CN104490956B - A kind of total seabuckthorn flavone purifying technique - Google Patents

A kind of total seabuckthorn flavone purifying technique Download PDF

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Publication number
CN104490956B
CN104490956B CN201410844325.8A CN201410844325A CN104490956B CN 104490956 B CN104490956 B CN 104490956B CN 201410844325 A CN201410844325 A CN 201410844325A CN 104490956 B CN104490956 B CN 104490956B
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Prior art keywords
seabuckthorn flavone
total seabuckthorn
purifying technique
vegetable oil
total
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CN201410844325.8A
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CN104490956A (en
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吕君蔚
姜慧
丁显廷
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of total seabuckthorn flavone purifying technique, including step:Fructus hippophae is cleaned, drained and is clayed into power;Add ethanol solution and vegetable oil, ultrasonic extraction for a period of time, obtain extract solution after filtering;By extract solution liquid separation, water alcohol phase is obtained;Water alcohol phase is dried into powder, the total seabuckthorn flavone as purified.The present invention purifying technique obtain total seabuckthorn flavone purity it is high, simple to operate, cost is cheap, be adapted to large-scale production.

Description

A kind of total seabuckthorn flavone purifying technique
Technical field
The invention belongs to food and medicine manufacture field, is related to a kind of purifying technique of total seabuckthorn flavone.
Background technology
Hippophate flavone contains Quercetin, Isorhamnetin and Kaempferol isoreactivity composition.With hypotensive, reducing blood lipid, reduce Blood viscosity, the enhancing function such as blood vessel elasticity, antiatherosclerosis is cardiovascular and cerebrovascular disease " jinx ".It is the elderly The preferred health products of cardiovascular and cerebrovascular disease are prevented and treated, existing market demand is huge.The extraction process of present main flow is supercritical CO 2 Extraction method, cost high-purity are low.And now, traditional purifying technique is generally decocting method used by domestic pharmaceutical factory, and products therefrom is pure Degree generally below 14%.
The content of the invention
In view of the drawbacks described above of prior art, the technical problems to be solved by the invention are by relatively simple purification Technique and less expensive cost solve the problems, such as that the cost high-purity of current generally existing is low.
To achieve the above object, the invention provides a kind of total seabuckthorn flavone purifying technique, comprise the following steps:
1) fructus hippophae is cleaned, drained and clayed into power;
2) add ethanol solution and vegetable oil, ultrasonic extraction for a period of time, obtain extract solution after filtering;
3) by extract solution liquid separation, water alcohol phase is obtained;
4) water alcohol phase is dried into powder, the total seabuckthorn flavone as purified.
Wherein, fructus hippophae described in step 1) is commercially available fructus hippophae.
The concentration that ethanol solution is added in step 2) is preferably 40%-70% ethanol, and the amount of addition is preferably every gram of sand The ethanol solution of spine fruit addition 3-8 milliliters, most preferably 5 milliliters;The amount for adding vegetable oil is preferably that every gram of fructus hippophae adds 1- 1.5 milliliters of vegetable oil, most preferably 1.25 milliliters;The time of ultrasonic extraction is preferably 40-60 minutes.
The temperature of drying is preferably 40-60 DEG C in step 4).
The present invention detects the absorbance of sample using ELIASA using rutin as standard items, draws standard curve and calculates Go out the purity of total seabuckthorn flavone in sample.Testing result shows the total seabuckthorn flavone for adding the combination of vegetable oil to extract with 60% ethanol Purity reached 50% or so.The effect of wherein vegetable oil has two aspects:One side vegetable oil can be used in extraction sea-buckthorn The flavonoid substance being dissolved in organic phase, reduce loss;Another aspect vegetable oil forms fluid-tight on the surface of water alcohol phase, super The volatilization of water alcohol is prevented during sound, reduces loss.
