KR20110000186A - Garlic oil extraction method using extremely high pressure method and organic solvent extraction, the garlic oil and the garlic oil capsule - Google Patents

Abstract

PURPOSE: A garlic oil extraction method using ultra high pressure extraction and organic solvent extraction processes is provided to massively extract garlic oil after simply removing the unique odor of garlic. CONSTITUTION: A garlic oil extraction method comprises the following steps: crushing or grinding peeled garlic; extracting the crushed or grinded garlic using ultra high pressure; and adding an organic solvent to the obtained extract for extracting. The ultra high pressure extracting process is performed in 100~2,000MPa.

Description

Garlic oil extraction method using extremely high pressure method and organic solvent extraction, the garlic oil and the garlic oil capsule}

The present invention relates to a garlic oil extraction method using ultra-high pressure extraction and organic solvent extraction and garlic oil and garlic oil capsules extracted by the method.

Garlic ( Allium sativum L.), a report of Phytochemical, is an indispensable seasoning in our lifetime, and is known for its excellent value as a food, as well as a variety of bioactive functions. Due to the recent development of a new, luxurious and various garlic products using garlic.

Currently, most garlic processing forms are garlic powders and paste products that can be used as intermediate materials of food, and recently, health supplements such as garlic drinks, garlic vinegar, and garlic rings have been released. However, most of these garlic processed products have a problem of irritating smell as well as discoloration such as browning and greening of garlic, and products released as health supplements also have poor commerciality due to poor eating and taste. Because of this, more than 98% of domestically produced garlic is used as raw garlic, and its processing rate is less than about 2%. Therefore, there is an urgent need for a method to effectively use garlic containing a large amount of physiologically active ingredients.

Oleoresin, defined as a mixture of essential oils and resins extracted from spices such as pepper, onion, and garlic, contains a lot of bioactive substances. Garlic oil is a kind of oleoresin, which not only maintains the characteristics of garlic's inherent bioactive substances, but also has high shelf life, enables uniformity and standardization of quality, thereby increasing interest in this. In order to find a way to commercialize garlic oil, various methods have been studied, but effective technologies have not been proposed due to problems such as economic efficiency and homogenization of extracted oil quality. Garlic oil, in particular, is not easily consumed by consumers due to the allicin (allicin) component that causes garlic's peculiar smell.

Extracting garlic with methanol yields crystalline amino acid S-allyl-L-cystein sulfoxide. When garlic is cut or crushed, the garlic cells are destroyed, and an enzyme called aliinaase present in the garlic cells converts allicin to allicin, pyruvic acid and ammonia. It is decomposed into methyl disulfide or the like to give garlic its distinctive aroma. Thiosulfate, such as allicin, which is present in garlic, is known to be involved in garlic's antidiabetic, lowering cholesterol, lowering blood pressure, anticancer and antibacterial functions.

However, allicin not only makes garlic hard to ingest due to its unique smell, but also has problems such as bad breath and bad body odor.

In the related art of garlic, patent publication No. 1996-14608, "Method for Extracting Oil-type Garlic Liquid," is dried and pulverized raw garlic and then heated to 60-80 ° C in garlic juice obtained by high-pressure concentration to evaporate moisture and allicin odor. In this garlic solution, the alcohol solution is 10 times the distillation treatment for 20 to 30 hours by hot air of 50 ~ 60 ℃ to remove the secondary odor smell discloses a method of obtaining an oil type garlic liquid.

However, the technique is time-consuming and expensive by going through two heat treatment or hot air distillation processes to remove allicin, which is not only economical, but also does not completely remove allicin.

In addition, in Patent No. 664091 "Microencapsulation method of garlic oleoresin and the microcapsules prepared by the method", ethanol is added to the garlic ground by peeling garlic and extracted with a crusher, and then filtered in a constant temperature water bath, and filtered. Disclosed is a method of preparing a microcapsule by mixing garlic oleoresin obtained by concentrating at 35 ° C. with an evaporator as a nucleus material of a microcapsule and mixing it with a capsule material of an aqueous food polymer material and an emulsifier.

