KR100682622B1 - A preparation method of grape seed oil and tea with high quality using organically grown grapesVitis vinifera L. - Google Patents

Abstract

The present invention relates to a method for producing high quality grape seed oil and grape seed tea from grape seeds obtained as processed by-products from organic grapes, and roasted and dried dry organic grape seeds and milked with a mechanical press to feed the grape seed oil and oil cake. Grape seed crude oil was naturally filtered through granular gel made of sintered stone and subjected to deodorization to produce unscented and odorless green refined grape seed oil, and the grape seed oil cake obtained above was pressurized and expanded after treatment. It then has the outstanding effect of providing a method of making high quality grape seed tea by aging. In addition, the high-quality organic grape seed oil manufactured in the present invention can be sold as a functional food to meet the Food Code standards, and also grape seed tea has a large amount of anti-cancer, antihypertensive and antioxidant unsaturated fatty acids, phytosterols, tocophenols and catechin compounds. It is effective in preventing and treating cancer, heart disease, high blood pressure and aging.

     Organic Grape (Vitis vinifera L.), Grape Seed, Grape Seed Oil, Grape Seed Tea, Functional Ingredients

Description

A preparation method of grape seed oil and tea with high quality using organically grown grapes (Vitis vinifera L.)}

1 shows a process for producing high quality grape seed oil from organic grapes.

Figure 2 shows the manufacturing process of high quality grape seed tea from organic grapes.

The present invention relates to a method for producing high quality grape seed oil and grape seed tea useful for the prevention and treatment of cancer, hypertension, heart disease and aging from organic grapes. More specifically, the grape seed obtained from organically grown grapes is roasted, pulverized and milked with a mechanical press to obtain grape seed crude oil and oil cake, and the grape seed crude oil is naturally filtered through a granular gel made of water stone and deodorized. Through the manufacture of unflavored and odorless green refined grape seed oil, the grape seed oil cake obtained from the above is directed to a method for producing high quality grape seed tea by drying after pressure expansion and then ripening.

Recently, as the environmental pollution is accelerating due to the rapid development of the industrial society, and the stability of chemical synthetic additives is increased due to the increased consumption of convenience foods and convenience foods, consumer preference for natural foods and health foods is increasing. In particular, the consumption of organic foods produced without using any pesticides and chemical fertilizers in the well-being boom in all areas of consciousness is increasing.

Grapes ( Vitis vinifera L.) are deciduous vines belonging to the Rhamnales family, Vitaceae , with about 700 species of 11 genera in the world, mainly in tropical and subtropical regions, and some even in temperate regions. It is. Grapes are one of the most cultivated fruits of temperate fruit, producing about 58 million tons in about 4.6 million ha, almost the size of South Korea as of 2003 (FAO, 2000). On the other hand, as of 2003, grape production in Korea was 376,430 MT, which is the second largest fruit after citrus fruits, mainly the Campbell Early varieties, Vitis labrusca L., followed by Geobong and Sha. Sheridan and other hybrids ( Vitis labruscana B.) are being cultivated. Domestic grapes are produced in Yeongcheon, Gyeongsan, Gimcheon, Sangju and Chungbuk in Yeongcheon, Gyeongsangbuk-do, and are also grown in Gyeonggi, Chungnam and Gangwon.

Not only does grapes contain sugars, organic acids and unique scents, but the skin contains anti-cancer, antihypertensive and anti-cancer pigments, phenolic acids, flavonoids (flavonols. Flavan-3-ols, and flavanonols), and resveratrol. Containing antioxidant polyphenolic compounds, the consumption of various processed foods such as grape juice, grape juice, wine and grape vinegar has increased significantly.

Grape seeds account for about 3-5% of the weight of grapes and contain large amounts of dietary fiber (about 45%) such as fat (9-12%), protein (8-12%) and hemicellulose, as well as Ca, Mg And a high content of minerals such as P. In addition, grape seed contains a large amount of anti-cancer, antihypertensive, and antioxidant catechin compounds, as well as vegetable sterols and tocophenols. Currently, grape seed oil and extracts are widely used as functional foods, cosmetics, and pharmaceuticals in many countries (Kinsella, JE, Food Technol. 28: 58-60, 1974; Kinsella, JE, Cosme.Toiletries 91: 19-24, 1976; Ricardo da Silva, JM, Rigaud, J., Cheynier, V., Cheminat, A. and Moutounet , M., Phytochemistry 30: 1259-1264, 1991).

