KR100651249B1 - A preparation methods of grape seed oil and extract with high quality - Google Patents

Abstract

The present invention relates to a method for producing a high quality functional grape seed oil and extract containing an antioxidant catechin compound, which is dried by pulverizing dried grape seeds for 1 minute in a microwave and then degreased with normal-hexane to remove crude grape oil and skim. Grape seed milk is obtained respectively, and grape seed crude oil is subjected to deoxidation, decoloring, and deodorization in order to produce purified grape seed oil, and skimmed grape seed cake is boiled with ethanol solution, filtered and concentrated to obtain grape seed ethanol extract, which is again subjected to ion resin adsorption chromatography. The grape seed extract obtained by concentrating the extract eluted in 20% and 60% ethanol aqueous solution using a graphography contains a large amount of antioxidant catechin compound, which is excellent in preventing and treating cancer, heart disease, high blood pressure and aging.

Grape Seed, Grape Seed Oil, Grape Seed Extract, Catechin Compound

Description

A preparation methods of grape seed oil and extract with high quality

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

Figure 2 shows a process for producing a high quality grape seed extract for functional food manufacturing raw materials from grape seeds.

Figure 3 shows a process for producing a high quality grape seed extract for the production of functional cosmetics from grape seeds.

The present invention relates to a process for producing high quality grape seed oil and grape seed extract. More specifically, the present invention is obtained by pulverizing the dried grape seed, heat treatment in a microwave oven, degreasing to obtain the crude grape seed milk and skim grape seed cake, through the deoxidation, decolorization and deodorization process from the crude grape seed oil to produce purified grape seed oil And a method for producing a catechin derivative-containing high quality grape seed extract by obtaining grape seed ethanol extract from skim grape seed cake and performing ion resin adsorption chromatography.

Recently, due to the rapid development of industrial pollution and the rapid transformation of dietary patterns into Westernization, meat consumption has increased significantly, and chronic degenerative diseases such as cancer, heart disease, hypertension, arteriosclerosis, diabetes, and dementia have greatly increased. Doing. Therefore, researches are being actively conducted to develop new bioactive substances derived from natural products that can prevent such chronic diseases. Especially, by improving the defense mechanism of the living body, preventing and recovering diseases, improving immune function and suppressing aging, etc. There is a great interest in natural antioxidants having bioregulatory functions. Antioxidants not only suppress the rancidity caused by the automatic oxidation of fats and fat-containing foods, but also produce free radicals in vivo ( ¹ O ₂ , O ^- ₂ , H ₂ O ₂ , .OH As a physiologically active substance that inhibits lipid peroxidation by), it prevents cancer, arteriosclerosis, inflammation, immunodeficiency and aging. Currently, synthetic antioxidants such as butylated hydroxyanisole and butylated hydroxytoluene and natural antioxidants such as α-tocopherol and L-ascorbic acid are used in the food, cosmetic and pharmaceutical industries. Although widely used in the field of safety, such as the toxicity and carcinogenic properties of synthetic antioxidants has been an issue, the development of safer and more effective natural antioxidants are actively being made.

Grape ( Vitis vinifera ) is a deciduous vine plant belonging to the Rhamnales vine family ( Vitaceae ), and has about 700 species in 11 genera worldwide, mainly native to tropical and subtropical regions, and partly to temperate regions. . 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.

Grapes contain sugars, organic acids and unique scents, as well as anticancer, antihypertensive and antioxidant polyphenols such as anthocyanin pigments, phenolic acids, flavonoids (flavonols. Flavan-3-ols and flavanonols) and resveratrol. The compound contains a significant increase in the consumption of various processed foods, such as grape juice, wine and grape vinegar (Renauds, S. et al . Lancet 339: 1523-1526, 1992; Kanner, J. et al. J. Agric Food Chem. 42: 64-69, 1994; Frankel, EN, J. Agric Food Chem. 43: 890-894, 1995; Tanahashi, H. et al. Am. J. Enol.Vitic. 46: 405-409 , 1995).

Grape seeds, on the other hand, account for about 3 to 5 percent of the weight of grapes and may contain large amounts of dietary fiber (about 45 percent) such as fat (9 to 12 percent), protein (8 to 12 percent), and hemicellulose. In addition, the content of minerals such as Ca, Mg and P is high. In addition, grape seed contains a large amount of unsaturated fatty acids such as linoleic acid, as well as a large amount of phytosterols, tocophenols and anticancer, antihypertensive and antioxidant catechins and is widely used as a material for functional foods, cosmetics and medicines (Kinsella , JE, Food Technol. 28: 58-60, 1974; Kinsella, JE, Cosme. Toiletries 91: 19-24, 1976; Ricardo da Silva et al . Phytochemistry 30: 1259-1264, 1991).

Grape seed oil does not have the smell and taste of oil, so the taste of ingredients can be kept clean after cooking, and the heating point is 250 ℃, which is higher than general cooking oil, and it does not burn food when cooked at high temperature (S & T Food News 42 Ho. 'Grape Seed Oil' Charm of the Well-being Family 'Cho', Metro Newspaper, Oct. 27, 2004). Currently, grape seed oil is produced by pressing and solvent extraction, but the oil recovery rate is very low compared to other vegetable oils, which is economical, and is produced only in some countries such as Italy, France, and Australia, where grape production is high. 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. It is necessary to develop high value-added grape seed oil manufacturing technology using domestic grape seeds to save the missing domestic grape farmers and cope with the price plunges caused by the influx of cheap imported grapes.