However, since the technique extracts garlic oleoresin by the organic solvent extraction method, there is a problem that the allicin component of garlic cannot be sufficiently removed.

Accordingly, an object of the present invention is to provide a method of removing the smell of garlic in a simple manner and extracting garlic oil in large quantities.

In addition, an object of the present invention is to provide a formulation easy to ingest by using the extracted garlic oil as a raw material.

As a result of the study to achieve the above object, the present inventors first make ultra-high pressure extraction of garlic to loosen the hard fibrous tissue of garlic, and then extract the organic oil using a second organic solvent to effectively extract a large amount of garlic oil by a simple method. Said.

In addition, the inventors have encapsulated the garlic oil extracted in this way to be more easily ingested.

The present invention is a method for extracting garlic oil,

Grinding or grinding the peeled garlic;

Ultra-high pressure extraction of the ground or ground garlic; And

It provides a garlic oil extraction method comprising; extracting by adding an organic solvent to the ultra-high pressure extract.

In addition, the present invention is a method for extracting garlic oil,

Grinding or grinding the peeled garlic;

Extracting by adding an organic solvent to the ground or ground garlic; And

It provides a garlic oil extraction method comprising a; step of extracting the ultra-high pressure of the extract.

Further, the present invention provides a garlic oil extraction method characterized in that the ultra-high pressure extraction proceeds in the range of 100 ~ 2,000MPa. Extraction at a pressure of less than 100 MPa does not result in high allicin removal efficiency.

The present invention also provides a garlic oil extraction method characterized in that the organic solvent is at least one selected from the group consisting of ethanol, methanol, propanol, butanol, ethanol aqueous solution, aqueous methanol solution, ethyl acetate, chloroform and hexane.

In addition, the present invention is extracted by the above method, provides a garlic oil having an allicin content of 20% by weight or less based on 100% by weight of raw garlic allicin.

In addition, the present invention provides a garlic oil capsule prepared by adding a food or acceptable carrier or excipient to the garlic oil extracted by the above method. Food acceptable carriers or excipients include maltodextrin, modified starch, gum arabic, gelatin, and the like, which may be used alone or in combination.

The present inventors compared the organic solvent extraction method and the ultra-high pressure extraction method for the preparation of garlic oil, and extracted by various methods focusing on the problem of eliminating allicin which is a characteristic ingredient of garlic and the yield problem of garlic oil extraction.

Figure 2 illustrates an example of extracting garlic oil by the ultra-high pressure extraction method. To facilitate extraction, garlic was peeled and pulverized, followed by stirring with water. This was filtered through filter paper and then centrifuged to obtain a supernatant. The obtained supernatant was dried at 30 ° C. for 30 minutes and then extracted using ultra high pressure equipment (Wave 6000/135).

1 is a result of measuring allicin removal efficiency while varying the pressure in the ultra-high pressure extraction method. Ultra high pressure extraction at 100, 300 and 500 MPa, respectively, resulted in an allicin content of less than 10% after 3 minutes at 500 MPa, and almost 4% of allicin was removed. From this result, it was found that the ultra-high pressure extraction effectively removes the allicin component contained in garlic.

However, as a result of measuring the extraction efficiency of garlic oil active ingredient by the ultra-high pressure extraction method, as shown in Fig. 3 showed very low yield even in the extraction of 10 hours, it was confirmed that there is a limit to the ultra-high pressure extraction method alone in extracting the active ingredient in garlic.

Extraction methods using organic solvents such as ethanol have been used for garlic oil extraction in the past, but it is difficult to remove allicin only by extracting organic solvents, and the fact that allicin content is lowered only by adding a method such as heat treatment or heat distillation is already used. It has been reported.

The inventors can simultaneously test the ultra-high pressure extraction method and the organic solvent extraction method to extract the garlic oil in garlic (mixed with "oleoresin" in the description and drawings of the present invention) in high yield with an allicin removal effect. Said that.