On the other hand, as a method of extracting oil contained in plant seeds, there are a compression method of compressing and milking after heat treatment, a solvent extraction method using a solvent such as normal-hexane, and a supercritical fluid extraction method using a gas such as carbon dioxide. Conventional pressing is a method of extracting oil by continually applying a constant pressure with a compress or milker after roasting the plant seeds at a suitable temperature and time condition. Many of the functional ingredients can be extracted at the same time, and the production costs are low, so it is often used to extract oil from oil-containing plant seeds such as sesame and perilla. However, not only the oil yield is very low in the production of plant seed oil by the pressing method, but also the generation of heat due to roasting or pressing and the occurrence of rancidity of the vegetable oil due to the contact of oxygen can occur easily. It is difficult to produce high quality vegetable oils in large quantities because they can be altered during production, resulting in an undesirable off flavor. Next, the solvent extraction method using normal-hexane has the advantage that the oil yield is very high compared to the compression method because the solvent extraction method using a solvent, the change in the quality of the oil that can occur during the compression process hardly occurs, and the solvent can be used continuously. . However, cumbersome refining process such as degumming, deacidification, decolorization, deodorization and deodorization to remove gums, lower fatty acids, pigments and scents present with fats in the extracted vegetable oil and to maintain the normal-hexane, which is toxic, is below the acceptable level. And expensive equipment accordingly. The supercritical fluid extraction method using carbon dioxide is easy to extract oil by controlling only the pressure (100 ~ 800 atm) and the temperature (20 ~ 80 ℃) which is safe and does not use solvents. That's how you can. In addition, the oil extraction process does not occur very hardly when the oil is contacted by high temperature and oxygen, and the extraction gas and the liquid are combined in parallel to extract oils of high purity that can effectively remove components other than oil that can be extracted at the same time. Way. However, since it is difficult to continuously put a sample into a high pressure extractor, and in particular, an expensive initial pressure such as an expensive high pressure and a gas recovery device has not been produced, the mass production of oil has not yet been carried out on a factory scale. , Hyungsul Publishing Co., p 120-125, 2002; Sovova H et al ., Chemical Engineering Science 49 (3): 415-420, 1994; Gomez AM et al ., The Chemical Engineering J. 61: 227-231, 1996; Lee et al ., Food Sci Biotechnol 9 (3): 174-178, 2000). Among these oil extraction methods, the conventional oil extraction method that compresses and milks plant seeds as they are, without the use of toxic extracting solvents such as normal-hexane in the well-being boom, has been in the spotlight. It is necessary to develop a technology for producing high quality grape seed oil from grapes.

Grape seed oil is more likely to be rancidified than other oils due to its high content of unsaturated fatty acids, but it is reported to be more stable to rancidity when heated at 180 ° C for 10 minutes than sesame oil, which is known to be stable to rancidity due to its high content of unsaturated fatty acids (Hwang et al. , Journal of the Korean Society of Food Science and Nutrition 12: 150-155, 1999) It is believed that rancidation is suppressed by antioxidants such as tocophenols and catechins in grape seeds (Jang JK, Han JY., Korean Food Science Society 34: 524-528, 2002). In addition, grapeseed oil does not have the smell and taste peculiar to oil, so that the taste of the ingredients can be kept clean after cooking. Especially, since the heating point is 250 ° C. higher than general cooking oil, food does not burn when cooked at a high temperature (S & Tech Food News No. 42. Grape Seed Oil Charm Well-being 'Holeok', Metro Newspaper, Oct. 27, 2004). Currently, grape seed oil is produced by pressing and solvent extraction methods. However, the oil recovery rate is low when milking by pressing, so it is less economical than other vegetable oils. Currently, grape seed oil is only produced in some countries, such as Italy, France, and Australia, where grape production is high. It is hardly produced in Korea. However, as the various physiological and pharmacological effects of grape seeds have become more recently known, as the grape juice and wine processing industries are activated in Korea, efficient utilization of grape seeds obtained as a by-product is greatly demanded. Especially, the Korea-FTA negotiations resulted in a crisis. In order to save the missing domestic grape farmers and cope with the price drop caused by the influx of cheap imported grapes, the development of high value-added grape seed oil and grape seed tea manufacturing technology using grape seeds obtained in large quantities as grape processing byproducts It is necessary.

To date, studies on grape seed oil have been carried out domestically and internationally, and many studies on fatty acid composition and physicochemical properties of grape seed oil and storage stability of grape seed oil have been conducted (Kinsella, JE, Food Technol. 28: 58-60, 1974; Kinsella, JE, Cosme.Toiletries 91: 19-24, 1976; Yoo JY et al ., Kor J. Food Sci Technol ., 16: 257-260, 1984; Rao PU, Food Chemistry , 50: 379-382, 1994 Kang HC et al ., Agric. Chem. Biotechnol ., 41: 578-582, 1998; Hwang JT et al ., Kor J. Food & Nutr ., 12: 150-155, 1999) For this study, Lee et al. (2000) reported a method of supercritical extraction of grape seed oil using carbon dioxide and ethanol solvents ( Food Sci Biotechnol , 9 (3): 174-178, 2000), Kang et al. (2002) A study on the improvement of the extraction method for increasing the yield of rice was reported ( Korean Journal of Food Science , 34 (5): 931- 934, 2002). In addition to the development of grape seed tea manufacturing technology using grape seeds, functional foods and cosmetics using grape seed oil and extracts have been developed (Kinsella, JE, Cosme. Toiletries 91: 19-24, 1976; Tokutake S et al ., New Food Industry 43: 1-9, 2001; Yamakoshi J & Tokutake S, Food Style 21 4: 41-44, 2002). Thus far, there have been many studies on fatty acid composition, physicochemical properties and oxidative stability of grapeseed oil, while few studies have been conducted on the analysis of functional components of organic grape seeds and the development of high quality grapeseed oil and grape seed tea. It is true.

Accordingly, it is an object of the present invention to provide a method for producing high quality grape seed oil and grape seed tea having anticancer, antihypertensive, and antioxidant activity from organic grapes.

The object of the present invention is to roast the organic dry grape seed for 5 minutes, pulverized and milked for 30 minutes with a mechanical press to obtain the grape seed oil and oil cake (oil cake), respectively, the grape seed oil is obtained by supernatant obtained by natural immersion for one month After natural filtration on granular gel made of water hydrated stone, deodorization process using a steam distillation apparatus at 250 ° C. for 2 hours produces high quality grape seed oil. The skimmed grape seed oil cake is dried and pressurized and expanded. It was then matured to achieve high quality grape seed tea.

EMBODIMENT OF THE INVENTION Hereinafter, the structure of this invention is demonstrated concretely.