Grape seed extract contains 5-20% of catechin compounds (proanthocyanidin, oligomeric and polymeric polyhydroxyflavan-3-ol units), most of which are esterified by oligomeric procyanidins and gallic acid such as dimers, trimers and specification bodies And the remaining monomeric catechins [(+)-catechin and (-)-epicatechin and (-)-epicatechin gallate] components. More than 55% of the oligomeric procyanidins are composed of polymeric procyanidins (more than five monomer units, polymerization degree 2.3-15.1 or 2.4-16.7) which have not yet been identified. It is contained. These catechin compounds contained in grape seeds have several important physiological effects such as anticancer, antimutagenic, antihepatic, antihypertensive, anti-inflammatory, antibacterial and antioxidant activity (Ricardo, JM et al . J. Agric. Food Chem. 39: 1549 -1552, 1991; Gali, HU et al. Planta Med. 60: 235-239, 1994; Tebib, K., J. Nutr. 124: 2451-2457, 1994; Bagchi, D. et al. Gen. Pharmacol. 30 (5): 771-776, 1998; Palma, M. et al. J. Agric.Food Chem. 47: 5044-5048, 1999; Koga, T. et al. J. Agric.Food Chem. 47: 1892 -1897, 1999; Yamaguchi, F. et al . J. Agric. Food Chem. 47: 2544-2548, 1999; Zhao, J., Carcinogenesis 20 (9): 1737-1745, 1999; Yamakoshi, J. et al Atherosclerosis 142: 139-149, 1999; Koga, T. et al. J. Agric. Food Chem. 47: 1892-1897, 1999; Castillo, J. et al. J. Agric. Food Chem. 48: 1738- 1745, 2000; Shirataki, Y. et al. , Anticancer Res. 20: 423-426, 2000; Fitzpatrick, DF et al . J. Agric.Food Chem. 48: 6384-6390, 2000; Sen, CK and Bagchi, D., Mol Cell Biochem 215:. . not 1-7, 2001) And not only as anti-peptic ulcer (Saito, M. et al J. Agric Food Chem 46:... 1460-1464, 1998), skin whitening (Yamakoshi J & Tokutake S., Food Style 21 6 (12): 41 -44, 2002), and eye retinal protective action (Yamakoshi, J. et al . J. Agric. Food Chem. 50: 4983-4988, 2002) and other useful microbial proliferation effects (Tebib, K. et al . Nutrition Res. 16 (1): 105-110, 1996) and are currently available in the United States, Europe, Japan, Australia, It is widely used as a dietary supplement and functional cosmetics in Korea and abroad (Tokutake S & Yamakoshi J, New Food Industry 43 (11): 1-9, 2001).

On the other hand, the catechins of grape seed extract not only have a bitter taste and bitter taste, but also easily change color to blackish brown by chemical and enzymatic browning reaction during processing and storage, thus adversely affecting the quality. (Oszmianski, J. et al . J. Food Sci. 50: 1505-1506, 1985; Romeyer, FM et al . Phytochemistry 25: 219-221, 1986; Robichaud, JL and Noble, AC, J. Sci. Food Agric. 53: 343-353, 1990). Therefore, it is necessary to develop a new high-quality grape seed extract manufacturing technology that can improve the bad taste and minimize the quality change of catechin components during processing while maintaining the excellent physiological activity of the grape seed extract.

To date, as a study on the manufacturing technology of grape seed extract, Ricardo da Silva et al. ( Phytochemistry 30: 1259-1264, 1991; J. Agric. Food Chem. 45: 1156-1160, 1997) polyamide column chromatography Has been reported to purely separate catechin and procyanidin components from methanol extracts of grape seeds, and Kalhithraka et al. ( Phytochemical Analysis 6: 265-267, 1995) reported that the optimum solvent conditions for the extraction of phenolic grape seeds were investigated. Has been investigated. See also Kovacer et al. ( Contempory Agric . 39: 5-17, 1991), Castillo et al. ( J. Agric. Food Chem. 48: 1738-1745, 2000) and Takashi et al. ( J. Agric. Food Chem. 50: 1254- 1259, 2002) reported the use of an ionic resin such as Amberlite XAD-7 to effectively separate catechin and procyanidin components from grape seeds, as well as similar research reports (Kikkoman Co, Japan; Yuda Chemical Co., Ltd., Japan Patent Publication). Japanese Unexamined Patent Publication No. 2001-292731; Whiprowpdir Co., Ltd., Japanese Unexamined Patent Publication No. 2000-125823; Haitai Confectionery Co., Ltd., Korean Unexamined Patent Publication No. 2000-0037080). In addition, in order to improve the bitter taste of grape seed extract, fermentation engineering technology has been actively developed using enzyme treatment such as tannase or yeast (Food Additives, Korea Food and Drug Administration, Moonyoungsa, Seoul, pp 967). -968, 2001; Japanese Patent, 2002-10-0292731). As described above, researches on the development of manufacturing technology of grape seed extract and the development of functional foods and cosmetics using the same have been conducted, but research on the development of high quality grape seed oil manufacturing technology is very insufficient.

Accordingly, it is an object of the present invention to provide an improved method for producing high quality grape seed oil and grape seed extract having anticancer, antihypertensive and anti-aging activity.

The object of the present invention is to microwave the pulverized dry grape seed and then degreased with normal-hexane to obtain grape seed crude oil and skim grape seed cake, the grape seed crude oil is subjected to the process of deoxidation, decoloration and deodorization to produce purified grape seed oil In addition, the skim grape seed cake was dried by adding an ethanol aqueous solution, followed by extraction with hot water, followed by filtration and concentration to obtain a grape seed ethanol extract, and then using ion resin adsorption chromatography to obtain a high quality grape seed extract containing a catechin compound.

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

The present invention is a microwave treatment step of grape seed, grape seed oil and ethanol extract preparation and yield measurement step according to the microwave treatment; Measuring fatty acid composition content of grapeseed oil; Preparing purified grape seed oil from dry grape seeds; Measuring the total catechin and four catechin compounds in the grape seed extract; It consists of preparing a high quality grape seed extract containing catechin compound from skim grape seed cake.

The present invention is pulverized dry grape seed, microwave treatment for 1 minute, then degreased with normal-hexane, grape grape oil obtained by degumming (0.15% phosphoric acid), deoxidation (5% NaOH solution) and deodorization (steam distillation, 220 ℃, 2 hours, 5 mmHg) provides a process for producing high quality grape seed oil comprising the step of producing grape seed oil.

In addition, the present invention is pulverized dry grape seed for 1 minute and then microwave treatment, and then first degreasing with normal-hexane degreasing grape seed cake obtained by heating and extracting with 20% ethanol aqueous solution, filtered and concentrated to obtain a degreasing grape seed ethanol extract and ions again The present invention provides a method for preparing a high quality grape seed extract containing a catechin derivative which can be used as a raw material for preparing functional foods by eluting with 20% ethanol aqueous solution using resin adsorption chromatography.

