CN106581318A - Method for improving dissolution rate of grape seed extract flavones in press-shear assisted interaction mode - Google Patents

Method for improving dissolution rate of grape seed extract flavones in press-shear assisted interaction mode Download PDF

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Publication number
CN106581318A
CN106581318A CN201611184962.2A CN201611184962A CN106581318A CN 106581318 A CN106581318 A CN 106581318A CN 201611184962 A CN201611184962 A CN 201611184962A CN 106581318 A CN106581318 A CN 106581318A
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vitis viniferae
semen vitis
press
powder
flavones
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CN201611184962.2A
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Chinese (zh)
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李淑英
徐牧
贺栋业
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SAIMU BIOENGINEERING TECHNOLOGY Co Ltd DALIAN
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SAIMU BIOENGINEERING TECHNOLOGY Co Ltd DALIAN
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Publication of CN106581318A publication Critical patent/CN106581318A/en
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/87—Vitaceae or Ampelidaceae (Vine or Grape family), e.g. wine grapes, muscadine or peppervine
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10—Preparation or pretreatment of starting material
    • A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Microbiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention discloses a method for improving dissolution rate of grape seed extract flavones in a press-shear assisted interaction mode, and belongs to the technical field of plant active component extraction. The method comprises the following steps: washing grape seeds, drying the washed grape seeds, and crushing the dried grape seeds to obtain grape seed meal; carrying out ultrafine grinding on the grape seed meal and a physical assistant to prepare press-shear assisted powder; removing grease from the press-shear assisted powder by using petroleum ether, carrying out ultrasonic ethanol extraction, and carrying out reduced pressure distillation on obtained extract liquid to obtain concentrate dry powder which is grape seed extract; and detecting the content of the flavones in the obtained extract by using aluminum sulfate colorimetry to determine the target component release rate. Compared with the prior art, the method for assisted extraction of the grape seed flavones in the press-shear assisted interaction mode effectively the dissolution of the flavones in a water solution in a press-shear assisted powder state and further improves the precipitation rate of the flavones.