The present invention is a functional component content measuring step of the organic grape seed; A step of roasting and grinding grape seeds, measuring grape seed oil yield, fatty acid composition, acid value and peroxide value and chlorophyll content according to roasting and grinding; Grape seed crude milk manufacturing step according to milking; Preparing grape seed oil from grape seed crude; It is composed of a step of producing a high-quality grape seed tea by pressure swelling the previously obtained grape seed oil cake (oil cake).

The present invention provides a high quality grape seed oil production method from organic grape seeds comprising the following steps:

Roasted dry organic grape seeds for 5 minutes (grain temperature: 100 ℃, cooker temperature: 200 ℃), crushed and milked with a mechanical press for 30 minutes at 700kg / cm ² to obtain the grape seed crude oil,

The grape seed crude oil was dehydrated with granular gel made of water hydrated stone after natural immersion for 30 days in 10 ° C. and dark, and decolorization and desorption at 100 ° C. for 1 hour by adding a mixture of activated clay and activated carbon 5: 1. Headed and deodorized with steam distillation at 230 ° C. for 3 hours to obtain purified grapeseed oil.

In addition, the present invention is dried grape seed oil cake (oil cake) obtained as a byproduct in the milking step of the organic grape seed according to the high-quality grape seed oil manufacturing method for 12 hours at 50 ~ 60 ℃ and then pressurized expansion treatment at 30 ~ 40 ℃ It is characterized by providing a method for producing grape seed tea by aging for 12 hours.

Hereinafter, the specific configuration of the present invention will be described in detail with reference to Examples, but the scope of the present invention is not limited only to the following Examples.

EXAMPLE

Example 1 Preparation of High Quality Grape Seed Oil Using Organic Grapes

In order to produce high quality grape seed oil using organic grapes, we investigated the functional components of common grapes and organic grapes, and investigated the yield, unit cost, peroxide value and chlorophyll pigment content of milking grape seed oil by roasting and grinding organic grape seeds. High-quality grape seeds from organic grape seeds by investigating the effects of various minerals on the deoxidation treatment of milking grape seed crude oil, and by varying the yield and acid value and peroxide value of milking grape seed oil by steam distillation. Optimal refining conditions for oil production were established.

Experimental Example 1: Determination of Functional Contents of Organic Grape Seeds

Differences in the content of functional components (fatty acid, phytosterol, tocopherol, catechin) between normal and organic grapes were compared. To this end, organically grown Campbellly grapes and general cultivated Campbellly grapes, which are produced in Modong, Sangju, Gyeongbuk, were harvested in mid-September, and then artificially harvested grape seeds were used as grape seed oil and extract samples after washing with water.

First, 10 g of dried grape seed was extracted twice with 100 mL of a chloroform-methanol (2: 1, v / v) solution in an ultrasonic extractor at room temperature for 2 hours, filtered and concentrated under reduced pressure to obtain grapeseed oil and grapeseed skim foil. The oil was again dissolved in 10 mL of normal-hexane, filtered to remove the residue, and concentrated to obtain purified grapeseed oil. Next, the grape seed ethanol extract obtained above was repeatedly extracted with 100 mL of 80% ethanol aqueous solution for 2 hours under boiling water, filtered and concentrated under reduced pressure to obtain grape seed ethanol extract. The acid value and peroxide value of grapeseed oil were tested according to the Food Code Test (Korea Food and Drug Administration, Moonyoungsa, Seoul, 2003) .The total catechin and four catechin components of grape seed extract, together with the fatty acid composition, phytosterol and tocophenol content of grape seed oil, The content analysis of was performed according to Choi et al. (Korean Food Science Society, 35: 576-585, 2003; J. Food Sci. Nutr ., 9: 144-149, 2004).

Lab Example 1: Comparison of Grape Seed Oil Yields between Organic Grapes and Commonly Grown Grapes

The yields of grapeseed oil from organic and general grapes were compared.

Yield Comparison of Grapeseed Oil from Organic and Commonly Grown Grapes Grape seed Yield of grape seed oil (%, dry grape seed) Organic Grape Seeds 10.2 Common grape seed 8.8 All measurements were presented as average values after three repeated measurements, with standard deviations omitted for convenience. There is statistical significance ( p <0.05) between the measurements of each item.

As shown in Table 1, the yield of grape seeds obtained from organic grapes was about 10.2%, which was slightly higher than the yield of 8.8% of grape seed oil obtained from conventionally grown grapes.

Experimental Example 2: Comparison of Fatty Acid Composition of Grape Seed Oil

Table 2 shows the results of measuring the difference in fatty acid composition of grape seed oil obtained from organic and general cultivated grapes.

Comparison of Fatty Acid Composition of Grape Seed Oil from Organic and Commonly Grown Grapes Grape seed Fatty acid (Mol%) Myristic acid (C _{14: 0} ) Palmitic acid (C _{16: 0} ) Palmitoleic acid (C _{16: 1} ) Stearic acid (C _{18: 0} ) Oleic acid (C _{18: 1} ) Linoleic acid (C _{18: 2} ) Linolenic acid (C _{18: 3} ) Organic Grape Seeds - 8.65 - 2.99 19.96 67.85 0.55 Common grape seed - 8.41 - 3.02 20.24 67.83 0.50 All measurements were presented as average values after three repeated measurements, with standard deviations omitted for convenience. There is statistical significance ( p <0.05) between the measurements of each item.

As shown in Table 2, fatty acid composition of organic grape seed oil was occupied by palmitic acid (8.65%), stearic acid (2.99%), oleic acid (19.96%), linoleic acid (67.85%) and linolenic acid (0.55%). On the other hand, the fatty acid composition of grape seed oil was palmitic acid (8.41%), stearic acid (3.02%), oleic acid (20.24%), linoleic acid (67.83%) and linolenic acid (0.50%). Fatty acid composition content was found to be almost no difference.

