyl compound A process for producing a dermis powder according to claim 1, wherein the dermis comprises a dermis powder having a dermis quality characteristic, A mixture of 49.10% by weight of the dermis powder, 16.37% by weight of lactose, 16.37% by weight of starch, 16.37% by weight of glucose, 1.63% by weight of mannitol, 0.08% by weight of vitamin C and 0.08% 5 to 10% water is added to the mixture and mixed. After 18mesh filtering And then dried at 50 DEG C for 2 hours. The composition comprising the dermis powder, which is improved in the quality of the dermis and the content of the non-dodecyl compound, is increased

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