CN105130941B - A kind of preparation method of grape seed extract - Google Patents

A kind of preparation method of grape seed extract Download PDF

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Publication number
CN105130941B
CN105130941B CN201510542574.6A CN201510542574A CN105130941B CN 105130941 B CN105130941 B CN 105130941B CN 201510542574 A CN201510542574 A CN 201510542574A CN 105130941 B CN105130941 B CN 105130941B
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China
Prior art keywords
grape
extract
extraction
grape pip
powder
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Expired - Fee Related
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CN201510542574.6A
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Chinese (zh)
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CN105130941A (en
Inventor
文继承
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Hangzhou Regenerative Muscle Biotechnology Co ltd
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GUILIN MINGXING BIOTECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/58Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
    • C07D311/60Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
    • C07D311/62Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/025Pretreatment by enzymes or microorganisms, living or dead
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Biochemistry (AREA)
  • Microbiology (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The present invention discloses a kind of preparation method of grape seed extract, comprises the following steps:1) grape pip is crushed, added water and yeast, at room temperature sealing and fermenting, obtain pre-processing grape pip powder after vacuum drying;2) fluid constituted is pressed as extractant using propane and dimethyl ether, subcritical abstraction, obtained extract as grape-kernel oil is carried out to pretreatment grape pip powder;After after grape-kernel oil extraction completely, it is changed to carry out subcritical abstraction by extractant of absolute ethyl alcohol, extract is concentrated under reduced pressure, after concentrate is dried through active carbon adsorption, obtained bronzing powder as procyanidin extract.The extracting method that the present invention is provided combines various effective extracting methods, can effectively improve the purity of yield and extract, so as to obtain the product of very high quality.