Lab Example 3: Comparison of Phytosterol Contents of Grapeseed Oil

Table 3 shows the results of measuring the difference in phytosterol content of grapeseed oil obtained from organic and general grown grapes.

Comparison of Phytosterol Contents of Grapeseed Oil from Organic and Commonly Grown Grapes Grape seed Phytosterol (mg%, grapeseed oil) Camposterol Stigmasterol Beta-sitosterol Organic Grape Seeds 20.78 15.93 119.50 Common grape seed 20.40 15.14 116.10 All measurements were presented as average values after three repeated measurements, with standard deviations omitted for convenience. There is statistical significance ( p <0.05) between the measurements of each item.

As shown in Table 3, the phytosterol content of organic grapeseed oil is occupied by campestrol (20.78 mg%), stigmasterol (15.93 mg%), and beta-sitosterol (119.50 mg%), whereas the phytosterol content of ordinary grapeseed oil is camphorsterol. (20.40 mg%), stigmasterol (15.14 mg%), and beta-sitosterol (116.10 mg%), while the organic and regular grapeseed oils had almost the same content of campesterol and stigmasterol, but the beta-sitosterol content of organically grown grape seeds was normal. It was slightly higher than grape seeds.

Lab Example 4: Comparison of Tocopherol Contents of Grapeseed Oil

Table 4 shows the results of comparing the tocophenol contents of grapeseed oil obtained from organic and conventionally grown grapes.

Comparison of Tocophenol Contents in Grape Seed Oil from Organic and Commonly Grown Grapes Grape seed Tocopherol (mg%, grapeseed oil) Alpha-tocopherol Beta-tocopherol Gamma-Tocopherol Delta-tocopherol Organic Grape Seeds 0.78 ND ² ND ND Common grape seed T ¹ ND ND ND All measurements were presented as average values after three repeated measurements, with standard deviations omitted for convenience. ¹ T: trace (<0.1 mg%); ² ND: not detected.

As shown in Table 4, only alpha-tocophenol was detected in grape seed oil among the four tocophenols, and the alpha-tocophenol content of organic grape seed oil was 0.78 mg%, which was somewhat higher than that of general grape seed oil.

Laboratory Example 5 Comparison of Total Catechin Content in Grape Seeds

Table 5 shows the results of comparing the total catechin content of the grape seeds obtained from organic and conventionally grown grapes.

Comparison of Total Catechin Content in Grape Seeds from Organic and Commonly Grown Grapes Grape seed Total catechin content (%, dry grape seed) Organic Grape Seeds 3.36 Common grape seed 3.29 All measurements were taken as average after 3 repeated measurements, with standard deviation omitted for convenience. There was statistical significance ( p <0.05) between all measurements.

As shown in Table 5, the total catechin content of organic and normal grape seeds was 3.36% and 3.29%, respectively, and there was no significant difference in the total catechin content according to the cultivation method.

Lab Example 6: Comparison of Four Catechin Compositions of Grape Seeds

The results of comparing the four catechin compositions of grape seeds obtained from organic and general grown grapes are shown in Table 6.

Comparison of Four Catechin Compositions of Grape Seeds from Organic and Commonly Grown Grapes Grape seed Catechin Compounds (%, Dried Grape Seed) (+)-Catechin Procyanidin B ₂ (-)-Epicatechin (-)-Epicatechin gallate Total Catechin Organic Grape Seeds 0.286 0.034 0.286 0.021 0.627 Common grape seed 0.285 0.025 0.276 0.015 0.601 All measurements were taken as average after 3 repeated measurements, with standard deviation omitted for convenience. There was statistical significance ( p <0.05) between all measurements.

As shown in Table 6, the contents of the four catechin compounds of organic grape seed were (+)-catechin (0.286%), procyanidin B ₂ (0.034%), (-)-epicatechin (0.286%), and (-)-epicatechin. Gallate (0.021%) occupies the four catechin contents of normal grape seed, while (+)-catechin (0.285%), procyanidin B ₂ (0.025%), (-)-epicatechin (0.276%), and (- ) -Epicatechingallate (0.015%) showed that the four catechin contents of organic grape seeds were somewhat higher than those of normal grape seeds.

Taken together these results (Table 1 ~ Table 6) it can be seen that the content of the functional component of organic grape seed is somewhat higher than the general grape seed.

Experimental Example 2 Measurement of Yield, Acid Value, Peroxide Value, and Chlorophyll Pigment Content of Organic Milked Grape Seed Oil by Roasting and Grinding

The yield, acid value and peroxide value, and chlorophyll pigment content of milking grape seed oil were measured by roasting and grinding organic grape seeds. Grape seeds obtained from organic Campbell early grapes produced in Sangdong, Gyeongsangbuk-do were placed in a stir-fryer (grain temperature 100 ° C, pot temperature 200 ° C, Dongkwang hydraulic, Korea) and roasted for 1 minute, 3 minutes, 5 minutes and 10 minutes. . Next, after cooling the grape seed was cooled and pulverized about 10 mesh in a blender and put into the mold of a mechanical compactor milked for 30 minutes at 700 kg / cm ² pressure to obtain the grape seed crude oil.

The results of measuring the yield, acid value and peroxide value and content of chlorophyll pigment of organic grape seed oil according to roasting and grinding are shown in Tables 7 to 9, respectively.