In addition, the present invention is pulverized dry grape seed for 1 minute after microwave treatment, first degreasing with normal-hexane degreasing grape seed cake obtained by heating and extracting with 80% ethanol aqueous solution, filtered and concentrated to obtain a degreasing grape seed ethanol extract and this again ions The present invention provides a method for preparing high-quality grape seed extracts containing catechin derivatives which can be used as raw materials for functional cosmetic preparation by eluting with 60% ethanol aqueous solution using resin adsorption chromatography.

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 from Grape Seeds

In order to establish high quality grape seed oil from grape seed, the change of yields of grape seed oil and extract were measured by three heat treatments (roasting, steaming and microwave treatment) to establish the optimum processing condition of grape seed. The fatty acid composition of grapeseed oil and the catechin content of grapeseed extract were measured, and the yield change of grapeseed oil by degumming and deoxidation treatment, and the change in the yield of oilseeds with deodorization treatment temperature and time by steam distillation were measured. Grape seed oil was prepared according to the manufacturing process established therefrom and its physicochemical quality characteristics were investigated.

Experimental Example 1: Change in yield of grape seed oil and extracts by heat treatment

Grape seeds obtained from Campbell early grapes grown in Modong, Gyeongbuk, Korea were roasted (grain temperature 100 ℃, pot temperature 200 ℃, Dongkwang hydraulic, Korea) for 3 minutes, 5 minutes and 10 minutes roasting or pulverized grape seeds. After putting in a steaming pot (steaming) was steamed for 10 minutes, 30 minutes and 60 minutes. The pulverized grape seeds are placed in a microwave oven (Samsung RE-C200T, frequency 2450 MHz, pulsed variable MW power output from 90 to 700 W by a timer, inner volume 21.8 L, Samsung, Korea) for 1 minute, 3 minutes, and 5 minutes. Microwaves were processed.

To determine the yield of grape seed oil and extracts according to the three heat treatments, 10 g of dry grape seed was extracted twice with 100 mL of chloroform-methanol (2: 1, v / v) solution at an ultrasonic extractor for 2 hours at room temperature, followed by filtration and Concentrated under reduced pressure, grape seed oil was obtained, and the resultant was dissolved in 10 mL of normal-hexane, filtered to remove the residue, and concentrated to obtain partially purified grape seed oil. The grape seed skim foil obtained in the above step was repeatedly extracted twice with boiling water for 100 hours with 100 mL of 80% ethanol aqueous solution, filtered and concentrated under reduced pressure to obtain a grape seed ethanol extract.

Yield Changes of Grape Seed Oil and Extracts According to Three Heat Treatments of Grape Seeds Heat treatment Minutes Yield (%, dry grape seed) Grapeseed oil Ethanol extract Control (non heat treatment) 7.37 ± 0.53 4.50 ± 0.13 stir-fry 3 7.31 ± 0.43 (99.2) ^* 4.45 ± 0.14 (98.9) ^* 5 7.94 ± 0.64 (107.7) 4.52 ± 0.27 (100.4) 10 7.58 ± 0.28 (102.9) 4.73 ± 0.32 (105.1) Steamed 10 7.69 ± 0.34 (104.3) 4.55 ± 0.24 (101.1) 30 7.82 ± 0.41 (106.1) 4.25 ± 0.16 (94.4) 60 8.31 ± 0.54 (112.8) 3.66 ± 0.10 (81.3) microwave One 7.57 ± 0.33 (102.7) 5.26 ± 0.43 (116.9) 3 7.77 ± 0.36 (105.4) 4.94 ± 0.34 (109.8) 5 7.79 ± 0.52 (105.7) 4.88 ± 0.31 (108.4)

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 1, the yield of grapeseed oil increased by 13% and 6%, respectively, by steaming and microwave treatment, compared to the control (non-heat treatment), while the roasting treatment increased by about 8% up to 5 minutes, but slightly after 10 minutes. Decreased by about 3%.

On the other hand, the yield of the grape seed extract was increased as the treatment time was increased by 5 minutes up to 10 minutes in the roasting treatment, while the steaming treatment decreased by 19 hours and decreased by 19% until the treatment time. The microwave treatment increased about 17% until one minute of treatment, but decreased after that, and increased by 8% at five minutes of treatment.

In this way, the microwave treatment of the three different heat treatment was found to be a heat treatment process that can simultaneously increase the yield of grape seed oil and extract.

Experimental Example 2 Measurement of Fatty Acid Composition Content of Grape Seed Oil by Heating Treatment of Grape Seed Oil

After grinding 100 g of dried grape seed (20-40 mesh), 0.01% BHT (butylhydroxytoluene, Jusei Chem. Co., Ltd. Japan) and 500 mL of normal-hexane were added thereto, followed by ultrasonic cleaner (30 hours at 30 ° C). Bransonic 5210R-DTH, USA) was extracted twice, filtered and concentrated to give grape seed oil. Next, grapeseed oil (100 mg) was methylated with 10 mL of 6% H ₂ SO ₄ (in MeOH), and fatty acids were analyzed using Hewlett-Packard 6890 series, USA (GC). At this time, the column is Supelcowax ^TM -10, the column temperature is maintained at 100 ℃ (after 5 minutes → 4 ℃ / min (warm temperature) → 220 ℃ 20 minutes), the injection temperature is 250 ℃, the detector is FID (Flame Ionized Detector , 260 ℃) and N ₂ (52.5 mL / min) were used for the gas carrier. The results of measuring the fatty acid composition of grape seed oil according to three different heat treatments of grape seeds are shown in Table 2.

