KR102448998B1 - Development of Yuja processing technology using microhomogenization and drying condition - Google Patents

Abstract

The present invention comprises the steps of (1) preparing citron juice by pressing citron; (2) preparing an excipient by mixing maltodextrin and glucidex; (3) adding the excipient prepared in step (2) to the citron juice prepared in step (1), followed by stirring to prepare a citron mixture; (4) preparing by slicing the yuja jeongi including seeds; (5) mixing the citron mixture prepared in the step (3) with the sliced citron prepared in the step (4) and vacuum grinding to prepare a pulverized citron; (6) preparing a homogeneous citron by treating the pulverized citron prepared in step (5) with ultrasonic waves or ultra-high pressure; and (7) drying the citron homogenate prepared in the step (6).

Description

Development of Yuja processing technology using microhomogenization and drying condition

The present invention relates to a method for producing a citron powder, comprising the step of micro-homogenizing and then drying the pulverized citron, and to the citron powder produced by the method.

Recently, more than 70% of fresh citron fruit produced in the citron processing industry is used for processing. There is a need for research on the method.

Among the types of citron tea distributed in the market, the blue form is the most common, and the liquid, juice, and powder are in the order of powder. There is a need for practical research that can be done.

Ultrasonic homogenization is a mechanical process that reduces particles in a liquid and enables ultra-fine homogenization by making the target material fine from micro to nano level by uniformly small and uniformly distributed.

High pressure homogenization (HPH) has been used to shorten the extraction time of active ingredients in food or to inactivate microorganisms, but recently it has also been used to enhance sensory or to preserve nutrients such as vitamins. It was also used for inactivation of microorganisms or to increase texture in the processing of fruits and vegetables.

Korean Patent Publication No. 2003-0013000 discloses a method for producing citron powder, and Korean Patent No. 1394527 discloses a method for producing fine citron powder. different from development.

The present invention has been derived from the above needs, and an object of the present invention is to develop a citron powder material with improved fragrance components and functional and sensory properties, such as micro-homogenization technique, drying method, citron pretreatment and selection of excipients, etc. An object of the present invention is to provide a method for producing high-quality citron powder by optimizing the production conditions.

In order to solve the above problems, the present invention comprises the steps of (1) producing citron juice by cold-pressing citron; (2) preparing an excipient by mixing maltodextrin and glucidex; (3) adding the excipient prepared in step (2) to the citron juice prepared in step (1), followed by stirring to prepare a citron mixture; (4) preparing by slicing the yuja jeongi including seeds; (5) mixing the citron mixture prepared in the step (3) with the sliced citron prepared in the step (4) and vacuum grinding to prepare a pulverized citron; (6) preparing a homogeneous citron by treating the pulverized citron prepared in step (5) with ultrasonic waves or ultra-high pressure; and (7) drying the citron homogenate prepared in the step (6).

In addition, the present invention provides a citron powder prepared by the above method.

The citron powder produced by the method of the present invention also improves color, fragrance, and overall preference, and the citron powder produced through the manufacturing process of the present invention is more efficient than other processing processes, can be processed in a short time, and loss of raw materials is reduced. It has the effect of being able to manufacture high-quality powder while minimizing it.

1 is a photograph of citron powder prepared by varying the type and mixing ratio of excipients.
2 is a photograph of citron powder prepared by varying the mixing ratio of maltodextrin (MD) and glucidex (GD).
3 is a photograph of citron powder and the citron powder dissolved in water according to the ultrasonic treatment time. From the far left, it means citron powder that has been sonicated for 15 minutes, 30 minutes, 1 hour, and 1 hour and 30 minutes.
4 is a photograph of citron powder ultrasonicated spray-dried (US) according to the type of excipient (maltodextrin (MD), glucidex (GD), gum arabic (GA)).
5 is a photograph of citron powder observed using a scanning electron microscope.
6 is a photograph comparing the storage stability of citron powder according to room temperature storage and refrigerated storage period.
7 shows the results of electronic nose multivariate statistical analysis (PCA) to confirm the relative difference in fragrance components between samples of citron powder.
8 is a graph comparing the DPPH radical scavenging ability and ABTS radical scavenging ability of citron powder.
5 to 8 Y-UF, Y-US, Y-UM, Y-HF, Y-HS, Y-HM see Table 1

In order to achieve the object of the present invention, the present invention

(1) cold-pressing citron to prepare citron juice;

(2) preparing an excipient by mixing maltodextrin and glucidex;

(3) adding the excipient prepared in step (2) to the citron juice prepared in step (1), followed by stirring to prepare a citron mixture;

(4) preparing by slicing the yuja jeongi including seeds;

(5) mixing the citron mixture prepared in the step (3) with the sliced citron prepared in the step (4) and vacuum grinding to prepare a pulverized citron;

(6) preparing a homogeneous citron by treating the pulverized citron prepared in step (5) with ultrasonic waves or ultra-high pressure; and

(7) provides a method for producing citron powder, characterized in that it comprises the step of drying the citron homogenate prepared in step (6).