In the present invention, peeling, pulverizing and extracting the ultrahigh pressure garlic as shown in Figure 4, the organic solvent was added to extract the active ingredient of garlic sufficiently and then centrifuged to obtain a supernatant, filtered and concentrated to obtain a good quality garlic oil.

In FIG. 4, an ultra-high pressure extraction process is first performed, followed by an organic solvent extraction process. However, the scope of the present invention is not limited to the example of FIG. 4. First, after performing the organic solvent extraction process, the ultrahigh pressure extraction process was able to achieve a similar degree of allicin removal effect (95% or more) and garlic oil obtaining effect (about 90%) (data not shown).

Furthermore, the present inventors attempted to prepare a variety of formulations in order to easily ingest the garlic oil obtained as described above, when the garlic oil is powdered to make a capsule formulation, the intake is easier than liquid oil, and the active ingredient deterioration is hardly observed. It also confirmed that the storage is easy.

According to the present invention, the allicin component of garlic can be removed by a simple process.

In addition, according to the method of performing a combination of ultra-high pressure extraction and organic solvent extraction of the present invention can remove the allicin component and obtain a high yield of garlic oil which is the active ingredient contained in garlic.

In addition, according to the present invention it is possible to easily ingest the active ingredient of garlic by encapsulating the garlic oil obtained as described above.

Hereinafter, the configuration of the present invention will be described in more detail with reference to specific embodiments. However, it will be apparent to those skilled in the art that the scope of the present invention is not limited only to the description of the embodiments.

Materials and methods

1. Experimental material

Garlic used in this experiment was purchased by Seosan garlic harvested in June 2008 and used to peel only the diameter of the area. Peeled garlic was used after grinding for about 3-5 minutes with a mill to facilitate oil extraction.

2. Ultra High Pressure Extraction Method

The application of the ultra-high pressure extraction process to garlic was largely focused on two things. In other words, the first analyzes the removal effect of allicin, a unique ingredient of garlic, and the second analyzes whether garlic oil can be extracted by using the allicin-free garlic.

1) In this embodiment, the ground garlic was extracted by ultra high pressure using a Wave 6000/135 model which is an ultra high pressure device. At this time, the pressure was applied to adjust to 100, 300, 500MPa respectively.

2) To extract the oil of garlic using the ultra-high pressure extraction method, the garlic was first ground or pulverized, and then water was added about twice the weight of garlic (W / V), and then stirred at 45 ° C. for 3 hours and filtered. The filtered garlic extract was centrifuged at 6,000 rpm for 10 minutes, the supernatant was obtained, dried and then subjected to an ultrahigh pressure process.

3. Garlic oil extraction using organic solvent

After adding ethanol in the ratio of 1: 1, 1: 2, 1: 3 of the weight of garlic, the extraction temperature is 20 ~ 50 ℃, and the extraction time is 1 ~ 4 hours. Extraction and measurement of oleoresin (or garlic oil) content and thiosulfate content are shown in FIGS. 7 and 8.

As shown in Figs. 7 and 8, the extraction yield of garlic oil by organic solvent was found to be very good, about 32%, and the thiosulfate content was 170.13 μmol / g, which is equivalent to the quality of garlic oil by ultra high pressure extraction. .

Therefore, the optimum extraction conditions of garlic oil by the organic solvent was determined as ethanol content 1: 2 (garlic: ethanol), extraction temperature 30 ℃, extraction time 3 hours.

4. Ultra high pressure extraction process and extraction process using organic solvent

In order to effectively extract a large amount of garlic oil from garlic, in this embodiment, two processes of ultra-high pressure extraction process and organic solvent extraction process were performed in parallel.

Water was added to twice the weight of garlic to ground or ground garlic as shown in Figure 4, stirred for 3 hours at 45 ℃ and filtered, the filtrate was 6,000rpm, centrifuged for 10 minutes to obtain a supernatant and then dried for 30 minutes Ultra high pressure extraction was performed.

10 times the amount of ethanol was added to the extract obtained by ultra-high pressure extraction, and the mixture was sufficiently stirred, followed by centrifugation for 10 minutes at 6,000 rpm. The supernatant obtained here was filtered and concentrated to give a dark yellow garlic oil (see Fig. 5).