Changes in Fatty Acid Composition of Grape Seed Oil by Three Different Heat Treatments Heat treatment Time (min) 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} ) Control 0.1 ± 0.1 10.2 ± 0.8 0.2 ± 0.1 3.0 ± 0.1 22.5 ± 0.1 64.0 ± 0.9 0.4 ± 0.1 stir-fry 3 0.1 ± 0.0 10.5 ± 0.4 0.2 ± 0.0 3.1 ± 0.1 22.5 ± 0.4 63.2 ± 0.0 0.5 ± 0.0 5 0.1 ± 0.1 10.0 ± 0.7 0.2 ± 0.0 3.1 ± 0.1 22.8 ± 0.1 63.5 ± 0.8 0.5 ± 0.1 10 0.1 ± 0.0 10.3 ± 0.1 0.2 ± 0.0 3.1 ± 0.1 23.0 ± 0.1 62.8 ± 0.0 0.6 ± 0.1 Steamed 10 0.1 ± 0.0 9.9 ± 0.1 0.2 ± 0.0 3.0 ± 0.0 22.3 ± 0.1 64.1 ± 0.3 0.5 ± 0.1 30 1.2 ± 0.3 10.3 ± 0.3 0.3 ± 0.0 2.9 ± 0.0 22.2 ± 0.5 62.5 ± 0.2 0.5 ± 0.0 60 1.3 ± 0.1 10.2 ± 0.3 0.3 ± 0.0 2.0 ± 0.1 21.9 ± 0.0 62.9 ± 0.4 0.5 ± 0.0 microwave One 1.2 ± 0.2 10.1 ± 0.0 0.3 ± 0.0 2.1 ± 0.1 20.0 ± 0.1 62.8 ± 0.6 0.5 ± 0.1 3 1.4 ± 0.1 10.8 ± 0.8 0.4 ± 0.1 2.3 ± 0.2 20.3 ± 0.0 61.4 ± 1.2 0.5 ± 0.1 5 0.7 ± 0.1 10.1 ± 0.9 0.5 ± 0.1 2.6 ± 0.3 20.0 ± 0.9 62.6 ± 2.6 1.5 ± 1.1

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

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

As shown in Table 2, the fatty acid composition of grape seed oil shows myristic acid (0.1%), palmitic acid (10.2%), palmitoleic acid (0.2%), stearic acid (2.0%), oleic acid (22.5%), It was composed of linoleic acid (64.0%) and linolenic acid (0.4%), it can be seen that there is little change in the fatty acid composition content of grape seed oil by three heat treatments (roasting, steaming and microwave).

Experimental Example 3: Determination of total catechin and four catechin composition contents of grape seed extract

The total catechin content of the grape seed extract was determined by the Food Code (KFDA, Moon Youngsa, pp.

330-331, 2000) was measured according to vanillin colorimetric method, and four catechin composition contents were measured by HPLC according to the method of Choi et al. (Korean Food Science Society, 35: 576-585, 2003). Table 3 shows the results of measuring the total catechin content of grape seeds according to the three heat treatments.

Changes in Total Catechin Content of Grape Seed by Three Heat Treatments Heat treatment Minutes Total catechins (%, dry grape seed) Control 4.22 ± 0.32 stir-fry 3 4.21 ± 0.51 (100.0) ^* 5 3.74 ± 0.28 (88.6) 10 2.75 ± 0.43 (65.2) Steamed 10 4.02 ± 0.34 (95.3) 30 4.04 ± 0.47 (95.7) 60 3.86 ± 0.55 (91.5) microwave One 4.33 ± 0.42 (102.6) 3 3.34 ± 0.27 (79.2) 5 2.34 ± 0.39 (55.5)

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 3, the total catechin content of grape seeds was significantly reduced by roasting and steaming, except for microwave treatment during the three heat treatments. However, the total catechin content was increased by 3% compared to the control during 1 minute of microwave treatment, but the content decreased significantly with time. In this way, compared with the roasting and steaming of grape seeds, it can be seen that microwave treatment can improve the extraction yield of total catechin, the main bioactive substance of grape seeds.

In addition, the results of measuring the change in the content of four catechin composition of grape seeds according to the three heat treatments are shown in Table 4.

Changes in the Contents of Four Catechins in Grape Seed by Three Heat Treatments Heat treatment Time (min) Catechin (%, Dried Grape Seed) (+)-Catechin Procyanidin B ₂ (-)-Epicatechin (-)-Epicatechin gallate Total ^{Catechin *} Control 0.627 ± 0.0298 0.047 ± 0.0028 0.507 ± 0.0226 0.031 ± 0.0007 1.212 ± 0.0757 stir-fry 3 0.581 ± 0.0200 0.032 ± 0.0132 0.478 ± 0.0239 0.027 ± 0.0021 1.118 ± 0.0684 5 0.579 ± 0.0164 0.029 ± 0.0070 0.456 ± 0.0228 0.028 ± 0.0009 1.092 ± 0.0527 10 0.334 ± 0.0166 0.022 ± 0.0085 0.229 ± 0.0196 0.016 ± 0.0005 0.601 ± 0.0283 Steamed 10 0.583 ± 0.0080 0.039 ± 0.0024 0.487 ± 0.0078 0.028 ± 0.0017 1.137 ± 0.0194 30 0.524 ± 0.0105 0.027 ± 0.0039 0.431 ± 0.0130 0.020 ± 0.0008 1.002 ± 0.0241 60 0.385 ± 0.0150 0.022 ± 0.0031 0.387 ± 0.0132 0.014 ± 0.0007 0.808 ± 0.0319 microwave One 0.623 ± 0.0123 0.043 ± 0.0068 0.498 ± 0.0146 0.033 ± 0.0005 0.197 ± 0.0258 3 0.693 ± 0.0175 0.042 ± 0.0080 0.582 ± 0.0166 0.034 ± 0.0016 0.351 ± 0.0314 5 0.627 ± 0.0234 0.040 ± 0.0048 0.521 ± 0.0166 0.034 ± 0.0022 0.222 ± 0.0501

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.

^- catechin procyanidin B ₂ + + (-) - epicatechin + (-) - epicatechin gallate

As shown in Table 4, the contents of the four catechin components during the roasting and the steaming treatment decreased significantly compared to the control as the treatment time progressed, whereas the contents of the four catechin components (except procyanidine B ₂ ) in the microwave treatment group It increased slightly until 1 minute and then decreased. In this way, the microwave treatment was found to improve the extraction yield of total catechin and four catechin components, which are the main bioactive substances of grape seeds, compared to the roasting and steaming treatment.

Experimental Example 4: Measurement of grape seed oil yield change by degumming treatment

Obtained by extraction with hexane In order to set the optimum degumming treatment conditions for removing the phospholipids and resins contained in the crude grape seed crude oil, the results of the measurement of the grape seed crude oil yield according to the phosphate concentration (the temperature of 85-95 ° C) are shown in Table 5.