In the method for producing citron powder of the present invention, the excipient in step (2) is preferably a mixture of maltodextrin and glucidex in a weight ratio of 0.8 to 1.2:1.8 to 2.2, more preferably maltodextrin. and glucidex may be mixed in a weight ratio of 1:2. The use of excipients mixed in the same type and ratio as above does not affect the taste and flavor of the citron powder, and the dried powder is not sticky and dissolves well in water. will be selected

In addition, in the method for producing citron powder of the present invention, the citron mixture in step (3) is preferably stirred for 50 to 70 minutes after adding 28 to 32% (w/v) of excipients compared to citron juice to citron juice. and, more preferably, 30% (w/v) of excipient compared to citron juice is added to citron juice and stirred for 60 minutes. When the excipient was added to the citron juice extracted from the citron under the same conditions as above and stirred, the excipient was well dissolved and the flavor and color of the prepared powder could be further enhanced.

In addition, in the method for producing citron powder of the present invention, the pulverized citron in step (5) is preferably mixed with 80 to 120 g of sliced citron and 270 to 330 mL of citron mixture and vacuum pulverized for 4 to 6 minutes. It can be prepared, and more preferably, 300 mL of citron mixture is mixed with 100 g of sliced citron and vacuum pulverized for 5 minutes. Mixing the citron mixture with the citron mixture under the same conditions as above gave better taste and could be mixed under the conditions for easy powdering.

In addition, in the method for producing citron powder of the present invention, the ultrasonic treatment in step (6) may preferably be performed at 28 to 32 kHz for 12 to 18 minutes, more preferably at 30 kHz for 15 minutes. Can be sonicated. In addition, the ultra-high pressure treatment may be preferably performed at an ultra-high pressure of 800 to 1200 bar, and more preferably at an ultra-high pressure of 1000 bar.

Ultrasonic or ultra-high pressure treatment under the same conditions as described above could finely homogenize the citron vacuum pulverized material that was not homogenized due to cellulose without damaging the citron flavor.

In addition, in the method for producing citron powder of the present invention, the drying in step (7) may be preferably freeze-drying, spray-drying or microwave drying, but is not limited thereto.

The freeze-drying may be preferably freeze-dried at -70 to -90°C for 40 to 60 hours, more preferably freeze-dried at -80°C for 48 hours. Freeze-drying under the same conditions as above improved the storage stability of the prepared powder, and it was possible to increase the palatability and quality characteristics.

In addition, the spray drying may be preferably performed using a spray dryer set at an injection temperature of 160 to 200 ° C, a discharge temperature of 90 to 110 ° C, and a sample supply rate of 40 to 50 ml/min, and more preferably at an injection temperature It can be dried using a spray dryer set at 180° C., release temperature 100° C., and sample feed rate 45 ml/min.

In addition, the microwave drying may be preferably performed using a micro vacuum dryer set at an infrared temperature of 50 to 60 ° C and an air temperature of 20 to 40 Torr, more preferably an infrared temperature of 56 ° C. and an air temperature of 28 Torr. It can be dried using a set micro vacuum dryer.

The manufacturing method of the citron powder of this invention, more specifically,

(1) cold-pressing citron to prepare citron juice;

(2) preparing an excipient by mixing maltodextrin and glucidex in a weight ratio of 0.8 to 1.2: 1.8 to 2.2;

(3) After adding 28-32% (w/v) of the excipient prepared in the step (2) compared to the citron juice to the citron juice prepared in the step (1), and stirring for 50 to 70 minutes to prepare a citron mixture step;

(4) preparing citron jeongi, including seeds, cut into 3-5 equal parts;

(5) Mix 270-330 mL of the citron mixture prepared in step (3) with 80-120 g of the sliced citron prepared in step (4) and vacuum-pulverize for 4-6 minutes to prepare a pulverized citron ;

(6) preparing a homogeneous citron by treating the pulverized citron prepared in step (5) with ultrasonic waves or ultra-high pressure; and

(7) may include the step of drying the citron homogenate prepared in step (6),

more specifically

(1) preparing citron juice by pressing citron;

(2) preparing an excipient by mixing maltodextrin and glucidex in a weight ratio of 1:2;

(3) preparing a citron mixture by adding 30% (w/v) of the excipient prepared in step (2) compared to citron juice to the citron juice prepared in step (1) and stirring for 60 minutes;

(4) preparing citron jeongi including seeds by slicing it into quarters;

(5) mixing 300 mL of the citron mixture prepared in step (3) with 100 g of the sliced citron prepared in step (4) and vacuum grinding for 5 minutes to prepare a pulverized citron;

(6) preparing a homogeneous citron by treating the pulverized citron prepared in step (5) with ultrasonic waves or ultra-high pressure; and

(7) It may include the step of drying the citron homogenate prepared in step (6).