Description

A kind of preparation method of grape seed extract
Technical field
The present invention relates to the preparation method of plant extracts, specifically a kind of preparation method of grape seed extract.
Background technology
Grape pip is generally the leftover bits and pieces after grape wine brewing, can account for the 5%~7% of whole grain grape.Containing abundant in grape pip Grape-kernel oil and OPC.Wherein, the unsaturated fatty acid content in grape-kernel oil is up to 90%, unrighted acid More than 75% is linoleic acid, is a kind of high vegetable oil of quality.And OPC then has significant anti-oxidant and removed certainly It is active by base, with the various functions such as angiocarpy, preventing hypertension, anti-mutation, antitumor, whitening and skin-protecting are protected, extensively Applied to fields such as food, medicine and cosmetics.And the existing method that grape-kernel oil and OPC are extracted from grape pip Have:Low yield, extract are there is in aqueous solution soaking method, organic solvent extractionprocess, supercritical extraction etc., these methods The shortcoming that purity is low, production cost is high.
The content of the invention
The purpose of the present invention is in view of the shortcomings of the prior art, there is provided a kind of preparation method of grape seed extract, to have The advantages of yield is high, product purity is high.
The present invention uses following technical scheme:
A kind of preparation method of grape seed extract, comprises the following steps:
1) grape pip is crushed, adds the water and 0.05%~0.15% yeast of grape pip weight 30%~40%, room The lower sealing and fermenting of temperature 3~8 days, is dried under vacuum to moisture content≤6%, obtains pre-processing grape pip powder;
2) 2~3 are pressed with propane and dimethyl ether:4~7 weight is extractant than the fluid of composition, to pretreatment grape pip Powder carries out subcritical abstraction, and Extracting temperature is 49~53 DEG C, and extractions pressure is 2.5~2.9MPa, extraction time for 30~ 60min, obtained extract as grape-kernel oil;After after grape-kernel oil extraction completely, it is changed to enter by extractant of absolute ethyl alcohol Row subcritical abstraction, extraction temperature is 58~63 DEG C, and extracting pressure is 3.4~3.7MPa, and extraction time is 30~50min, extraction Thing is taken to be concentrated under reduced pressure into the 1/3~1/6 of original volume, after concentrate is dried through active carbon adsorption, obtained bronzing powder As procyanidin extract.
In above-mentioned technical proposal,
The active carbon adsorption is molten with 70% ethanol for concentrate is crossed into activated-charcoal column with 0.5~1.0BV/h flow velocity Eluent, is then concentrated and dried by liquid eluant, eluent.
It is preferred that, added water and yeast is respectively the 35% and 0.1% of grape pip weight.
It is preferred that, when extracting for the first time, the weight ratio of propane and dimethyl ether is 2.5:6, Extracting temperature is 52.5 DEG C, is extracted Pressure is 2.7MPa, and extraction time is 40min.
Compared with prior art, the present invention has advantages below:
The extracting method that the present invention is provided combines various effective extracting methods, can effectively improve yield and extract Purity, so as to obtain the product of very high quality.Wherein, obtained grape-kernel oil residual oil content is less than 1.5%;Obtained former cyanine Plain yield may be up to 85%, and purity may be up to 98%.
Embodiment
It is further described below with specific embodiment, but the present invention is not limited to these embodiments.
Embodiment 1
1) grape pip is crushed, adds the water and 0.1% yeast of grape pip weight 35%, at room temperature sealing and fermenting 6 days, Moisture content≤6% is dried under vacuum to, obtains pre-processing grape pip powder;
2) 2.5 are pressed with propane and dimethyl ether:6 weight is extractant than the fluid of composition, and pretreatment grape pip powder is entered Row subcritical abstraction, Extracting temperature is 52.5 DEG C, and extraction pressure is 2.7MPa, and extraction time is 40min, and obtained extract is i.e. For grape-kernel oil;After after grape-kernel oil extraction completely, it is changed to carry out subcritical abstraction, extraction temperature by extractant of absolute ethyl alcohol For 60 DEG C, extracting pressure is 3.6MPa, and extraction time is 40min, and extract is concentrated under reduced pressure into the 1/5 of original volume, by concentrate Activated-charcoal column is crossed with 0.7BV/h flow velocity, with 70% ethanol solution eluant, eluent, is then concentrated and dried eluent, what is obtained is red Brown powder is procyanidin extract.
Embodiment 2
1) grape pip is crushed, adds the water and 0.1% yeast of grape pip weight 30%, at room temperature sealing and fermenting 8 days, Moisture content≤6% is dried under vacuum to, obtains pre-processing grape pip powder;
2) 2 are pressed with propane and dimethyl ether:5 weight is extractant than the fluid of composition, and pretreatment grape pip powder is carried out Subcritical abstraction, Extracting temperature is 53 DEG C, and extraction pressure is 2.5MPa, and extraction time is 50min, obtained extract as Portugal Grape seed oil;After after grape-kernel oil extraction completely, it is changed to carry out subcritical abstraction by extractant of absolute ethyl alcohol, extraction temperature is 63 DEG C, extracting pressure is 3.4MPa, and extraction time is 40min, and extract is concentrated under reduced pressure into the 1/6 of original volume, by concentrate with 0.5BV/h flow velocity crosses activated-charcoal column, with 70% ethanol solution eluant, eluent, is then concentrated and dried eluent, what is obtained is reddish brown Color powder is procyanidin extract.
Embodiment 3
1) grape pip is crushed, adds the water and 0.15% yeast of grape pip weight 38%, at room temperature sealing and fermenting 3 My god, moisture content≤6% is dried under vacuum to, obtains pre-processing grape pip powder;
2) 2.5 are pressed with propane and dimethyl ether:7 weight is extractant than the fluid of composition, and pretreatment grape pip powder is entered Row subcritical abstraction, Extracting temperature is 49 DEG C, and extraction pressure is 2.6MPa, and extraction time is 60min, and obtained extract is Grape-kernel oil;After after grape-kernel oil extraction completely, it is changed to carry out subcritical abstraction by extractant of absolute ethyl alcohol, extraction temperature is 58 DEG C, extracting pressure is 3.5MPa, and extraction time is 50min, and extract is concentrated under reduced pressure into the 1/3 of original volume, by concentrate with 0.5~1.0BV/h flow velocity crosses activated-charcoal column, with 70% ethanol solution eluant, eluent, is then concentrated and dried eluent, obtains Bronzing powder is procyanidin extract.
Embodiment 4
1) grape pip is crushed, adds the water and 0.05% yeast of grape pip weight 40%, at room temperature sealing and fermenting 5 My god, moisture content≤6% is dried under vacuum to, obtains pre-processing grape pip powder;
2) 3 are pressed with propane and dimethyl ether:4 weight is extractant than the fluid of composition, and pretreatment grape pip powder is carried out Subcritical abstraction, Extracting temperature is 51 DEG C, and extraction pressure is 2.9MPa, and extraction time is 30min, obtained extract as Portugal Grape seed oil;After after grape-kernel oil extraction completely, it is changed to carry out subcritical abstraction by extractant of absolute ethyl alcohol, extraction temperature is 61 DEG C, extracting pressure is 3.7MPa, and extraction time is 30min, and extract is concentrated under reduced pressure into the 1/5 of original volume, by concentrate with 1.0BV/h flow velocity crosses activated-charcoal column, with 70% ethanol solution eluant, eluent, is then concentrated and dried eluent, what is obtained is reddish brown Color powder is procyanidin extract.