Changes in the Maintenance Yield of Grape Seed Crude Oil (100 g) According to Phosphoric Acid Concentration Phosphoric Acid Concentration Oil yield (%) Control 100 0.05% 98.5 ± 2.3 0.1% 98.4 ± 1.7 0.15% 97.2 ± 1.9 0.2% 93.6 ± 1.8 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 5, the yield of grape seed oil obtained by centrifugation after degumming the grape seed oil while increasing the phosphate concentration up to 0.05% -0.2% showed that the oil yield decreased slightly as the phosphate concentration increased. At 0.2% concentration, the decrease was somewhat large. Therefore, it was found that the optimum phosphoric acid concentration at the time of degumming treatment of grape seed crude oil is preferably performed at 0.2% or less.

Experimental Example 5 Measurement of Changes in Yield, Acid Value and Peroxide Value of Grape Seed Oil by Deoxidation Treatment

In order to set the optimum deoxidation condition for removing free fatty acid contained in grape seed crude oil extracted by hexane, the results of measuring the yield, acid value and peroxide value of grape seed crude oil according to NaOH concentration and throughput were measured. 7 is shown respectively. At this time, the acid value (AV) and peroxide value (POV) were measured according to the Food Code Test Method (Food and Drug Administration, Moonyoungsa, Seoul, 2003).

Changes in Oil Yield, Acid Value, and Peroxide Value of Grape Seed Crude Oil (100 g) According to NaOH Concentration NaOH concentration NaOH throughput (mL) Oil yield (%) Acid value (AV) Peroxide Value (POV) Control 30 100 4.81 ± 0.51 18.72 ± 0.42 1% NaOH solution 30 62.5 ± 1.3 3.21 ± 0.22 16.54 ± 0.33 3% NaOH solution 30 61.4 ± 1.4 2.92 ± 0.16 16.26 ± 0.41 5% NaOH solution 30 55.2 ± 1.6 2.24 ± 0.15 15.44 ± 0.23 10% NaOH solution 30 48.4 ± 0.8 1.72 ± 0.04 14.15 ± 0.28 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 6, as the NaOH concentration was increased to 1% -10%, the oil yield decreased as the NaOH concentration increased, especially in the 10% NaOH solution. Next, the acid and peroxide values of the grape seed crude oil extracted with hexane were 4.81 and 18.72, respectively, but as the NaOH concentration increased from 1% to 5%, the acid and peroxide values decreased to 2.24 and 15.44, respectively. However, in 10% NaOH treatment, the acid value and peroxide value were 1.72 and 14.15, respectively, slightly lower than those of the 5% NaOH treatment, but the oil yield was significantly lower to 48.4% than the control. Therefore, the results of the grape seed oil yield and chemical test (acid value and peroxide value) showed that 5% NaOH treatment was the optimal concentration for deoxidation of crude oil of grape seed.

Changes in Oil Yield, Acid Value, and Peroxide Value of 5% NaOH Treated Grape Oil (100 g) in Deoxidation NaOH throughput (mL) Oil yield (%) Acid value (AV) Peroxide Value (POV) 10 58.2 ± 2.1 2.55 ± 0.33 16.53 ± 0.21 30 55.2 ± 1.6 2.24 ± 0.15 15.44 ± 0.23 50 54.2 ± 1.6 2.03 ± 0.16 15.12 ± 0.33 70 53.5 ± 1.7 1.74 ± 0.22 15.05 ± 0.25 100 49.2 ± 1.4 1.36 ± 0.19 14.91 ± 0.15 All measurements were expressed as mean ± SD after three repeated measurements. There is statistical significance ( p <0.05) between the measurements of each item.

On the other hand, as shown in Table 7, the increase in 5% NaOH throughput from 10mL to 70mL decreased the acid value and peroxide value at the same time lowered to 1.74 and 15.05 when treated with 5% NaOH 70mL respectively. However, the acid value and peroxide value of 100 mL of 5% NaOH solution were slightly lower than that of 70 mL, but the oil yield was significantly lower than that of the control (49.2%). Therefore, from the yield and chemical tests (acid value and peroxide value) of grape seed oil, it was found that the most suitable amount of 5% NaOH solution for the deoxidation of grape seed oil was 70mL.

Experimental Example 6 Measurement of Changes in Oil Yield, Acid Value and Peroxide Value According to Deodorization Treatment Temperature of Grape Seed Oil by Steam Distillation

previously Degumming and In order to set the optimum deodorization condition to remove not only normal-hexane and free fatty acid contained in trace amount of deoxidized grape seed crude oil, but also odor and odor, steam distillation stationary was used for each temperature (220 ~ 250 ℃, pressure 3 ~ 5 mmHg or less, 2 hours) The results of measuring the changes in yield, acid value and peroxide value of grape seed crude oil are shown in Table 8.

Changes in Oil Yield, Acid Value and Peroxide Value of Grape Seed Oil by Steam Distillation Steam distillation treatment temperature (℃) Oil yield (%) Acid value (AV) Peroxide Value (POV) Control 100 1.74 ± 0.22 15.05 ± 0.21 200 99.3 ± 1.3 1.70 ± 0.18 15.04 ± 0.22 210 98.3 ± 1.5 1.70 ± 0.15 14.44 ± 0.16 220 98.2 ± 1.4 0.87 ± 0.20 12.02 ± 0.17 230 95.2 ± 1.1 0.84 ± 0.18 11.94 ± 0.15 240 92.7 ± 1.6 0.83 ± 0.23 12.19 ± 0.12 250 91.6 ± 2.1 0.72 ± 0.12 12.15 ± 0.20 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 8, the acid value and peroxide value of the grape seed crude oil before deodorization treatment were 1.74 and 15.05, respectively, but the yield of grape seed oil gradually decreased with increasing the deodorization treatment temperature, especially at 230 ° C. And the acid value and peroxide value decreased simultaneously and lowered to 0.87 and 12.02, respectively, up to treatment 220 ° C. However, the acid value and peroxide value of grapeseed oil at treatment 230 ° C. did not differ significantly from treatment 220 ° C., while the oil yield was somewhat lower. Therefore, the deodorization treatment temperature of partially purified grape seed oil by steam distillation was found to be the most appropriate.