Description

The interaction mode that a kind of employing micro-cutting helps improves Semen Vitis viniferae extract flavone dissolution Method
Technical field
The invention belongs to active components of plants extractive technique field, is related to the extraction skill of new resource food Semen Vitis viniferae composition Art, is related specifically to the extracting method of Semen Vitis viniferae functional active components.
Background technology
Fructus Vitis viniferae is one of fruit crop maximum in the world, 69,000,000 tons of annual production.Semen Vitis viniferae accounts for most of Fructus Vitis viniferae 5%, it is the principal by product in the Grape processing industry such as Sucus Vitis viniferae and wine.Nowadays, because Semen Vitis viniferae is to various healthy obstacles There is the report of potential healthy benefits, Semen Vitis viniferae extract (GSE) is just obtaining more and more from scientist, threpsology and consumption The interest of person.Based on its potential non-oxidizability, anticancer, antibacterial, defying age, anti-hepatotoxin and anti-inflammatory activity, their quilts Widely as dietary supplement, and it is safe state by Food and Drug Administration's certification.The beneficial activity of Semen Vitis viniferae has it The probability of medicine and food service industry is used for as Drug therapy and health product.Contain more work in Semen Vitis viniferae extract Property material, active component has procyanidin, flavone, polyphenol, saponin, polysaccharide etc..Wherein Main Function has：Antioxidation, anti-spoke Penetrate antimutagenic, antiinflammatory, anticancer, blood circulation promoting, sight protectio, elimination edema, skin care beauty, heart protective agent etc..
In the last few years, many Chinese scholars constantly to plant effective active composition extract technique groped with it is excellent Change, some new extractions and isolation technics constantly emerge in large numbers appearance, such as microwave, ultrasound wave, supercritical, although these new techniques There is significant progress than conventional art, but the low problem of effective ingredient poorly water-soluble, availability is not also fundamentally solved Certainly, and some technologies due to equipment it is special, be also only limitted to laboratory research, and may not apply to Industrialized Production Practice.Can See, the imperfection of extractive technique always governs plant effective active composition deeper into research and the key of development and application Problem.Therefore, the extraction efficiency of effective ingredient is improved, reduces cost develops skill Maturity so as to reach industrialized production The exploitation of new technique is extremely urgent.Micro-cutting helps interaction mode as the new method of high efficiency extraction animals and plants active component in recent years, Its ultimate principle is：Animal-plant material cluster of grains becomes cell breakage through micro-cutting, and cell surface produces fresh tangent plane, auxiliary agent with have There is group or intermolecular mutual absorption or effect between effect composition, change the micro-property of effective ingredient, surface energy increases, Specific surface area increases, and adsorptivity and polarity increase, and helps the micro-cutting that interaction mode is obtained after processing to help powder in water by micro-cutting Dissolubility is greatly improved.Patent of invention：One kind is used for effective plant component extracting process, granted patent number： ZL200510130852.3, its main technical scheme is to crush the plant material being extracted, and is added in plant coarse powder The chemical assistant of 0.5-20% solid bases, solid acid, sucrose or salt compounds powder, and the inert material of fragility or sharp property Processed together, from water or ethanol dissolution process product, separate and collect soluble constituents and obtain effective ingredient.Therefore, plant Thing active component extraction efficiency is low, and elapsed time length etc. is problem demanding prompt solution.
The content of the invention
The technical problem to be solved in the present invention is to provide the seed of Fructus Vitis viniferae flavone extraction i.e. ultrasonic wave added micro-cutting of new technique and helps interaction Mode extracts seed of Fructus Vitis viniferae flavone, it is therefore an objective to provide a kind of new method that flavone dissolution is improved from Semen Vitis viniferae.The technological synthesiss The effective combination of interaction mode is helped to improve Semen Vitis viniferae extract extraction ratio and flavones content using ultrasonic technique and micro-cutting.
Specifically, employing micro-cutting of the present invention helps the method that interaction mode improves Semen Vitis viniferae extract flavone dissolution, with Semen Vitis viniferae is raw material, is comprised the following steps：
(1) take Semen Vitis viniferae to clean, vacuum condition is dried, then crush dried Semen Vitis viniferae, cross 40～60 mesh sieves, obtain Semen Vitis viniferae coarse powder；
(2) Semen Vitis viniferae coarse powder and physics auxiliary agent 0.5%～2% are put in vibromill and are ground by mass percentage 10min, obtains micro-cutting and helps powder；
(3) micro-cutting is helped into powder and 60% ethanol by solid-liquid ratio 1g:15ml is sufficiently mixed, and is that 40KHz, power are in frequency 100W, temperature are supersound extraction 20min under 40 DEG C of ul-trasonic irradiation, filter extracting solution, filter extracting solution, collect to obtain filtrate；
(4) filtrate is carried out into vacuum distillation by Rotary Evaporators, reclaims ethanol extractant, obtain Semen Vitis viniferae concentration dry Powder；
(5) Semen Vitis viniferae concentrated dry powder is configured to into certain density solution to be measured, with rutin as standard substance, using aluminum sulfate Colorimetry is detected to flavones content in extract.
The present invention extracts new technique as seed of Fructus Vitis viniferae flavone, can effectively extract Semen Vitis viniferae extract and flavones content, 20g Raw material can obtain extract 1.60g～1.80g, and 1.89 times are improved compared with traditional extraction process, and flavones content reaches 44.22mg/g～47.84mg/g, improves 1.42 times compared with traditional extraction process.Using ultrasound assisted extraction, by original leaching Bubble 24h shorten to 20min, greatly reduces flavone dissolution time, saves the operating time, improves extraction efficiency.Micro-cutting helps interaction side The use of formula so that the dissolution raising of flavone and the integrity of effective protection flavone, substantially increases the extraction ratio of flavone.This Invented technology is simple to operate, cost-effective, is more beneficial for industrialization.
Description of the drawings
Fig. 1 is the Semen Vitis viniferae particle size distribution figure of different pulverization process.
Fig. 2A is 60 mesh sieve Semen Vitis viniferae particulate scan electron microscopes.
Fig. 2 B are that Semen Vitis viniferae micro-cutting helps powder particles scanning electron microscope (SEM) photograph.
Fig. 3 is different pulverization process Semen Vitis viniferae extract extraction ratio figures.
Fig. 4 A are rutin standard curve figures.
Fig. 4 B are flavones content figures in different pulverization process Semen Vitis viniferae extracts.
Specific embodiment
The specific embodiment of the present invention is described in detail below in conjunction with technical scheme and accompanying drawing.
Embodiment 1
The method that interaction mode improves Semen Vitis viniferae extract flavone dissolution is helped using micro-cutting, with Semen Vitis viniferae as raw material, bag Include following steps：
(1) take Semen Vitis viniferae to clean, vacuum condition is dried, then crush dried Semen Vitis viniferae, cross 60 mesh sieves, obtain Fructus Vitis viniferae Seed coarse powder；
(2) the mesh powder 20g of Semen Vitis viniferae 60 is taken, by solid-liquid ratio 1g:15ml adds the ethanol of 300mL 60% to be sufficiently mixed, and is in frequency 40KHz, power are supersound extraction 20min under 100W, the ul-trasonic irradiation that temperature is 40 DEG C, filter extracting solution, collect to obtain filtrate；
(3) filtrate is carried out into vacuum distillation by Rotary Evaporators, reclaims ethanol extractant, obtain Semen Vitis viniferae concentration dry Powder；
(4) Semen Vitis viniferae concentrated dry powder is configured to into certain density solution to be measured, with rutin as standard substance, using aluminum sulfate Colorimetry is detected to flavones content in extract.
Embodiment 2
The method that interaction mode improves Semen Vitis viniferae extract flavone dissolution is helped using micro-cutting, with Semen Vitis viniferae as raw material, bag Include following steps：
(1) take Semen Vitis viniferae to clean, vacuum condition is dried, then crush dried Semen Vitis viniferae, cross 60 mesh sieves, obtain Fructus Vitis viniferae Seed coarse powder；
(2) the mesh coarse powder 500g of Semen Vitis viniferae 60 is taken, 1% physics auxiliary agent 5g is added by mass percentage, is put in vibromill Row grinding 10min, obtains micro-cutting and helps powder；
(3) take Semen Vitis viniferae micro-cutting and help powder 20g, by solid-liquid ratio 1g:15ml adds the ethanol of 300mL 60% to be sufficiently mixed, in frequency It is supersound extraction 20min under 100W, the ul-trasonic irradiation that temperature is 40 DEG C for 40KHz, power, filters extracting solution, collecting filters Liquid；
(4) filtrate is carried out into vacuum distillation by Rotary Evaporators, reclaims ethanol extractant, obtain Semen Vitis viniferae concentration dry Powder；
(5) Semen Vitis viniferae concentrated dry powder is configured to into certain density solution to be measured, with rutin as standard substance, using aluminum sulfate Colorimetry is detected to flavones content in extract.