Changes in Yield, Acid Value and Peroxide Value of Grape Seed Oil by Roasting Process Heat treatment Minutes Grape seed oil yield (%, dry grape seed) Acid Peroxide value Control (non heat treatment) 4.37 ± 0.37 6.3 ± 0.5 10.3 ± 1.5 stir-fry 3 3.84 ± 0.35 (87.9) * 6.4 ± 0.4 13.3 ± 1.6 5 4.75 ± 0.54 (108.7) 4.8 ± 0.3 14.5 ± 1.7 10 4.14 ± 0.31 (94.7) 10.0 ± 0.2 21.5 ± 2.4

All measurements were expressed as mean ± S.D. After three repeated measurements.

There is statistical significance ( p <0.05) between the measurements of each item.

^* % Change for control

As shown in Table 7, as the roasting time was increased from 3 minutes to 5 minutes, the yield of grapeseed oil increased and then decreased at 10 minutes. In addition, the acid value and the peroxide value did not change significantly during the roasting process for 5 minutes, but increased significantly after 10 minutes. Therefore, considering the yield of milking grape seed oil, it was found that the conditions for roasting grape seeds for 5 minutes were most appropriate.

Changes in Yield, Acid and Peroxide Values and Chlorophyll Pigment Contents of Milked Grape Seed Oil with or without Roasted Grape Seeds Grinding Yield (%, roasted grape seeds) Acid Peroxide value Chlorophyll pigment Crushed (no) 4.37 ± 0.37 6.3 ± 0.5 10.3 ± 1.5 0.04 ± 0.01 Grinding 5.43 ± 0.83 6.9 ± 0.8 18.4 ± 2.4 0.29 ± 0.03 All measurements were expressed as mean ± SD after three repeated measurements. There is statistical significance ( p <0.05) between the measurements of each item. ^* Dissolve grape seed oil (0.25 g) with normal-hexane (2 ml) and measure the absorbance at 670 nm.

As shown in Table 8, when the roasted grape seeds were milked as they were, the grape seed oil yield was 4.37%, the acid value was 6.3, the peroxide value was 10.3, and the chlorophyll pigment 0.04, respectively, but when the roasted grape seeds were ground and milked, the grape seed oil yield was 5.43%. An acid value of 6.9, a peroxide of 18.4, and a chlorophyll pigment 0.29 were shown respectively. As the roasted grape seeds were pulverized, the acid value and peroxide value of grape seed oil increased, but the yield of grape seed oil and the content of chlorophyll, which is an indicator of quality of grape seed oil, increased significantly.

Changes in Fatty Acid, Phytosterol and Tocophenol Contents of Milked Grape Seed Oil with or without Roasted Grape Seeds Grinding Fatty acid (mol%) Phytosterol (mg%, grapeseed oil) Alpha-Tocophenol (mg%, Grapeseed Oil) Mry. C ₁₄ Pal. C ₁₆ Stea. C ₁₈ Olei C _{18: 1} Linolei C _{18: 2} Linolen C _{18: 3} Camposterol Stigmasterol Beta-sitosterol radish 0.1 ± 0.1 10.2 ± 0.8 3.0 ± 0.1 22.5 ± 0.1 64.0 ± 0.9 0.4 ± 0.1 12.43 ± 1.53 10.32 ± 1.63 74.03 ± 3.65 ND * U 0.1 ± 0.1 10.4 ± 0.8 3.1 ± 0.1 21.5 ± 0.1 62.0 ± 0.9 0.3 ± 0.1 15.33 ± 2.24 12.12 ± 1.92 89.45 ± 4.25 0.021 ± 0.002 All measurements were expressed as mean ± SD after three repeated measurements. There is statistical significance ( p <0.05) between the measurements of each item. ^* Not detected

As shown in Table 9, the content of fatty acid composition was not significantly different from that of the non-crushed grapes, as the roasted grape seeds were ground and milked. As a result of the above (Table 8 & Table 9), it can be seen that by crushing and milking the roasted grape seeds can produce a high quality grape seed oil.

Experimental Example 3: Deoxidation Effect of Milked Grape Seed Crude Oil by Various Minerals

In order to set the optimum deoxidation conditions for the removal of free fatty acids in the crude grape seed oil obtained by milking from organic grapes, various mineral types (pigmentation) were developed to develop physical treatment methods suitable for organic grapes instead of chemical treatment with alkalis. Chemistry, Pohang, Korea) and the change of yield, acid value and peroxide value of grape seed crude oil according to the treatment concentration are shown in Table 10 and Table 11, respectively.

Changes in Oil Yield, Acid Value and Peroxide Value of Grape Seed Crude Oil (20 g) by Various Minerals Mineral Throughput (g) Oil yield (%) Acid value (AV) Peroxide Value (POV) Control 100 6.9 ± 0.8 18.4 ± 2.4 Zeolite C-100 10 92.5 ± 2.3 6.4 ± 0.7 19.5 ± 3.3 Zeolite C-200 10 92.4 ± 2.8 6.5 ± 0.6 18.2 ± 4.1 Zeolite Figurine 10 92.2 ± 2.9 6.4 ± 0.5 18.4 ± 2.3 Zeolite Figurine I 10 90.4 ± 2.8 6.6 ± 0.4 18.1 ± 2.8 Haeposeok SP-325 2 81.3 ± 2.3 6.5 ± 0.6 17.5 ± 2.5 Meteorite SS-80 2 80.7 ± 2.5 6.4 ± 0.6 17.9 ± 2.1 Swimming Stone FRM-400 2 78.3 ± 2.2 2.5 ± 0.4 15.7 ± 1.9 Seprolite 10 91.4 ± 3.2 6.5 ± 0.7 18.1 ± 3.2 All measurements were expressed as mean ± SD after three repeated measurements. There is statistical significance ( p <0.05) between the measurements of each item.