Experimental Example 7 Measurement of Changes in Oil Yield, Acid Value and Peroxide Value According to Deodorization Treatment Time of Grape Seed Oil by Steam Distillation

Steam distillation (temperature; 220 ℃, pressure: 3 ~ 5 mmHg) to change the yield, acid value and peroxide value of grape seed crude oil by time (1-5 hours) to set the optimum deodorization condition are shown in Table 9. .

Changes in Oil Yield, Acid Value and Peroxide Value of Steam Seed Oil by Deodorization Treatment Time by Steam Distillation Steam Distillation Processing Time (min) Oil yield (%) Acid value (AV) Peroxide Value (POV) Control 100 1.74 ± 0.22 15.05 ± 0.25 30 99.3 ± 1.4 1.67 ± 0.21 15.04 ± 0.23 60 98.5 ± 1.6 1.52 ± 0.18 13.44 ± 0.19 90 98.2 ± 1.5 1.07 ± 0.19 13.53 ± 0.18 120 97.3 ± 1.2 0.64 ± 0.15 12.43 ± 0.13 150 93.7 ± 1.8 0.63 ± 0.12 12.27 ± 0.17 180 90.6 ± 1.5 0.62 ± 0.13 12.13 ± 0.16 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 9, the acid value and peroxide value of the grape seed crude oil before deodorization treatment were 1.74 and 15.05, respectively, but as the deodorization treatment time elapsed, the acid value and the peroxide value decreased simultaneously and lowered to 0.64 and 12.43, respectively, up to 2 hours of treatment. However, the acid value and peroxide value of grapeseed oil after 2 hours of treatment were not significantly different than 2 hours of treatment, while the oil yield was slightly lower. Therefore, the deodorization treatment time of the partially purified grape seed oil by steam distillation was found to be 2 hours.

Preparation Example 1 Preparation of Purified Grape Seed Oil from Dry Grape Seeds

Based on the grape seed crude oil refining process established above, a high quality grape seed oil manufacturing process is shown in FIG. 1, which will be described in detail.

Dry grape seed (1kg, water content 10%) was crushed into 30 ~ 50 mesh using a grinder, and then microwaved for 1 minute in a microwave oven, allowed to cool, and was then added to normal-hexane (5kg) in an extractor equipped with a reflux condenser. Oil was extracted for 2 hours while heating to 70 ~ 80 ℃ and filtered to obtain hexane extract and grape seed skim foil, respectively. Next, the hexane extract obtained after performing the above extraction process twice was concentrated under reduced pressure at 40 ℃ or less to obtain grape seed crude oil (80 ~ 85g, acid value: 4.90, peroxide value: 20.42). Next, the grape seed crude oil was stirred for 5 minutes in a water bath warmed to 85 to 95 ° C. in advance, and then 0.1% phosphoric acid (to 100 g of grape seed oil) was added thereto, followed by mixing at high speed for 3 minutes, followed by centrifugation (5,000 rpm, 20 minutes) 15 mL of the same amount of 5% NaOH solution was added to the obtained supernatant, deoxidized with stirring for 3 minutes, allowed to cool, and centrifuged again to obtain an oil extract of the upper layer. 5 g of the granules mixed with activated clay and activated carbon at 2: 1 were added thereto, followed by decolorization treatment under reduced pressure (50 mmHg or less) for 1 hour at 90 to 100 ° C, followed by filtration under reduced pressure to obtain grapeseed oil. Finally, to deodorize the grapeseed oil, using a steam distillation apparatus to deodorize at 220-230 ° C. for 2 hours under reduced pressure (3-5 mmHg or less) to completely remove the traces of normal-hexane, imitate and off-flavor present in the oil. After removal, finally purified grape seed oil (55 ~ 65g) was prepared.

Experimental Example 8: Physicochemical Properties of Grape Seed Oil

The results of the physicochemical quality characteristics of grape seed oil prepared in the preparation example, that is, grape seed oil properties, linoleic acid and catechin content, acid value, peroxide value and presence of E. coli are shown in Table 10.

Physicochemical Properties of Refined Grape Seed Oil Physicochemical Quality Characteristics Grapeseed oil Property It has a unique light yellow color and flavor and no odor Linoleic Acid (%) 69.5 Catechin (mg / 100 g) ¹ 323.56 Acid 0.2 Peroxide value 4.5 Coliform group ² voice ¹ Method for measuring total catechin content using vanillin colorimetric method in food industry. ^{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 10, refined grapeseed oil has an inherent pale yellow color and flavor and has no off-flavor. The linoleic acid content of grapeseed oil was 69.5 (mol%), the catechin content was 323.56 mg%, the acid value and peroxide value were 0.2 and 4.5, and the E. coli was negative. The physicochemical quality characteristics of the refined grape seed oil were found to be in compliance with the grape seed oil food standards specified in the current Food Code.

Example 2: Preparation of High Quality Grape Seed Extract from Grape Seeds

Grape seed extracts of high quality which can be used for the preparation of functional foods or functional cosmetic raw materials from grape seeds were prepared and their catechin contents were compared.

Preparation Example 1 Preparation of High Quality Grape Seed Extract for Preparation of Functional Food Ingredients from Grape Seed

20% ethanol extract containing the procyanidin component, which is the main catechin compound of grape seeds, and a process for preparing the purified fraction are shown in FIG. To explain this in detail, the skim grape seed cake obtained from dried grape seeds (1 kg) was dried in a hot air dryer (50-60 ° C., 6-12 hours) (the grape seed cake weight was 860 g) and 20% alcohol ethanol solution (10 L) After adding and heating repeatedly repeated 3 times at 70 ~ 80 ℃ for 3 hours, filtered and concentrated under reduced pressure to obtain a grape seed cake 20% ethanol extract (80.5g). Next, take 5.0g of this (at this time, the remaining 75.5g is continuously treated with the next purification process), suspended in 30mL distilled water, adjust the pH of the suspension to 3.0 using citric acid, and equilibrate with distilled water in advance. After filling with adsorption chromatography (4cm × 40cm), distilled water (2.0L) was used to remove organic acids, amino acids and proteins contained in the extract, and then eluted with 20% ethanol aqueous solution (4.0L). A 20% ethanol extract (0.2 g, yield: 322 mg% dry grape seed) containing a catechin derivative (catechin minor and multimer procyanidins) was obtained.

