KR20080069284A - Development of lycopene recovery by supercritical carbon dioxide extraction - Google Patents

Abstract

A method for preparing a lycopene concentrated extract is provided to isolate lycopene without destruction from watermelon with high concentration, high yield and stability using supercritical CO2, thereby the recovered lycopene being utilized into various kinds of food products. A method for preparing a lycopene concentrated extract comprises the steps of: (a) after crushing watermelon flesh using a chopper, a colloid mill and a homogenizer in sequence, centrifuging the crushed flesh and storing cake and serum, separately; and (b) preparing the lycopene concentrated extract from lipophilized watermelon cake or a wet-state watermelon cake using supercritical CO2. Another method for preparing a lycopene concentrated extract comprises the steps of: (a) extracting lycopene from a wet-stage watermelon sample using a fatty acid ethyl ester of coconut oil as an entraciner and using supercritical CO2; and (b) preparing the lycopene concentrated extract from the lycopene extract obtained from the step(a) under the pressure of 1,600 psi and the temperature of 50 deg.C.

Description

Development of lycopene recovery by supercritical carbon dioxide extraction

Figure 1a is a photomicrograph before and after the grinding of the watermelon flesh, Figure 1b is a photograph after 24 hours storage at 4 ℃ after grinding, Figure 1c is a photograph of a cake separated by centrifugation.

Figure 2 is a graph showing the lycopene content according to the storage period and storage temperature of the watermelon cake for each stage of grinding.

3 is a perspective view showing a system for supercritical carbon dioxide extraction of the present invention.

Figure 4 is a graph showing the lycopene content of the extract at 1600 psi and 40 ℃ conditions in supercritical carbon dioxide extraction conditions.

The present invention separates lycopene, an antioxidant component from watermelon, in a method having high concentration, high yield and stability, and extracts an active ingredient (Lycopenene, lycopene) from the watermelon pulp without using supercritical carbon dioxide fluid. It relates to a method for producing an extract lycopene finally concentrated and to an extract thereof.

Lycopene is an antioxidant known mainly as a pigment component of tomatoes, a kind of carotenoids. In addition to tomatoes, it is also found in watermelons and persimmons. It is well known that lycopene has antioxidant activity that can effectively defend against free radicals that damage cells. Together with vitamins E, C and other compounds as antioxidants and free radical phagocytes, it plays a major role in the antioxidant mechanisms in humans and organisms. Lycopene has also been demonstrated to cooperate with low density lipoproteins that reduce the oxidation of cholesterol and other lipids and thus prevent blood vessel damage and further demonstrate an inverse correlation between lycopene levels in the blood and prostate cancer.

Watermelon, which is known to be good for preventing heart disease and aging, has been reported to contain significant amounts of lycopene. However, there is no research or report on how to separate the watermelon lycopene in high concentration and high yield as it is.

Lycopene has very low oxidative stability against heat and light, so it is oxidized immediately after exposure to air and destroys about 30% of the freeze-drying process. It is also sensitive to oxygen and easily loses its usefulness during the manufacturing process. However, there have been no studies or reports on extracting lycopene from watermelon in a stable and economical way using supercritical carbon dioxide.

Therefore, an object of the present invention is to extract a high yield, high concentration of lycopene from the watermelon in an optimal manner in consideration of economics and preservation, and to provide a natural antioxidant lycopene obtained by this and food using the same.

In order to achieve the above object, the present invention is (a) the watermelon pulp (chopper), colloid mill (colloid mill) and homogenizer (homogenizer) sequentially crushed and centrifuged cake (cake) And (b) separating and storing the lyophilized watermelon cake using supercritical carbon dioxide under 6,000 psi and 40-70 ° C. .

In addition, (a) the watermelon flesh is collected and crushed sequentially with a hopper, a colloid mill and a homogenizer, and centrifuged to separate the cake and the serum and store it. Step, (b) provides a method for producing an extract of the concentrated lycopene using a supercritical carbon dioxide in the wet state of the watermelon cake in a wet state of more than 6,000 psi and 40 ~ 70 ℃.

In addition, the present invention (a) using a non-dried watermelon sample by using a palm oil fatty acid ethyl ester as an intrainer, using supercritical carbon dioxide under conditions of 6,000 psi or more and 40 to 70 ° C. A first step of lycopene extraction, (b) the lycopene extract of the step (a) comprises a method for producing an extract of concentrated lycopene using supercritical carbon dioxide at a pressure of 1600 psi and a temperature of 50 ℃.