Claims (3)

1. a kind of preparation method of grape seed extract, it is characterised in that comprise the following steps:
1) grape pip is crushed, adds the water and 0.05%~0.15% yeast of grape pip weight 30%~40%, at room temperature Sealing and fermenting 3~8 days, is dried under vacuum to moisture content≤6%, obtains pre-processing grape pip powder;
2) 2~3 are pressed with propane and dimethyl ether:4~7 weight is extractant than the fluid of composition, and pretreatment grape pip powder is entered Row subcritical abstraction, Extracting temperature is 49~53 DEG C, and extraction pressure is 2.5~2.9MPa, and extraction time is 30~60min, is obtained The extract arrived as grape-kernel oil;After after grape-kernel oil extraction completely, the progress by extractant of absolute ethyl alcohol is changed to subcritical Extraction, extraction temperature is 58~63 DEG C, and extracting pressure is 3.4~3.7MPa, and extraction time is 30~50min, extract decompression The 1/3~1/6 of original volume, after concentrate is dried through active carbon adsorption is concentrated into, obtained bronzing powder is former flower Blue or green extract;
The active carbon adsorption is washed for concentrate is crossed into carbon column with 0.5~1.0BV/h flow velocity with 70% ethanol solution Eluent, is then concentrated and dried by de- agent.
2. preparation method according to claim 1, it is characterised in that:Before fermentation, added water and yeast is respectively grape The 35% of seed weight and 0.1%.
3. preparation method according to claim 1, it is characterised in that:When extracting for the first time, the weight of propane and dimethyl ether Than for 2.5:6, Extracting temperature is 52.5 DEG C, and extraction pressure is 2.7MPa, and extraction time is 40min.
CN201510542574.6A 2015-08-31 2015-08-31 A kind of preparation method of grape seed extract Expired - Fee Related CN105130941B (en)

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CN107137952B (en) * 2017-03-20 2019-03-19 河南雍华生态农业科技有限公司 A kind of subcritical method for implanting of grape pip anthocyanidin
CN107445699A (en) * 2017-08-30 2017-12-08 太仓市林港农场专业合作社 A kind of preparation method of vegetable cultivation special efficient slow release fertilizer
CN107417412A (en) * 2017-08-30 2017-12-01 太仓市林港农场专业合作社 A kind of vegetable cultivation special efficient is sustained selenium-enriched fertilizer
CN107522545A (en) * 2017-08-30 2017-12-29 太仓市林港农场专业合作社 A kind of preparation method of vegetable cultivation special efficient sustained release selenium-enriched fertilizer
CN107417411A (en) * 2017-08-30 2017-12-01 太仓市林港农场专业合作社 A kind of vegetable cultivation special efficient slow release fertilizer
CN107721966A (en) * 2017-10-30 2018-02-23 潍坊友容实业有限公司 A kind of Suaeda salsa anthocyanidin and biogenic salt combined extraction method
CN107653227A (en) * 2017-11-13 2018-02-02 重庆斯德姆生物技术有限公司 A kind of inducing culture and abductive approach for promoting Differentiation of Marrow Stromal Stem Cells Into Neurons
CN107828723A (en) * 2017-11-13 2018-03-23 重庆斯德姆生物技术有限公司 A kind of type I collagen culture medium and preparation method thereof
CN108251357A (en) * 2017-12-26 2018-07-06 重庆斯德姆生物技术有限公司 A kind of induction cell culture fluid and differentiation method of the skeletal muscle stem Cells to Chondrocyte Differentiation
CN109207548B (en) * 2018-09-06 2020-10-30 山东省花生研究所 Peanut coat oligomeric proanthocyanidin, and preparation method and application thereof
CN112843780A (en) * 2021-01-05 2021-05-28 陕西科技大学 Pigment extraction process of mulberry pomace
CN112852182A (en) * 2021-01-05 2021-05-28 陕西科技大学 Pigment extraction process of blackcurrant raisin skin residues
CN112707880A (en) * 2021-01-05 2021-04-27 陕西科技大学 Anthocyanin extraction process for dried lycium ruthenicum fruits

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JPH09221484A (en) * 1996-02-14 1997-08-26 Kikkoman Corp Production of proanthocyanidin
CN101692999A (en) * 2009-10-22 2010-04-14 浙江大学 Mouth wash containing grape pip procyanidin extract and application
CN102851114A (en) * 2012-09-21 2013-01-02 南京泽朗农业发展有限公司 Method for extracting grape seed oil and proanthocyanidin

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Effective date of registration: 20200429

Address after: No. 181, erbatou, taimuyang village, Qinyu Town, Fuding City, Ningde City, Fujian Province

Patentee after: Deng Weixiao

Address before: Yingbin Road, Xingan County Guilin 541300 the Guangxi Zhuang Autonomous Region (Guilin Lingqu chemical factory warehouse)

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Address after: Room 613, Jiangjin international building, 251 Tongjiang Road, Changhe street, Binjiang District, Hangzhou City, Zhejiang Province

Patentee after: Hangzhou regenerative muscle Biotechnology Co.,Ltd.

Address before: No. 181, erbatou, taimuyang village, Qinyu Town, Fuding City, Ningde City, Fujian Province

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Granted publication date: 20170728