The present invention also provides a citron powder prepared by the above method.

Hereinafter, production examples and examples of the present invention will be described in detail. However, the following Preparation Examples and Examples only illustrate the present invention, the content of the present invention is not limited to the following Preparation Examples and Examples.

Preparation Example 1. Sonication and freeze-dried citron powder (Y-UF)

(1) Citron juice was prepared by cold-pressing citron at -10°C or lower without applying heat.

To ensure the safety of the citron raw material used above, 320 pesticide residue tests were conducted, and bifenthrin, sulfoxaflor, carbendazim, and pyridalyl were detected below the allowable standard, and the safety of all remaining 316 ingredients was verified. raw material that has been

(2) An excipient was prepared by mixing maltodextrin and glucidex in a weight ratio of 1:2.

(3) 30% (w/v) of the excipient prepared in step (2) was added to the citron juice prepared in step (1), compared to citron juice, and stirred for 1 hour to prepare a citron mixture.

(4) Prepared by cutting the yuja jeongi including seeds into 4 equal parts.

(5) Mix 300 mL of the citron mixture prepared in step (3) with 100 g of the sliced citron prepared in step (4), and vacuum grind for 5 minutes, and filter large particles using a vacuum pump using pressure to prepare a yuzu pulverized product.

(6) The citron pulverized product prepared in step (5) was sonicated at 30 kHz for 15 minutes to prepare a fine homogenized citron homogenate.

(7) The citron homogenate prepared in step (6) was dried for 48 hours using a freeze dryer (Freeze dryer, IlShin Bio Base) while maintaining -80°C and a vacuum pressure of 5×10 ^-³ .

Preparation Example 2. Ultrasonic Treatment and Spray Dried Citron Powder (Y-US)

(1) A pulverized citron was prepared in the same manner as in (1) to (5) of Preparation Example 1.

(2) The pulverized citron prepared in step (1) was sonicated at 30 kHz for 15 minutes to prepare a fine homogenized citron homogenate.

(3) A spray dryer (B-290, Buchi mini spray dryer) set at an injection temperature of 180° C., a discharge temperature of 100° C., and a spray rate of 45 mL/min of sample supply for the citron homogenate prepared in step (2) was dried using

Preparation Example 3. Ultrasonic Treatment and Microwave Vacuum-Dried Citron Powder (Y-UM)

(1) A pulverized citron was prepared in the same manner as in (1) to (5) of Preparation Example 1.

(2) The pulverized citron prepared in step (1) was sonicated at 30 kHz for 15 minutes to prepare a fine homogenized citron homogenate.

(3) The citron homogenate prepared in step (2) was dried using a microwave vacuum dryer (V1400, UNION Tech Co, Ltd, Cheonan, Korea) set at an infrared temperature of 56° C. and a vacuum degree of 28 Torr in the furnace.

Preparation Example 4. Ultra-high pressure treatment and freeze-dried citron powder (Y-HF)

(1) A pulverized citron was prepared in the same manner as in (1) to (5) of Preparation Example 1.

(2) The pulverized citron prepared in step (1) was subjected to ultra-high pressure treatment at 1000 bar for 3 cycles to prepare a fine homogenized citron homogenate.

(3) The citron homogenate prepared in step (2) was dried for 48 hours using a freeze dryer (IlShin Bio Base) while maintaining -80°C and a vacuum pressure of 5×10 ^-³ .

Preparation 5. Ultra-high pressure treatment and spray-dried citron powder (Y-HS)

(1) A pulverized citron was prepared in the same manner as in (1) to (5) of Preparation Example 1.

(2) The pulverized citron prepared in step (1) was subjected to ultra-high pressure treatment at 1000 bar for 3 cycles to prepare a fine homogenized citron homogenate.

(3) A spray dryer (B-290, Buchi mini spray dryer) set at an injection temperature of 180° C., a discharge temperature of 100° C., and a spray rate of 45 mL/min of sample supply for the citron homogenate prepared in step (2) was dried using

Preparation Example 6. Ultra-high pressure treatment and microwave vacuum drying citron powder (Y-HM)

(1) A pulverized citron was prepared in the same manner as in (1) to (5) of Preparation Example 1.

(2) The pulverized citron prepared in step (1) was subjected to ultra-high pressure treatment at 1000 bar for 3 cycles to prepare a fine homogenized citron homogenate.

(3) The citron homogenate prepared in step (2) was dried using a microwave vacuum dryer (V1400, UNION Tech Co, Ltd, Cheonan, Korea) set at an infrared temperature of 56° C. and a vacuum degree of 28 Torr in the furnace.