In addition, the present invention includes lycopene extracts, such as lycopene extracts or concentrates, which are prepared by the method described above. The foods are fruits, vegetables, dried or cut products of fruits or vegetables, fruit juices, vegetable juices, mixed juices or beverages containing acidic beverages, cookies, candies, caramels, gums, etc. Products, fermented milk products such as tea, yogurt, dairy foods, condiments, alcoholic beverages, canned or bottled foods, noodles, livestock processed foods, fish processed foods, microbial fermented foods, soybean foods, cereals, meat processed foods, licorice And herbs.

In the present invention, the cake obtained through the pulverization and centrifugation process from the watermelon flesh is a breakthrough method to obtain lycopene in a high content and a high yield, it is revealed that the optimum pretreatment process for the production of high content of lycopene.

The temperature, pressure, and extraction conditions of the supercritical carbon dioxide used in the present invention were established through continuous studies and repeated tests by the present inventors, and the technical spirit of the present invention is included within the scope of the present invention as well as the detailed numerical limitation. It will be self explanatory.

Hereinafter, the content of the present invention will be described in more detail with reference to Examples. However, these examples are only presented to understand the content of the present invention, the scope of the present invention should not be construed as being limited to these embodiments.

< Example  1: Watermelon Pretreatment and Storage Experiment>

Watermelon pulp was harvested and wet milled sequentially with chopper, colloid mill and homogenizer. As shown in Figure 1a it can be seen that the watermelon flesh structure is disassembled in a structure suitable for lycopene extraction. The pulverized lodged flesh was stored for 24 hours at refrigeration temperature and then separated into cake and serum by centrifugation at 10,000 rpm for 30 min (see FIGS. 1B and 1C).

Table 1 shows the content and concentration of lycopene through watermelon grinding and separation. It was analyzed that 807.3mg of lycopene per kg weight was concentrated in the cake prepared by watermelon pretreatment, and the recovery rate was 93.75%, proving that the watermelon pretreatment process of the present invention is a breakthrough method of concentrating lycopene in high yield and high content. Could.

[Table 1] Weight and Lycopene Yield during watermelon Pretreatment

Weight yield (Kg) conc . Lycopene (Mg / kg) Lycopene yield (Mg) Watermelon 100 - - Rind 31.5 - - Seed 0.42 - - Flesh 68.08 37.4 2546 Juice 63.08 2.83 152.42 (5.99) Cake 5.0 807.3 2387 (93.75)

< Experimental Example : Storage Experiments>

Watermelon pulp and the watermelon pulp cake prepared in Example 1 was sealed and packed with a polyethylene film bag per unit to store the content of lycopene (weekly unit) while storing at a storage temperature of 5 ℃, 0 ℃, -20 ℃ or -70 ℃ By measuring the shelf life of the watermelon flesh and cake according to the degree of grinding.

As shown in Figure 2, the lycopene content in the watermelon cake was maintained in a large significant amount during the storage period without a great influence on the storage temperature, in particular, it was found that the lycopene content is stably maintained as the lycopene content is increased sequentially. . Therefore, when the watermelon pretreatment process of the present invention separates the juice of less than 5% lycopene loss and hermetically packaged at -5 ℃ or less can be stored in a high yield and high content of lycopene showing a lycopene loss rate of less than 20% Once again it was a breakthrough.

< Example  2: from dry watermelon cake Lycopene  Extract>

From the freeze-dried watermelon cake, lycopene was extracted by the conventional supercritical extraction method under the conditions of 6000, 7500 and 9000 psi and the temperature of 40, 60 and 80 ° C. And relatively high extraction and recovery at temperatures above 60 ° C.

[Table 2] Extraction rate and recovery rate by supercritical extraction

extraction yield (%) recovery yield (%) 6000psi 40 ℃ 75.8 8.5 60 ℃ 99.7 11.9 80 ℃ 99.9 20.5 7500 psi 40 ℃ 97.9 12.1 60 ℃ 99.8 16.8 80 ℃ 99.9 21.6 9000 psi 40 ℃ 98.9 14.2 60 ℃ 99.6 18.4 80 ℃ 99.8 22.4

Lycopene has about 30% destruction during the freeze drying process because of its very low oxidation stability against heat and light. Meanwhile, lycopene was extracted from the freeze-dried watermelon sample using the supercritical carbon dioxide extracting apparatus as shown in FIG. 3. As shown in Fig. 3, soybean oil or medium-chained triglycerides (MCT) was added to the liquid extractor No. 12 as an intrainer, and the lyophilized watermelon sample was added to the solid extractor No. 13, but the extraction was performed. The extraction rate was faster but higher pressures of 6000 psi were required. At this time the temperature was carried out at 40-70 ℃. Extraction pressures of 6000 psi or more can be somewhat problematic for economics and practical use, thus inventing other pretreatment methods, such as mixing direct fats (soybean oil and MCT) with a non-wet watermelon sample.