Preparation Example 2 Preparation of Grape Seed Extract for Raw Material of High Quality Functional Cosmetics from Grape Seed

80% ethanol extract mainly containing monomeric catechins ((+)-catechin, (-)-epicatechin, (-)-epicatechin gallate) and dimer catechin (procyanidin B ₂ ) in grape seed catechin compounds and purified fractions The manufacturing process of is shown in FIG.

80% ethanol aqueous solution (10L) was added to the dried skim grape seed cake (860 g) obtained in Preparation Example 1, followed by repeated heating and extraction twice at 50 to 60 ° C. for 3 hours, followed by filtration and concentration under reduced pressure. (85.5 g) was obtained. Take 5.0g of this (the remaining 80.5g is also treated with the following purification process in succession), suspended in 30mL 20% ethanol solution and equilibrated with 20% ethanol aqueous solution (4cm × 40cm). And then eluted with 20% ethanol aqueous solution (1.0 L) and 60% ethanol aqueous solution (4.0 L), respectively, followed by 60% ethanol extract (0.38 g) containing monomer catechin and dimer procyanidins (dimer procyanidins). , 646 mg% / dry grape seed).

Experimental Example 1: Comparison of catechin content of 20% and 80% ethanol crude extracts of skim grape seed cake

The results of comparing the content of the total catechin and the four catechin components of the 20% ethanol crude extract and 80% ethanol crude extract of skim grape seed prepared above are shown in Tables 11 and 12.

Comparison of Total Catechin Contents of 20% Ethanol and 80% Ethanol Crude Extracts from Skim Grape Seeds Crude extract Yield (%, dry grape seed) Total catechin content (%, dry grape seed extract) Total catechin content (%, dry grape seed) 20% ethanol 8.05 ± 0.28 49.44 ± 0.83 3.83 ± 0.54 80% ethanol 8.50 ± 0.39 76.50 ± 1.24 6.58 ± 0.82

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.

As shown in Table 11, the yields of 20% ethanol crude extract and 80% ethanol crude extract of skim grape seed cake were 8.05% and 8.50%, respectively, and the yield of 80% ethanol crude extract was somewhat higher than that of 20% ethanol crude extract. Total catechin content was 49.44% (dry grape seed extract, 3.83% dry grape seed) in 20% ethanol crude extract, and 80.ethanol crude extract was 76.50% (dry grape seed extract, 6.58% dry grape seed) in 20% ethanol crude extract. About two times higher.

Comparison of the Contents of the Four Main Catechin Components from 20% Ethanol and 80% Ethanol Extracts of Skim Grape Seeds Crude extract Catechin (% skim grape seed cake) (+)-Catechin Procyanidin B ₂ (-)-Epicatechin (-)-Epicatechin gallate gun 20% ethanol 1.060 ± 0.017 (0.912 ± 0.015) 0.063 ± 0.012 (0.054 ± 0.010) 0.596 ± 0.013 (0.513 ± 0.011) 0.025 ± 0.003 (0.022 ± 0.002) 1.744 (1.501) * 80% ethanol 0.859 ± 0.017 (0.739 ± 0.016) 0.017 ± 0.013 (0.015 ± 0.011) 0.872 ± 0.017 (0.750 ± 0.018) 0.042 ± 0.004 (0.036 ± 0.003) 1.789 (1.539) * All measurements were expressed as mean ± SD after three repeated measurements. There is statistical significance ( p <0.05) between the measurements of each component. ^* Content per 100g of dried grape seed

As shown in Table 12, the contents of the four main catechin components of the 20% ethanol crude extract were (+)-catechin 1.060%, procyanidin B ₂ 0.063%, (-)-epicatechin 0.596% and (-)-epicatechin gal. The content of 80% ethanol crude extract was 0.825% of (+)-catechin 0.859%, procyanidin B ₂ 0.017%, 0.872% of (-)-epicatechin and 0.042% of (-)-epicatechin gallate (+) The contents of catechin and procyanidin B ₂ were 20% ethanol crude extract higher than 80% ethanol crude extract, while the contents of (-)-epicatechin and (-)-epicatechin gallate were higher than 80% ethanol crude extract 20% ethanol crude extract. . However, the total content of the four catechin components, the main bioactive substance of grape seed, was 80% ethanol crude extract (1.744% skim grape seed cake) rather than 20% ethanol crude extract (1.789% skim grape seed cake).

Experimental Example 2: Comparison of catechin content between 20% ethanol fraction and 80% ethanol fraction

The results of comparing the contents of the total catechins and the four catechins of the 20% ethanol fraction separated from the 20% ethanol crude extract separated by ion resin adsorption chromatography and the 60% ethanol fraction separated from the 80% ethanol crude extract are shown in Table 13. And Table 14, respectively.

Comparison of Total Catechin Contents of 20% Ethanol Fractions Isolated from 20% Ethanol Crude Extracts from Defatted Grape Seed Park and 60% Ethanol Fractions Isolated from 80% Ethanol Crude Extracts by Ion Resin Adsorption Chromatography Fraction Yield (%) / dried grape Total catechin content (%, dry grape seed extract) Total catechin content (%, dry grape seed) 20% ethanol 0.39 ± 0.10 11.75 ± 1.21 1.41 ± 0.15 60% ethanol 2.65 ± 0.11 36.86 ± 1.42 3.17 ± 0.17 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 yield of the 20% ethanol fraction separated from the 20% ethanol crude extract by ion resin adsorption chromatography was about 0.39%, which is about 2.65% of the 60% ethanol fraction separated from the 80% ethanol crude extract. The total catechin content was 1.41% (dry grape seed) in 20% ethanol fraction, 3.17% in 60% ethanol fraction and about 2 times higher in 60% ethanol fraction than 20% ethanol fraction.