Example 1. Establishment of pretreatment conditions for citron samples for micro-homogenization technology

The citron whole fruit was crushed (500 g) with the rind and seeds using a slicer and vacuum crushed for 5 minutes by adding 1000, 750, 500, and 250 g of water. Freeze-drying for time was compared. At this time, 2.5 g, 5 g, and 10 g of maltodextrin were added to 100 mL of vacuum-milled citron grinding solution, and the mixture was stirred for 12 hours. As a result of the experiment, the higher the mixing amount of maltodextrin, the better it dissolves in water, and the more time passes, the more citron scent is. Therefore, it was judged that it would be better not to add the excipient directly to the pulverized citron.

After extracting citron oil by centrifuging cold-pressed citron juice, maltodextrin was added and powdering was attempted. At this time, 30% of maltodextrin was added to citron juice, and 0%, 0.5%, 1%, and 2% of citron oil were added. In the case of the citron oil addition port, despite the addition of 30% of maltodextrin, the citron oil was separated and separated upon drying, so it was decided not to add the citron oil separately. In addition, when maltodextrin is added to citron juice, it is easily soluble and can be prepared as a powder with a small particle size, so it was decided to add an excipient to citron juice.

As a result of a preference survey with powder according to the ratio of cold-pressed citron juice and citron crushed product stirred with the addition of excipients, it was found that it was best to add it in a ratio of 3:1. In addition, the use of citron juice in crushed citron increased the stickiness of the powder compared to water, but resulted in a higher flavor and color of the powder. Therefore, it was decided to mix citron juice with crushed citron and use instead of water.

In addition, as a result of evaluating the preference according to the presence or absence of filter treatment, it was evaluated that the flavor of the unfiltered sample was better than that of the filtered sample. There was no significant difference from the sample, so only large particles were filtered out using vacuum pump filtering.

Example 2. Selection of excipients for powdering and establishment of optimal mixing ratio

After mixing 60 g of citron with water and vacuum grinding for 20 minutes, 5, 10, 15, and 20% maltodextrin were prepared in an aqueous solution, then mixed with the ground citron in a 1:1 ratio, stirred for 12 hours, and dried. The fragrance of citron in the state of being powdered and the fragrance of citron dissolved in water were compared. In the powder state, the lower the content of maltodextrin, the more fragrant, but in the state of dissolving in water, the higher the content, the stronger the flavor.

After mixing 60 g of citron and water and vacuum grinding for 20 minutes, 5, 10, 15, and 20% maltodextrin powder was added 1:1 with the crushed citron, stirred for 12 hours, and dried to obtain a powdery state. The fragrance and the fragrance of citron dissolved in water were compared. The scent was stronger when mixed with crushed citron in powder form than when mixed with crushed citron in an aqueous solution of maltodextrin.

Maltodextrin was used, sonication was fixed at 30 minutes, and the amount of maltodextrin was increased to 25, 5, and 10 g for comparison. The less maltodextrin was added, the more yellow the color was, and the higher the content, the closer it was to white, and the better it was soluble in water.

Using maltodextrin, glucidex, and gum arabic as excipients, the amount of the three powders was varied and 30% of the powder was added to citron juice and compared. As a result of comparing maltodextrin and glucidex in a ratio of 1:2, gum arabic and glucidex 1:2, and maltodextrin, glucidex and gum arabic in a ratio of 1:1:1, It is judged that the addition will give off a sour flavor, which will decrease the preference. Therefore, the experiment was conducted using only maltodextrin and glucidex except gum arabic (FIG. 1).

Using maltodextrin (MD) and glucidex (GD) as excipients, 30% of the two powdered materials were added to citron juice at different ratios and compared. As a result of the preceding experiment, it was found that the single use of maltodextrin resulted in severe whitening and masking of the scent, and the single use of glucidex had less masking of the scent than maltodextrin, but the powder was not sticky and hard. As the ratio of maltodextrin increased, whitening occurred, and when dried, it was not sticky and brittle. On the other hand, the higher the ratio of glucidex, the more the color of citron juice is maintained, and it is easily soluble in water and has a fragrance. However, when the ratio of maltodextrin to glucidex is 1:3, and the ratio of glucdex is higher, the dry matter becomes sticky and the ratio of maltodextrin to glucidex 1:2 is judged to be the optimal ratio (Fig. 2). .

Example 3. Establishment of conditions for ultra-high pressure homogenization or ultrasonic homogenization

Citron (60 g) and water (750 mL) were vacuum-pulverized until no large particles were visible to the eye.

After vacuum pulverizing 60 g of citron and 750 mL of water for 20 minutes, ultrasonication was performed for 15 minutes, 30 minutes, 1 hour, and 1 hour and 30 minutes, respectively, to compare the solubility and fragrance in water. As a result of comparing the fragrance of citron powder in a powder state and a state dissolved in water, it is determined that 15-minute sonication is the most appropriate (FIG. 3).