Claims (2)

1. a kind of employing micro-cutting helps the method that interaction mode improves Semen Vitis viniferae extract flavone dissolution,
With Semen Vitis viniferae as raw material, it is characterised in that comprise the following steps：
(1) take Semen Vitis viniferae to clean, vacuum condition is dried, then crush dried Semen Vitis viniferae, cross 40～60 mesh sieves, obtain Fructus Vitis viniferae Seed coarse powder；
(2) Semen Vitis viniferae coarse powder and physics auxiliary agent 0.5%～2% are put in vibromill and are ground 10min by mass percentage, Obtain micro-cutting and help powder；
(3) micro-cutting is helped into powder and 60% ethanol by solid-liquid ratio 1g:15ml is sufficiently mixed, frequency be 40KHz, power be 100W, Temperature is supersound extraction 20min under 40 DEG C of ul-trasonic irradiation, filters extracting solution, collects to obtain filtrate；
(4) filtrate is carried out into vacuum distillation by Rotary Evaporators, reclaims ethanol extractant, obtain Semen Vitis viniferae concentrated dry powder；
(5) Semen Vitis viniferae concentrated dry powder is configured to into certain density solution to be measured, with rutin as standard substance, using aluminum sulfate colorimetric Method is detected to flavones content in extract.
2. a kind of employing micro-cutting according to claims 1 helps interaction mode to improve Semen Vitis viniferae extract flavone dissolution Method, it is characterised in that described physics auxiliary agent is sharp property material-conch meal.
CN201611184962.2A 2016-12-20 2016-12-20 Method for improving dissolution rate of grape seed extract flavones in press-shear assisted interaction mode Withdrawn CN106581318A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102517144A (en) * 2011-11-28 2012-06-27 宁夏大学 Method for extracting oil and procyanidin from grape seeds
CN104958440A (en) * 2015-05-22 2015-10-07 大连理工大学 Camellia nitidissima Chi flower extract as well as preparation method and application thereof
CN106146582A (en) * 2016-07-18 2016-11-23 唐翔 A kind of method using micro-cutting to help interaction technology assisted extraction Hesperidin

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102517144A (en) * 2011-11-28 2012-06-27 宁夏大学 Method for extracting oil and procyanidin from grape seeds
CN104958440A (en) * 2015-05-22 2015-10-07 大连理工大学 Camellia nitidissima Chi flower extract as well as preparation method and application thereof
CN106146582A (en) * 2016-07-18 2016-11-23 唐翔 A kind of method using micro-cutting to help interaction technology assisted extraction Hesperidin

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王强等: "葡萄籽粗多糖的超声波提取工艺优化及抗氧化活性", 《食品科学》 *

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