5. Manufacture of Capsules by Spray Drying Method

Garlic oil obtained as described above was put into a spray dryer with dextrin and gum arabic to attempt to powder the capsules. This process is carried out by a conventional method well known to those skilled in the art, detailed description thereof will be omitted.

6. Quality Analysis

1) Analysis of content of oleoresin (garlic oil): Garlic oil content measurement is extracted from a constant temperature water bath maintained at a constant temperature by adding ethanol to the garlic shredded with garlic and crushed for 3 to 5 minutes with a crusher, then centrifuged and filtered The extract was taken. The extract was concentrated under reduced pressure at 40 ° C to be oleoresin. Yield and solid content of the garlic at this time was measured by 105 ℃ atmospheric pressure drying method.

2) Determination of thiosulfate content: Thiosulfate content was concentrated under reduced pressure of 0.5 ml of cysteine-containing buffer, and 0.1 ml of solution dissolved in 1 ml of ethanol was added thereto, and 4.4 ml of 50 mM buffer was added to the total reaction. The volume of the solution was 5 ml. 2 ml of the reaction solution was further prepared, prepared in 50 mM buffer, and then mixed with 2 ml of 0.4 mM DTNB, and then absorbed at 412 nm using an absorbance spectrophotometer.

Results and Discussion

1. Ultra high pressure extraction method

1) Allicin Removal Effect of Garlic by Pressure

In this experiment, the experiments were carried out at different pressures of 200MPa up to 100 ~ 500MPa in order to analyze the effect of removing allicin causing spicy taste and unpleasant smell of garlic under high pressure.

As shown in FIG. 1, allicin was gently removed up to 3 minutes at 100 Mpa pressure, and then rapidly decreased after 3 minutes. The allicin removal form was the same under 100Mpa and 300Mpa pressure. In the case of 500 Mpa pressure, as shown in FIG. 1, allicin is abruptly removed up to 2 minutes until about 38%, and up to 17% of the total allicin content is removed by 3 minutes, and after about 4 minutes, allicin is removed. Showed.

2) Extraction Analysis of Garlic Oil

In this experiment, using garlic which was autoclaved for 4 minutes under 500Mpa, which is 100% of allicin, which is a unique ingredient of garlic, was extracted as shown in FIG. Extraction was carried out, wherein the thiosulfate content was 179,92 μmol / g, and the oleoresin yield was as shown in FIG. 3.

As shown in FIG. 3, the extraction of garlic oil under the pressure of 500Mpa showed about 0.1% until 4 minutes of extraction time, and about 0.4% of the total content of garlic in 10 minutes of extraction time. In analyzing these results, 0.4% of garlic input was extracted during the extraction time of up to 10 minutes in the extraction of garlic oil using ultra-high pressure, and the overall yield was very low.

2. Ultra High Pressure Extraction Process and Organic Solvent Extraction Process

In this experiment, ultra high pressure extraction and organic solvent extraction were performed in parallel to remove the discomfort of garlic and to improve the maximum extraction yield of garlic oil. That is, to extract garlic oil, the garlic was first pulverized and then subjected to high pressure twice for 5 minutes at a pressure of 500 MPa and a temperature of 50 ° C. High-pressure garlic was again extracted through the organic solvent extraction process, centrifuged, filtered and concentrated to prepare garlic oil. The thiosulfate content of garlic oil obtained by the complex process was 197.83 μmol / g, and the yield of oleoresin was about 34.5%, which is 8 to 50% compared with the ultra high pressure extraction method or the organic solvent extraction method alone. It was shown that the yield increases over.

On the other hand, in the present invention, the extraction method of the ultra-high pressure extraction process and the organic solvent extraction process in the extraction of garlic oil was analyzed as the optimal method to analyze the quality characteristics of the garlic oil extracted by this method during storage.