The particle size of the citron powder treated with ultrasonication before drying was 1790±5021 nm, PDI was 0228, and Zeta Potential was 332mV, so the particles were very stable.

The color, flavor and particle size were compared when 1 cycle, 2 cycle, and 3 cycle treatment of the pulverized citron at 1000 bar (pressure) and ultra-high pressure. There was no noticeable difference in color and smell between the stock solution and cycle 1, 2, and 3, and 3 cycles at 1000 bar were established as treatment conditions in consideration of particle size and PDI.

Example 4. Trial of powdering using three different drying methods and establishment of conditions

Spray drying: The injection temperature was set to 180°C, the discharge temperature was set to 100°C, and the spraying rate was powdered using a spray dryer (B-290, Buchi mini spray dryer) under the condition of sample supply 45 mL/min. When the recovery amount was compared, the citron powder spray-dried using maltodextrin (MD) and glucidex (GD) at 200 mL had the most at 6430 g, followed by gum arabic (GA) and glucidex (GD). ) was 5639 g, and the citron powder using maltodextrin (MD), gum arabic (GA) and glucidex (GD) was 5354 g. The citron powder using the two excipients differed by more than 10 g (Fig. 4).

Freeze-drying: The temperature was maintained at -80°C and the vacuum pressure was 5×10 ^-³ , and it was dried for 48 hours using a freeze dryer (IlShin Bio Base).

Microwave vacuum drying: Infrared temperature 56 ℃, the vacuum degree in the furnace was set to 28 Torr, and powdered using a microwave vacuum dryer (V1400, UNION Tech Co, Ltd, Cheonan, Korea).

Microwave vacuum drying was not possible with citron juice itself. When the recovery amount was compared, the citron powder treated with microwave vacuum drying using gum arabic (GA) and glucidex (GD) as excipients had a higher recovery rate than other treated powders.

Example 5. Moisture content, particle size, particle surface structure and storage stability of powder by drying method

After ultra-high pressure homogenization treatment or ultrasonic homogenization treatment, three different drying methods were used to prepare powders (Table 1).

Citron Powder Type division processing conditions Y-UF Lyophilization after sonication Y-US After ultrasonication, spray drying Y-UM Microwave vacuum drying after ultrasonication Y-HF Freeze-drying after ultra-high pressure treatment Y-HS After ultra-high pressure treatment, spray drying Y-HM Microwave vacuum drying after ultra-high pressure treatment

1) Moisture content

The moisture content was measured by drying using an infrared moisture meter (MA100, sartorius) at 105° C. until the moisture content of 2 g of citron powder reached a constant weight. The spray-dried powder had the lowest water content in both ultra-high pressure treatment and ultrasonic treatment, and the lyophilized powder treated with ultrasonication showed the highest water content.

Moisture content measurement results by drying method Y-UF Y-US Y-UM Y-HF Y-HS Y-HM Moisture content (%) 3.96±0.18 1.85±0.45 3.76±0.16 3.62±0.08 2.43±0.32 3.64±0.10

2) particle size

The particle size was measured by using a particle size analyzer (HELOS/RODOS&SUCELL, Sympatec GmbH) based on the laser diffraction theory in the flow-air-dispersion method (unit ㎛). The particle size of the ultra-high pressure-treated powder was smaller than that of the ultrasonic-treated powder. Among them, the ultra-high pressure-treated spray-dried powder had the smallest size, and the ultrasonic-treated and freeze-dried powder had the largest size.

Particle size analysis result by drying method Y-UF Y-US Y-UM Y-HF Y-HS Y-HM Particle size (㎛) 15.19±0.50 4.27±0.07 14.77±0.89 10.61±0.94 4.11±0.31 13.33±0.56

3) Measurement of particle surface structure

Scanning electron microscopy (SEM) was used to measure the particle morphology and particle surface structure of the dried citron powder. Citron powder was coated with gold for 40 seconds before SEM measurement, and an SEM image was obtained at an acceleration voltage of 3 kV. The freeze-dried citron powder and microwave vacuum-dried citron powder had a large particle size, and the spray-dried citron powder had a smaller particle size compared to other dry powders (FIG. 5).

4) Storage stability

In order to observe the storage stability of the powder, the change of the powder for each period was observed during refrigeration and room temperature storage. As a result of observing one week, the powders stored at room temperature showed agglomeration compared to the powders stored in the refrigerator, and it was observed that the agglomeration of the spray-dried powder was the most severe (FIG. 6).

Example 6. Analysis of physicochemical properties of powder by drying method

After ultra-high pressure homogenization treatment or ultrasonic homogenization treatment, three different drying methods were used to prepare powders, and then physicochemical properties were measured.