< Example  3: not dry From watermelon Lycopene  Extract>

  -When using triglyceride form

Soybean oil or MCT was added as an entrainer to extract lycopene directly from wet watermelon samples to prevent severe destruction of lycopene during drying, and then mixed in an ice bath using a laboratory homogenizer for 2 minutes. As a result, about 80% of lycopene was transferred from wet samples to soybean oil and MCTs used as entrainers. The above extracts are also in triglyceride form and therefore require a pressure of over 6,000 psi as in the case of using dried samples, and have a high energy and expensive high pressure device. Accordingly, in the present invention, as an edible sample having high solubility in supercritical carbon dioxide, an extraction method using palm oil fatty acid ethyl ester, which has high solubility in supercritical state and is easy to extract even at low pressure, has been created.

 -When palm oil fatty acid ethyl ester is used

 Extraction process using wet type samples such as soybean oil and MCT was carried out using palm oil fatty acid ethyl ester, and this method was also able to obtain efficient extraction efficiency with more than 80% extraction rate. After extraction with a homogenizer, centrifugation was performed at 6,000 x g to obtain a supernatant, lycopene and palm oil ethyl ester mixture, lycopene extract.

< Example  4: Supercritical  Carbon dioxide lycopene  Thickening>

After obtaining lycopene extract (lycopene content: 0.0367%) using palm oil fatty acid ethyl ester, the extraction process was carried out at various pressures of 1400, 1600, 1800 psi and various temperatures ranging from 30 to 60 ℃. The present invention is to optimize the operating conditions to extract only fatty acid esters using supercritical carbon dioxide from the lycopene extract extracted primarily using palm oil fatty acid ethyl ester and lycopene remaining in the extractor. In this case, since the container is filled with atmospheric inert gas (CO2), oxidation is prevented when CO2 is removed, and high purity lycopene can be obtained. At each temperature range, the extraction pattern of fatty acid ester according to the amount of carbon dioxide gas used and the lowest lycopene content in the extracted fatty acid ester were established, and the pressure of 1600 psi and 50 ℃ were the most effective operating conditions.

Figure 4 shows the extraction pattern obtained by the operation under the above conditions and the content of lycopene in the extracted extract as a result of the relatively high extraction rate at 1600 psi, a very low pressure in the case of fatty acid ethyl ester, while the lycopene content in the extracted extract is very Low (0.002% or less) results were shown. On the other hand, the remaining lycopene concentrate in the extractor showed a lycopene content of 0.48%, resulting in more than 10-fold concentration. The present invention reveals that 20 to 30 times more concentrated concentrate can be obtained if the extraction process is actually carried out for a longer time. Therefore, by preparing a watermelon-derived lycopene extract of various concentrations, various types of foods containing the same (health functional food, beverages, porridge, confectionery, all other food formulations, etc.) can be developed.

The present invention separates lycopene, an antioxidant component from watermelon, in a method having high concentration, high yield and stability, and extracts an active ingredient (Lycopenene, lycopene) from the watermelon pulp without using supercritical carbon dioxide fluid. The present invention provides a method for producing natural antioxidants in high yield and high concentration, and may improve the availability of lycopene as a variety of materials recovered from watermelon. By separating lycopene, a natural antioxidant, from watermelon in its intact form, it will further increase its value as a natural material.

Claims (5)

(a) collecting watermelon flesh and sequentially crushing with a hopper, colloid mill and homogenizer and centrifuging to separate the cake and the serum and store it; (b) A method for preparing an extract of concentrated lycopene using lyophilized watermelon cake using supercritical carbon dioxide. (a) collecting watermelon flesh and sequentially crushing with a hopper, colloid mill and homogenizer and centrifuging to separate the cake and the serum and store it; (b) a method of preparing an extract of concentrated lycopene using a supercritical carbon dioxide from a watermelon cake in a wet state; (a) extracting lycopene first using supercritical carbon dioxide using a palm oil fatty acid ethyl ester as an intrainer using a non-dried watermelon sample, (b) step (a) Lycopene of the method using a supercritical carbon dioxide under pressure and temperature conditions to prepare a lycopene concentrated extract. Lycopene extract, characterized in that prepared by the method of claim 1, 2 or 3. Food containing the lycopene extract of claim 4.

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