As shown in Table 10, the yield, acid value and peroxide value of the supernatant crude oil obtained by pulverizing the roasted grape seeds and milking the grape seed crude obtained by milking each mineral, stirring at room temperature for 2 hours and centrifuging (5,000 rpm, 30 minutes) The results showed that the oil yield of the eight minerals decreased to 78%, but the acid value was 2.5, which was significantly lower than that of the control 6.9, and the peroxide value decreased from 18.4 to 15.7. While the effect was large, the deoxidation effect of the other seven minerals was hardly observed. Thus, it was found that Slugstone FRM-400 is most suitable as a deoxidizer for milking grape seed milk.

Changes in Yield, Acid Value and Peroxide Value of Milking Grape Seed Crude Oil According to the Concentration of Shrinkstone FRM-400 on Deoxidation of Grape Seed Crude Oil (100 g) Throughput (g) Oil yield (%) Acid value (AV) Peroxide Value (POV) Control 100 6.9 ± 0.8 18.4 ± 2.4 5 81.5 ± 2.3 6.0 ± 0.5 18.0 ± 2.7 10 78.4 ± 2.0 2.5 ± 0.4 18.0 ± 3.5 15 74.6 ± 1.6 1.9 ± 0.2 18.1 ± 2.7 20 72.1 ± 1.9 1.5 ± 0.3 18.1 ± 2.5 25 72.0 ± 1.5 0.7 ± 0.2 18.2 ± 2.3 All measurements were expressed as mean ± SD after three repeated measurements. There is statistical significance ( p <0.05) between the measurements of each item.

As shown in Table 11, as a result of examining the deoxidation effect of hydrolyzed stone FRM-400 with excellent deoxidation effect of milking grape seed crude oil, the yield of oil decreased slightly as the concentration increased from 5% to 25%. However, the acid value, which is an indicator of rancidity of oil, decreased from 10% (for milking milk) from 6.9 to 2.5, especially at 25% of the treated concentration. As such, it was found that the optimal deoxidation concentration of milking grape seed crude milk by Slugstone FRM-400 was about 10-25% most suitable for grape seed crude oil.

Experimental Example 4 Measurement of Changes in Oil Yield, Acid Value and Peroxide Value According to Deodorization Treatment Temperature of Milked Grape Seed Oil by Steam Distillation

previously In order to set the optimum deodorization condition to remove not only free fatty acids and pigments, but also odors and odors, which are contained in the deoxidized milking grape seed oil, by temperature (220 ~ 250 ℃, pressure 3 ~ 5mmHg) Hereinafter, the results of measuring changes in yield, acid value and peroxide value of grape seed crude oil are shown in Table 12.

Changes in Oil Yield, Acid and Peroxide Values According to the Deodorizing Temperature of Milked Grape Seed Oil by Steam Distillation Steam distillation treatment temperature (℃) Oil yield (%) Acid value (AV) Peroxide Value (POV) Control 100 0.7 ± 0.2 18.2 ± 2.3 200 98.4 ± 1.5 0.7 ± 0.1 16.0 ± 1.3 210 98.3 ± 1.3 0.7 ± 0.1 12.4 ± 1.6 220 97.2 ± 1.6 0.7 ± 0.2 10.2 ± 1.7 230 97.0 ± 1.0 0.5 ± 0.1 5.7 ± 1.1 240 93.5 ± 1.5 0.5 ± 0.2 2.5 ± 0.5 250 92.6 ± 2.0 0.2 ± 0.1 2.0 ± 0.3 All measurements were expressed as mean ± SD after three repeated measurements. There is statistical significance ( p <0.05) between the measurements of each item.

As shown in Table 12, the acid value and peroxide value of the grape seed crude oil before deodorization treatment was 0.7 and 18.2, respectively, but the yield of grape seed oil gradually decreased with increasing the deodorization treatment temperature, especially at 240 ° C. The acid value did not change significantly with the increase of treatment temperature, but the peroxide value decreased slightly from 18.2 to 10.2 at 220 ℃ and then significantly decreased from 230 ℃ to 5.7 and then slightly decreased with increasing temperature. Thus, considering the oil yield, the deodorizing treatment temperature of milking grape seed oil by steam distillation was found to be the most suitable 230 ℃.

Experimental Example 5 Measurement of Changes in Oil Yield, Acid Value and Peroxide Value According to Deodorization Treatment Time of Milked Grape Seed Oil by Steam Distillation

To set the optimum deodorization condition, the steam distillation (temperature; 230 ℃, pressure: 3 ~ 5 mmHg or less) hourly (1 ~ 5 hours) the milk yield, acid value and peroxide value were measured. .

Changes in Oil Yield, Acid Value and Peroxide Value According to Deodorization Treatment Time of Milked Grape Seed Oil by Steam Distillation Steam distillation treatment time (hours) Oil yield (%) Oil yield (%) Peroxide Value (POV) Control 100 0.7 ± 0.2 18.2 ± 2.3 One 98.3 ± 2.4 0.6 ± 0.2 10.4 ± 2.5 2 97.0 ± 2.7 0.5 ± 0.2 5.7 ± 1.3 3 96.2 ± 2.4 0.3 ± 0.1 2.5 ± 0.8 4 92.3 ± 1.9 0.3 ± 0.1 1.7 ± 0.8 5 90.7 ± 2.0 0.1 ± 0.1 1.2 ± 0.3 All measurements were expressed as mean ± SD after three repeated measurements. There is statistical significance ( p <0.05) between the measurements of each item.