1) pH, sugar content and water content

The pH and sugar content were dissolved by adding 10 times distilled water to the sample, and then using a pH meter (S20-K, METTLER-TOLEDO Inlab ^ⓡ 413, Switzerland) and a portable sugar meter (PAL-3, 0 to 93%, ATAGO) measured. For moisture content, 1 g of the sample was spread evenly on an aluminum sample pan, dried and heated using a moisture analyzer (HE53, METTLER TOLEDO, Switzerland), and then the weight was measured.

For each drying condition, the pH of the citron powder sample was 278~285, which was the highest in Y-UF and Y-HM, the sugar content was 10.2~10.5 Brix and there was no difference between the samples. Numerical values were shown (Table 4).

Physicochemical properties of citron powder by drying conditions Analysis items Y-UF Y-US Y-UM Y-HF Y-HS Y-HM pH 2.85 2.83 2.78 2.84 2.84 2.85 Sugar content (Brix) 10.2 10.3 10.2 10.3 10.5 10.3 moisture 3.67±0.25 2.19±0.31 3.45±0.51 3.65±0.23 2.58±0.45 3.68±0.38

2) Chromaticity

For chromaticity measurement, 1 g of the sample was measured using a colorimeter (Chromameter SP-80, Tokyo Denshoku, Japan) to measure the brightness L value (lightness) indicating the brightness level, the redness a value (redness) indicating the degree of redness, and the degree of yellowness. The indicated yellowness b value (yellowness) was measured, and the L, a, and b values of the citron powder samples by drying conditions showed similar numerical values.

Citron powder chromaticity by drying conditions Analysis items Y-UF Y-US Y-UM Y-HF Y-HS Y-HM chromaticity L 93.77±0.38 91.91±0.24 93.24±0.45 92.43±0.20 94.23±0.51 92.35±0.63 a -1.28±0.17 -1.62±0.08 -2.11±0.25 -2.09±0.08 -1.80±0.23 -1.88±0.25 b 11.93±0.09 10.91±0.21 12.45±0.16 12.06±0.31 11.74±0.82 12.84±0.48

3) Analysis of organic acids and free sugars

For the analysis of organic acids and free sugars, 0.5 g of citron powder was taken and purified with 10 mL of distilled water, filtered through a 0.22 μm membrane filter (Futecs Co., Ltd., Daejeon, Korea), and analyzed by HPLC system (Shimadzu Co., Kyoto, Japan). (analysis conditions Aminex HPX-87H Ion Exclusion column (300×7.8 mm, 9 μm, Bio-Rad Labs., Richmond, CA, USA), flow rate 0.6 mL/min, column oven temperature 35° C.) The content of each peak was calculated by comparing the peak area ratio and retention time of the standard material analyzed under the same conditions.

Organic acid content of citron powder by drying conditions (Unit: g/100g) Sample organic acid Citric acid malic acid succinic acid Y-UF 15.60±0.02 1.88±0.01 0.90±0.06 Y-US 12.60±0.05 1.36±0.17 0.58±0.07 Y-UM 17.52±0.03 2.06±0.02 1.07±0.02 Y-HF 13.72±0.04 1.55±0.07 0.70±0.06 Y-HS 13.90±0.03 1.71±0.02 0.89±0.02 Y-HM 13.78±0.01 1.72±0.04 0.88±0.03

The organic acid content was detected in the order of citric acid, malic acid, and succinic acid, and was high in the microwave vacuum-dried Y-UM sample after sonication (Table 6).

Free sugar content of citron powder by drying conditions (Unit: g/100g) Sample free sugar Sucrose Glucose Fructose Y-UF 7.99±0.20 4.91±0.21 5.09±0.26 Y-US 6.48±0.21 3.27±0.56 3.37±0.53 Y-UM 7.17±0.08 4.74±0.22 5.16±0.15 Y-HF 8.95±0.12 4.19±0.13 4.01±0.29 Y-HS 9.00±0.16 4.38±0.18 4.36±0.19 Y-HM 8.83±0.09 4.34±0.11 4.40±0.08

Sucrose, glucose, and fructose were detected as free sugars, sucrose in the ultra-high pressure spray-dried sample, glucose in the ultrasonic-treated freeze-dried sample, and fructose in the ultrasonic-treated microwave vacuum-dried sample. was detected (Table 7).

Example 7. Hygroscopicity and solubility of powder by drying method

After taking 1 g of a sample and leaving it for 3 hours in a desiccator controlled to a saturated state, the amount of moisture absorbed was measured to measure the degree of moisture absorption. After adding 20 times distilled water to 1.5 g of the sample, each time (10 minutes, 20 minutes) , 30 min) at room temperature, and after taking 20 mL each, the acidity was specified, and the solubility was indicated by the change in acidity. The acidity was titrated with 0.1N NaOH solution until pH 8.0 to obtain the consumed volume (ml) of the NaOH solution, and then converted into citric acid (conversion factor 0.0064).