Comparison of the Contents of Four Catechin Components from 20% Ethanol Fractions Isolated from 20% Ethanol Crude Extracts of Skim Grape Seeds and 60% Ethanol Fractions Isolated from 80% Ethanol Crude Extracts by Ion Resin Adsorption Chromatography Fraction Catechin (% Dry Grape Seed Fraction) (+)-Catechin Procyanidin B ₂ (-)-Epicatechin (-)-Epicatechin gallate gun 20% Ethanol Fraction 7.161 ± 0.303 (0.835 ± 0.021) 0.856 ± 0.126 (0.120 ± 0.042) 2.954 ± 0.421 (0.365 ± 0.041) 0.123 ± 0.020 (0.012 ± 0.004) 11.094 (1.33) * 60% Ethanol Fraction 10.893 ± 0.423 (0.802 ± 0.032) 1.550 ± 0.103 (0.053 ± 0.023) 9.546 ± 0.204 (0.755 ± 0.062) 0.231 ± 0.082 (0.035 ± 0.005) 22.220 (1.65) * All measurements were expressed as mean ± SD after three repeated measurements. There is statistical significance ( p <0.05) between the measurements of each component. ^* Total content of 4 catechin components per 100g of dried grape seeds (%)

As shown in Table 14, the contents of the four main catechin components of the 20% ethanol fraction separated from the 20% ethanol crude extract by ion resin adsorption chromatography were (+)-catechin 7.161%, procyanidin B ₂ 0.856%, 2.954% of (-)-epicatechin and 0.123% of (-)-epicatechin gallate. In contrast, the contents of the four catechin components of the 60% ethanol fraction separated from the 80% ethanol crude extract were 10.893% of (+)-catechin, 1.55% of procyanidin B ₂ , 9.546% of (-)-epicatechin and (-)-epicatechin gal. The rate was 0.231%, higher than the 20% ethanol fraction. As such, the 60% ethanol fraction separated from the 80% ethanol crude extract by ion resin adsorption chromatography was found to have higher content of catechins, the main bioactive substance of grape seeds, than the 20% ethanol fraction separated from the 20% ethanol crude extract. there was.

Experimental Example 3: Physicochemical Quality Characteristics of 20% Ethanol Fraction and 60% Ethanol Fraction Isolated by Ion Resin Adsorption Chromatography

Various physicochemical qualities, such as solubility, pH, sugar content, acidity, color and taste of 20% ethanol fraction and 60% ethanol fraction separated by ion-resistance chromatography, respectively The results of comparing the characteristics are shown in Table 15.

Comparison of Physicochemical Properties of 20% Ethanol Fraction and 60% Ethanol Fraction Isolated by Ion Resin Adsorption Chromatography Fraction Physicochemical Quality Characteristics Solubility ¹ pH Sugar content ² PH ³ Chromaticity ⁴ flavor L a b 20% Ethanol receptivity 6.43 ± 0.21 22.6 ± 1.3 1.61 ± 0.32 88.78 ± 2.92 2.87 ± 0.14 19.02 ± 1.52 Weak bitter taste 60% ethanol Water-insoluble 6.58 ± 0.23 20.2 ± 1.2 1.40 ± 0.17 74.19 ± 1.52 15.16 ± 0.31 23.50 ± 2.41 Strong astringent taste All measurements were expressed as mean ± SD after three repeated measurements. ^{1 Use} 10% grape seed extract. ² Measured by refractometer. ³ Measured 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).

As shown in Table 15, the 20% ethanol fraction is water soluble but the 60% ethanol fraction is water-insoluble (alcohol), pH is 6.43 and 6.58, sugars are 22.6 and 20.2, respectively, and acidity is 1.61 and 1.40, respectively. Was similar. The chromaticity of the 20% ethanol fractions ( L = 88.78, a = 2.87 and b = 19.02) is light brown, while the chromaticity of the 60% ethanol fractions ( L = 74.19, a = 15.16 and b = 23.50) is dark brown. And 20% ethanol fraction had a mild astringent taste and sweet taste, while 60% ethanol fraction had a strong bitter taste. The physicochemical properties of the 20% and 60% ethanol fractions indicated that the 20% ethanol fraction was suitable as a raw material for functional foods (drinks) such as juices and drinks, while the 60% ethanol fraction was suitable as a functional cosmetic raw material. .

From the above results, in order to manufacture high quality grape seed oil and extracts from grape seeds, the changes of various functional components according to the heat treatment of the grape seeds were first measured, and then microwave heat treatment was set as the optimum processing method of the grape seeds based thereon. Was extracted with normal-hexane to obtain grape seed crude oil and skim foil, respectively, and again grape seed crude oil was subjected to degumming, deoxidation and deodorization process to prepare purified grape seed oil. Development of high quality grape seed extract using adsorption chromatography. These grape seed oils and extracts contain high amounts of anti-cancer, antihypertensive, antioxidant and anti-aging catechins, which can prevent cancer, heart disease, hypertension and aging. Functional health food and It is expected to be in the limelight as material.

As described through the above Examples and Experimental Examples, the present invention relates to a method for producing high quality grape seed oil and extract from grape seeds, pulverized dry grape seed, and then degreased with normal-hexane, filtered and concentrated grape seed. Crude oil and grapeseed gourd are obtained, and grapeseed crude oil is made of high-quality purified grapeseed oil through degumming, deoxidation, and deodorization in turn, and skimmed grapeseed gourd is extracted by boiling water with ethanol solution, filtered and concentrated, and then ion resin adsorption chromatography By using graphy to prepare a catechin-containing high quality grape seed extract eluting in 20% and 60% ethanol aqueous solution has an excellent effect of providing an improved method of producing grape seed oil and grape seed extract. In addition, high-quality grape seed oil manufactured in the present invention can be sold as a functional food to meet the food standards, as well as grape seed extract is a new material of functional food, cosmetics and medicines that can prevent cancer, heart disease, high blood pressure and aging It can be used as an active ingredient as a very useful invention in the functional food industry.

Claims (3)

In the grape seed oil manufacturing method, Dry grape seed was pulverized and microwaved for 1 minute, then degreased with normal-hexane, and the obtained grapeseed crude oil was degumming at 0.15% phosphoric acid concentration, and then deoxidized with 5% NaOH solution and then steamed at 220 ° C. using a steam distillation apparatus. Grape seed oil production method characterized in that the deodorizing treatment at 5 mmHg pressure for a time. The dried grape seed was pulverized and microwaved for 1 minute, then degreased with normal-hexane. The obtained skim grape seed cake was heated and extracted with 20% or 80% ethanol aqueous solution, followed by filtration and concentration to obtain skim grape seed ethanol extract. Method for producing a catechin derivative-containing grape seed extract for functional food manufacturing raw materials, characterized in that eluted with 20% or 60% ethanol aqueous solution using chromatography. delete

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