As shown in Table 13, the acid value and peroxide value of the milking grape seed oil before deodorization treatment were 0.7 and 18.2, respectively, but as the deodorization treatment time was increased at 230 ° C., the acid value and the peroxide value decreased simultaneously and lowered to 0.3 and 2.5, respectively. However, after 3 hours of treatment, the acid value and peroxide value of grape seed oil were slightly lower than those of 3 hours, but the oil yield was slightly lower. Therefore, the deodorizing treatment time of the deoxidized milking grape seed oil by steam distillation was found to be the most appropriate at 3 hours at 230 ° C.

Preparation Example 1 Preparation of High Quality Refined Grape Seed Oil from Organic Grape Seeds

1 shows a high quality grape seed oil manufacturing process from organic grape seeds based on the milking grape seed crude oil refining process established above. In more detail,

Dry organic grape seeds (100kg, 10% moisture content) are roasted for 5 minutes in a fryer (grain temperature 100 ℃, pot temperature 200 ℃), crushed into a grinder with 30-50 mesh, and put into a mechanical press into 700 kg / cm ² . Milking for 30 minutes yielded grape seed crude (500-600 g). Next, grape seed crude oil was naturally immersed in a low temperature (10 ° C.) cow for 30 days, and then the obtained supernatant was passed through granular gel (20 kg) made of water hydrated stone to obtain partially purified grape seed oil. 5 kg of solid clay mixed with activated clay-activated carbon (5: 1) was added thereto, followed by decolorization and deodorization treatment under reduced pressure (50 mmHg or less) at 90-100 ° C. for 1 hour, followed by filtration under reduced pressure to obtain grapeseed oil. Finally, using steam distillation apparatus to steam grapeseed oil, steam distillation at 230 ° C. under reduced pressure (3 to 5 mmHg or less) for 3 hours to completely remove traces of saturated fatty acids and excess already and off-flavor. Purified grape seed oil (2.0-2.5 kg) was prepared.

Experimental Example 6: Physicochemical Properties of Refined Organic Grape Seed Oil

Physicochemical properties of purified organic grape seed oil prepared in Preparation Example 1, ie, grape seed oil properties, linoleic acid, catechin content, acid value, peroxide value and the presence of E. coli are shown in Table 14.

Physicochemical Properties of Refined Organic Grape Seed Oil Physical and chemical properties Grapeseed oil Property It has its own light green color and flavor and no smell Linoleic Acid (%) 68.9 Catechin (mg / 100 g) ¹ 343.72 Acid 0.2 Peroxide value 2.5 Coliform group ² voice ¹ Measured by vanillin colorimetric spectroscopy on food scale. ^{2 The} medium used was E coli. Analytical petrifilm (3M, USA) was used, the incubation time was 2 days, incubation temperature 33 ℃.

As shown in Table 14, refined organic grapeseed oil has an inherent pale green color and flavor and has no off-flavor. The linoleic acid content of grapeseed oil was 68.9, the catechin content was 343.72 mg%, the acid value and peroxide value were 0.2 and 2.5 and E. coli was negative, respectively. The physicochemical quality characteristics of the organic grape seed oil refined in this way was found to be in compliance with the grape seed oil food standard established in the current Food Code.

Example 2: Preparation of High Quality Grape Seed Tea from Organic Grape Seeds

2 shows a manufacturing process of high quality grape seed tea from organic grape seeds.

In detail, high-quality grape seed tea was prepared as shown in FIG. 2 using a grape seed oil cake obtained as a by-product of manufacturing organic purified grape seed oil. Grape seed oil (93 kg) was first dried overnight in a drying chamber (50 ~ 60 ℃), and then 4 kg of this was put in a pressure bulge was subjected to pressure expansion for 0.4 minutes at 0.4 mmHg. Next, it was allowed to cool overnight again in a low temperature (10 ° C.) cow and then aged at 30-40 ° C. for 12 hours to prepare high quality grape seed tea (88 kg).

Experimental Example 1: Determination of total catechin and four catechin compositions

The results of measuring the total catechin and the content of the four catechin compositions, which are indicators of the functional components of the grape seeds contained in the grape seed tea prepared above are shown in Tables 15 and 16.

Total Catechin Content in Organic Grape Seed Tea extract Yield (%, grape seed tea) Total catechin content (%, grape seed tea) Water extract 6.93 ± 0.17 1.83 ± 0.53 20% Ethanol Extract 7.02 ± 0.25 1.94 ± 0.83 80% Ethanol Extract 7.34 ± 0.39 2.52 ± 1.24 All measurements were expressed as mean ± SD after three repeated measurements. There is statistical significance ( p <0.05) between the measurements of each item.

As shown in Table 15, the yields of water, 20% ethanol and 80% ethanol extract of grape seed tea were 6.93%, 7.02% and 7.34%, respectively. On the other hand, the total catechin content of grape seed tea was 1.83% for water extract, 1.94% for 20% ethanol extract and 2.52% for 80% ethanol extract. The total catechin content of was higher than that of water extract and 20% ethanol extract.

Contents of the Four Main Catechin Constituents in Organic Grape Seed Tea extract Catechins (% Grape Seed Tea) (+)-Catechin Procyanidin B ₂ (-)-Epicatechin (-)-Epicatechin gallate Total Water extract 0.503 ± 0.025 0.034 ± 0.022 0.433 ± 0.063 0.013 ± 0.009 0.983 ± 0.021 20% Ethanol Extract 0.523 ± 0.032 0.036 ± 0.012 0.452 ± 0.033 0.015 ± 0.007 1.026 ± 0.033 80% Ethanol Extract 0.532 ± 0.025 0.042 ± 0.043 0.464 ± 0.032 0.021 ± 0.010 1.059 ± 0.035 All measurements were expressed as mean ± SD after three repeated measurements. There is statistical significance ( p <0.05) between the measurements of each component.