Hygroscopicity of citron powder by drying conditions division Y-UF Y-US Y-UM Y-HF Y-HS Y-HM hygroscopicity 1.21% 0.75% 1.18% 1.24% 0.69% 1.20%

The hygroscopicity was slightly higher in the freeze-dried and microwave vacuum-dried samples than the spray-dried samples in the samples by drying conditions (Table 8).

Solubility of citron powder by drying conditions hour Y-UF Y-US Y-UM Y-HF Y-HS Y-HM 10 minutes 6.41 6.53 6.46 6.83 6.60 6.57 20 minutes 6.62 6.49 6.55 6.89 6.74 6.62 30 minutes 6.74 6.62 6.68 6.90 6.79 6.74

The solubility did not show a significant difference over time in the samples for each drying condition, which is thought to be because maltodextrin and glucidex used as powdered substrates are water-soluble substances that dissolve well in water (Table 9).

Example 8. Analysis of the sensory properties of powder by drying method

The inspector consisted of about 100 students from Kunsan University and an external panel, and a 7-point rating method for citron powder and dissolved products. 5 points 'Somewhat good' 6 points 'Good' 7 points 'Very good'. As a result of the sensory evaluation test, the 794 product (Y-UF) had the highest preference for ‘citron fragrance’, and the overall preference was also good compared to other citron powders (Table 10).

Preference sensory test of citron powder by drying conditions characteristic Sample No. ¹⁾ 794 207 539 341 973 836 458 energy
like
do color 4.90±1.30 ^a 4.67±1.42 ^a 5.07±0.69 ^a 5.00±1.17 ^a 2.90±1.12 ^b 4.63±1.22 ^a 4.97±1.13 ^a color choice 5.03±1.13 ^a 4.50±1.20 ^ab 5.03±0.81 ^a 5.10±1.09 ^a 3.20±1.21 ^c 4.37±1.22 ^b 4.87±1.11 ^ab citron 5.33±0.88 ^a 3.90±1.03 ^c 4.13±1.11 ^bc 4.57±1.19 ^b 2.40±0.97 ^d 3.70±0.95 ^c 3.87±0.86 ^c Overall
symbol 5.10±1.03 ^a 4.37±1.00 ^cd 4.57±0.73 ^bc 4.87±0.90 ^ab 2.37±0.89 ^e 3.90±1.03 ^d 4.20±0.81 ^cd

Sample No. ¹⁾ 794: Y-UF, 207: Y-US, 539: Y-UM, 341: Y-HF, 973: YC, 836: Y-HS, 458: Y-HM

Example 9. Analysis of fragrance characteristics of powder by drying method

For the analysis of fragrance characteristics of 6 citron powder samples by drying conditions, quantitative analysis of fragrance components using GC-MS and qualitative analysis of fragrance patterns were performed using electronic nose. Citron powder samples were taken as headspace-vials, 1 g each, and used as a sample for analyzing fragrance characteristics.

1) Analysis of fragrance components using GC-MS

Quantitative analysis of citron powder fragrance components was performed using GCMS-QP2010 Plus (Shimadzu, Kyoto, Japan) instrument with GC/MS (Purge&Trap Gas Chromatography/Mass Spectrometer), and was collected by adsorption in a PAT adsorption tube at 60℃ for 30 minutes. The analysis conditions are as shown in Table 11, and the content was calculated by comparing the peak area ratio and retention time of the indicator material (DL-Limonene).

Conditions for analysis of citron powder fragrance components column DB-624 column (30mm×0.25mm×1.40㎛) Initial column temperature 40℃ Final column temperature 260℃ Oven temperature 40℃(3min) to 260℃(10min) at 10℃(1min) carrier gas He Make-up gas nitrogen MS temperature 250℃

The content of limonene, a fragrance component of citron, showed the highest content in the lyophilized sample (Y-UF) treated with ultrasonication, which was nearly three times higher than that of the control (Table 12).

Analysis of Limonene Content of Citron Powder Fragrance Ingredients by Drying Conditions sample control Y-UF Y-US Y-UM Y-HF Y-HS Y-HM Peak Area 6460411 19007447 493131 5225362 7127411 640071 4882369 μg 2.463 7.277 0.173 1.989 2.719 0.230 1.857 Sample amount (g) 0.49 0.49 0.5 0.49 0.52 0.5 0.5 Limonene
(μg/g) 5.03 14.85 0.35 4.06 5.23 0.46 3.71

2) Analysis of fragrance component pattern using electronic nose

Qualitative analysis of citron powder fragrance components was performed using electronic nose (Heracles II, Alpha, Toulouse, France) analysis equipment, detectors were FID (flame ionization detectors), and columns were MTX-5 (polar), MTX-1701 (non-polar). was used, and the temperature was maintained at 50-80°C (1°C/s) and 80-250°C (3°C/s) for 2 minutes. The flow rate was 1 ㎖/min, the injection amount was 1,000 μl, and data analysis was performed with AlphaSoft version 14.2, AroChemBase V6.