In order to analyze the quality characteristics according to the storage period of the garlic oil extracted by the method of the present invention while storing the garlic extract oil for 20 days at 4 ℃ and 20 ℃ measured the thiosulfate content change at 4 days intervals and the results 6 is shown. As shown in FIG. 6, the thiosulfate content changes at 4 ° C. showed that the thiosulfate content contained in garlic oil was preserved up to about 76% compared to the initial content. However, when stored at 20 ℃ the thiosulfate content was rapidly reduced to 70% or less than the initial content from the 8th day of storage, only a small amount of thiosulfate was measured after 16 days of storage. This is consistent with the report that diallyl disulfide among thiolsulfate, an oleoresin component, is heat sensitive. This is especially similar to the previous research showing that garlic oleoresin tends to decrease slowly at lower storage temperatures and decreases rapidly at higher storage temperatures.

Therefore, the present inventors analyzed that in order to maximize the utilization of the garlic oil extracted by the complex process of the present invention, it would be reasonable to commercialize it through the formulation of capsules rather than ingesting the liquid oil itself.

3. Powdering Garlic Oil by Spray Drying

In this example, using the extracted garlic oil to prepare a capsule containing garlic oil using the blending ratio shown in Table 1. That is, as shown in Table 1, the main component was garlic oil, and the excipients were dextrin and arabic gum, and the total formulation ratio was 100%, and the recipe was composed of 10% garlic oil, 84% dextrin, and 6% arabic gum.

division Raw material name Compounding ratio (% by weight) chief ingredient Garlic oil (100%) 10 Excipient
dextrin 84 Arabian sword 6 Sum 100

To prepare garlic oil capsules based on the blending ratio as shown in Table 1, Arabic gum was first added to a dissolution tank, and purified water was added, followed by garlic oil while maintaining 60 ° C, followed by homogenization for 30 minutes. After homogenization, dextrin was added to proceed with the second homogenization, and the entire solution was filtered and spray dried with a spray dryer to prepare a capsule. At this time, the garlic oil powder reference standard was a pale yellow powder, which was prepared with a moisture content of 10% or less.

Figure 1 is a graph showing the results measured by varying the pressure to reveal the change in the content of allicin by the ultra-high pressure.

Figure 2 shows an example of the garlic oil extraction process by the ultra-high pressure method.

Figure 3 is a graph showing the change in garlic oil yield over time in 500MPa ultra high pressure conditions.

Figure 4 shows an embodiment of a process for extracting garlic oil by applying a complex process of the present invention, that is, ultra-high pressure method and organic solvent extraction method.

5 is a picture of garlic oil extracted by the complex process of the present invention.

Figure 6 is a graph showing the thiosulfinate content change of garlic oil at each storage temperature.

Figure 7 is a graph showing the oleoresin (or garlic oil) content over time when the garlic oil extraction using an organic solvent (ethanol).

8 is a graph showing thiosulfate content over time when garlic oil is extracted using an organic solvent (ethanol).

Claims (6)

In the method of extracting garlic oil, Grinding or grinding the peeled garlic; Ultra-high pressure extraction of the ground or ground garlic; And Garlic oil extraction method comprising; extracting by adding an organic solvent to the ultra-high pressure extract. In the method of extracting garlic oil, Grinding or grinding the peeled garlic; Extracting by adding an organic solvent to the ground or ground garlic; And Garlic oil extraction method comprising the; step of extracting the ultra-high pressure of the extract. The method according to claim 1 or 2, Garlic oil extraction method characterized in that the ultra-high pressure extraction proceeds in the range of 100 ~ 2,000MPa. The method according to claim 1 or 2, The organic solvent is a garlic oil extraction method, characterized in that at least one selected from the group consisting of ethanol, methanol, propanol, butanol, ethanol aqueous solution, aqueous methanol solution, ethyl acetate, chloroform and hexane. Garlic oil extracted by the method of any one of claims 1 to 4, the content of the allicin 20% by weight or less based on 100% by weight of raw garlic allicin. Garlic oil capsules extracted by the method of any one of claims 1 to 4, prepared by adding a food or acceptable carrier or excipient to garlic oil having an allicin content of 20% by weight or less based on 100% by weight of raw garlic allicin.

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