As shown in Table 16, the contents of the four main catechin components of the water extract of grape seed tea were (+)-catechin 0.503%, procyanidin B ₂ 0.034%, (-)-epicatechin 0.433% and (-)-epicatechin gallate. The content of 20% ethanol extract was 0.523% of (+)-catechin, 0.036% of procyanidin B ₂ , 0.452% of (-)-epicatechin and 0.015% of (-)-epicatechin gallate and 80% of ethanol extract. Silver (+)-catechin 0.532%, procyanidin B ₂ 0.042%, (-)-epicatechin 0.464%, and (-)-epicatechin gallate 0.021%, compared to the water extract in ethanol extract than (+)-catechin and (+)-epicatechin. The contents were high and the other two catechin contents were almost similar.

Experimental Example 2: Physicochemical Quality Characteristics of Organic Grape Seed Tea

Various physicochemical properties such as the yield, pH, sugar content, acidity, color, taste, and total catechin content of grape seed tea (10 g of grape seed tea prepared in organic grape seed and boiled in 1,000 mL of boiling water and then cooled for 3 minutes) The investigated results are shown in Table 17.

Physicochemical Properties of Organic Grape Seed Teas Physicochemical Quality Characteristics yield(%) pH ¹ Sugar content ² PH ³ Chromaticity ⁴ Total catechins (%) flavor L a b 0.75 ± 0.15 5.44 ± 0.06 0.85 ± 0.03 0.38 ± 0.01 84.34 ± 2.43 5.63 ± 0.32 24.05 ± 1.67 1.49 ± 0.09 Fresh and weak bitter taste All measurements were expressed as mean ± SD after three repeated measurements. ¹ Filter the sample and measure with a pH meter (Mettler Toledo, China). ² Measured by refractometer (Attago, Japan). ³ Converted to citric acid from 0.01 N NaOH mL water consumed up to pH 8.2 by neutralization titration method. Measured with a ^four- color difference meter (Color JC 801, Color Techno System Co., Ltd., Japan), represented by L (lightness), a (redness) and b (yellowness). ⁵ Measured by Vanillin colorimetric method.

As shown in Table 17, the yield of organic grape seed tea boiled in water was 0.75%, pH was 5.44, sugar was 0.85, acidity was 0.38, chromaticity was L = 84.34, a = 5.63 and b = 24.05, and total catechin content was 1.49. % And tastes delicious and weak astringent taste. Therefore, grape seed tea was found to be suitable as a favorite drink like Sung Soong.

From the above results, in order to manufacture high quality grape seed oil and grape seed tea from organic grapes, first of all, the functional components of grape seeds obtained from organic grapes and general grapes were analyzed, and the quality of organic grape seeds was confirmed. After measuring the change in the functional components of the grape seed according to the roasting treatment condition was set as the optimum processing method for 5 minutes, and extracting the roasted grape seeds with a mechanical press to obtain the grape seed oil and skim oil cake (oil cake), respectively The grape seed crude oil was deoxidized with water hydrated stone and deodorized with a steam distillation apparatus to produce purified grape seed oil. Also, the grape seed oil was dried and dried under pressure and expanded to mature, and then developed high quality grape seed tea. Grape seed oil and grape seed tea contain anti-cancer, antihypertensive, antioxidant and anti-aging unsaturated fatty acids, phytosterols, tocophenols and catechins and are expected to attract attention as a functional health food that can prevent cancer, heart disease, high blood pressure and aging.

As described in the above Examples and Experimental Examples, the present invention relates to a method for producing high quality grape seed oil and grape seed tea from grape seeds obtained as processed by-products from organic grapes, and the present invention relates to grape seed obtained as processed by-products from organic grapes. The present invention relates to a method for producing high quality grape seed oil and grape seed tea, which is roasted and ground by drying organic grape seeds, milked with a mechanical press to obtain grape seed oil and oil cake, and the grape seed oil is granular Naturally filtered through gel to deodorize to produce an unflavored and odorless green refined grape seed oil, and the grape seed oil cake obtained above is dried after pressure swelling and matured to produce high quality grape seed tea. Has an excellent effect. In addition, the high-quality organic grape seed oil prepared in the present invention can be sold as a functional food to meet the Food Code standards, and the grape seed tea is relatively anti-cancer, antihypertensive and antioxidant unsaturated fatty acids, phytosterol, tocophenol and catechin compound It is expected to be used as a functional food that can prevent cancer, heart disease, high blood pressure and aging due to its large amount.

Claims (2)

Dry organic grape seeds were roasted for 5 minutes in a roaster with a grape seed temperature of 100 ° C. and a cooker temperature of 200 ° C. for 5 minutes, and milked at 700 kg / cm ² for 30 minutes using a mechanical press to obtain crude grape seed oil. The grape seed crude oil was dehydrated with granular gel made of water hydrated stone after natural immersion for 30 days in 10 ° C. and dark, and decolorization and desorption at 100 ° C. for 1 hour by adding a mixture of activated clay and activated carbon 5: 1. And deodorizing at 230 ° C. for 3 hours with steam distillation to obtain purified grape seed oil. Grape seed oil cake obtained as a byproduct in the milking step of the organic grape seed according to claim 1 was dried at 50 to 60 ℃ for 12 hours and then subjected to pressure swelling and aged at 30 to 40 ℃ for 12 hours to prepare grape seed tea. Method for producing a high quality organic grape seed tea, characterized in that it comprises a step.

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