The main volatile fragrance components of citron are limonene, γ-terpinene, linalool, β-myrcene, β-farnesene, α -Pinene (α-pinene) and β-pinene (β-pinene), etc. are known.

Major volatility of C (control), US (Y-US), UF (Y-UF), UM (Y-UM), HS (Y-HS), HF (Y-HF), HM (Y-HM) samples As a result of analyzing the fragrance component, the ultrasonically treated freeze-dried sample (UF) showed more than twice the content of limonene, γ-terpinene, and linalool compared to the control (Table 13).

As a result of multivariate statistical analysis (PCA) that confirms the relative difference between samples based on the content of major citron aroma components, the freeze-dried samples (Y-UF, Y-HF) treated with ultrasonic waves and ultra-high pressure on PCA were similar because the distance between each sample was close. With a pattern, other samples showed a fragrance pattern similar to that of the control (FIG. 7).

Example 10. Analysis of antioxidant efficacy of powder by drying method

DPPH (α,α-diphenyl-β-picrylhydrazyl) radical scavenging activity is obtained by dissolving 1 g of citron powder sample by adding 10 mL of distilled water. Absorbance was measured at 492 nm, and the activity was calculated by the formula DPPH radical electron donating capacity (%) = (1-absorbance of the sample added / absorbance of no sample) × 100.

ABTS (2,2′-Azino-bis(3-ethylbenzothiazoline-6-sulfonicacid)) radical scavenging activity was obtained by mixing 7 mM ABTS and 2.4 mM potassium persulfate in a 1:1 ratio and leaving it in a dark place for 24 hours. 2.7 mL of the diluted ABTS radical solution and 0.3 mL of the sample were mixed and reacted for 30 minutes, and absorbance was measured at 732 nm. The activity was calculated by 100.

As a result, the DPPH radical scavenging activity showed a high value in the freeze-dried or microwave vacuum-dried sample after ultrasonication, and the ABTS radical scavenging activity showed the highest activity in the lyophilized sample (Y-UF) treated with ultrasonication (Fig. 8).

Claims (6)

(1) cold-pressing citron to prepare citron juice;
(2) preparing an excipient of maltodextrin;
(3) adding the excipient prepared in step (2) to the citron juice prepared in step (1), followed by stirring to prepare a citron mixture;
(4) preparing by slicing the yuja jeongi including seeds;
(5) mixing the citron mixture prepared in the step (3) with the sliced citron prepared in the step (4) and vacuum grinding to prepare a pulverized citron;
(6) preparing a homogeneous citron by treating the pulverized citron prepared in step (5) with ultrasonic waves or ultra-high pressure; and
(7) A method for producing citron powder, characterized in that it comprises the step of drying the citron homogenate prepared in step (6). delete The method according to claim 1, wherein the drying in step (7) is freeze-drying, spray-drying or microwave drying. According to claim 1,
(1) cold-pressing citron to prepare citron juice;
(2) preparing an excipient of maltodextrin;
(3) After adding 28-32% (w/v) of the excipient prepared in the step (2) compared to the citron juice to the citron juice prepared in the step (1), and stirring for 50 to 70 minutes to prepare a citron mixture step;
(4) preparing by slicing the yuja jeongi including seeds;
(5) Mix 270-330 mL of the citron mixture prepared in step (3) with 80-120 g of the sliced citron prepared in step (4) and vacuum-pulverize for 4-6 minutes to prepare a pulverized citron ;
(6) preparing a homogeneous citron by treating the pulverized citron prepared in step (5) with ultrasonic waves or ultra-high pressure; and
(7) A method for producing citron powder, characterized in that it comprises the step of drying the citron homogenate prepared in step (6). 5. The method of claim 4,
(1) cold-pressing citron to prepare citron juice;
(2) preparing an excipient of maltodextrin;
(3) After adding 28-32% (w/v) of the excipient prepared in the step (2) compared to the citron juice to the citron juice prepared in the step (1), and stirring for 50 to 70 minutes to prepare a citron mixture step;
(4) preparing citron jeongi including seeds by slicing them into 3-5 equal parts;
(5) Mix 270-330 mL of the citron mixture prepared in step (3) with 80-120 g of the sliced citron prepared in step (4) and vacuum-pulverize for 4-6 minutes to prepare a pulverized citron ;
(6) sonicating the pulverized citron prepared in step (5) at 28 to 32 kHz for 12 to 18 minutes to prepare a citron homogenate; and
(7) A method for producing citron powder, comprising the step of freeze-drying the citron homogenate prepared in step (6) at -70 to -90° C. for 40 to 60 hours. A citron powder produced by the method of any one of claims 1, 3 to 5.

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