Total seabuckthorn flavone purity that the purifying technique of the present invention obtains is high, simple to operate, cost is cheap, is adapted to extensive raw Production;And the method for purification of the present invention is applicable not only to the purification of total seabuckthorn flavone, other water and ethanol but not of being dissolved in are applied also for It is dissolved in the purification of the medicine of lipid solvent.
Therefore, the purifying technique of the further present invention is used to being dissolved in water and ethanol but the medicine insoluble in lipid solvent Purification step is:
1) medicine is cleaned, drained and clayed into power;
2) add ethanol solution and vegetable oil, ultrasonic extraction for a period of time, obtain extract solution after filtering;
3) by extract solution liquid separation, water alcohol phase is obtained;
4) water alcohol phase is dried into powder, the medicine as purified.
Embodiment
Embodiments of the invention are elaborated below:The present embodiment is carried out lower premised on technical solution of the present invention Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation Example.
Embodiment 1
2g fructus hippophaes are weighed, cleans, drain and clay into power, add the ethanol solutions of 10ml 40% and 2.5ml vegetable oil, Ultrasonic extraction 40min, extract solution is obtained after filtering.Liquid separation, water alcohol phase are evaporated, and it is the sea-buckthorn purified to obtain brown powder solid General flavone.
Embodiment 2
2g fructus hippophaes are weighed, cleans, drain and clay into power, add the ethanol solutions of 10ml 60% and 2.5ml vegetable oil, Ultrasonic extraction 40min, extract solution is obtained after filtering.Liquid separation, water alcohol phase are evaporated, and it is the sea-buckthorn purified to obtain brown powder solid General flavone.
Embodiment 3
2g fructus hippophaes are weighed, cleans, drain and clay into power, add the ethanol solutions of 10ml 70% and 2.5ml vegetable oil, Ultrasonic extraction 40min, extract solution is obtained after filtering.Liquid separation, water alcohol phase are evaporated, and it is the sea-buckthorn purified to obtain brown powder solid General flavone.
Comparative example
With decocting method conventional in the market as a comparison, specific method is;2g fructus hippophaes are weighed, cleans, drain simultaneously Clay into power, 1h is decocted in the ethanol solutions of 10ml 40%, filter, be evaporated to obtain powder.
Product purity determines
Using ELIASA, with glucose as a standard product measure absorbance, draw standard curve.From embodiment 1-3 and contrast It is each in the total seabuckthorn flavone that example obtains to weigh 20mg samples, absorbance is measured, calculates the purity of total seabuckthorn flavone in sample.Its Step is:Sampling, is 10mL with absolute ethyl alcohol constant volume;1mL constant volume solution is taken, adds 1mL 1% alchlor ethanol solution, Again 10mL is settled to absolute ethyl alcohol;Stand 10 minutes;With the absorbance at ELIASA detection 430nm.
In order to judge the validity of detection means and sensitivity, we employ standard items rutin and tested first.Mark Quasi- product be purity close to 100% sterling.We are equipped with the standard items under different diluted concentrations, and use our test hand Duan Jinhang is identified.Analyze test result to show, our detection method, can effectively identify the various concentrations of standard items. The standard items curve of acquisition is Y=0.4419X+0.0379, R2=0.9984 (X is sample purity, and Y is spectrophotometric value).From On standard items curve, it is more that we may determine that the detection method that we use can efficiently and accurately detect target substance matrimony vine The content of sugar.
Product purity testing result is as shown in the table:
Sample Embodiment 1 Embodiment 2 Embodiment 3 Comparative example
Spectrophotometric value 0.173 0.257 0.208 0.095
Purity 30.6% 49.6% 38.5% 12.9%
Preferred embodiment of the invention described in detail above.It should be appreciated that one of ordinary skill in the art without Creative work can is needed to make many modifications and variations according to the design of the present invention.Therefore, all technologies in the art Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea Technical scheme, all should be in the protection domain being defined in the patent claims.

Claims (4)

1. a kind of total seabuckthorn flavone purifying technique, it is characterised in that comprise the following steps:
1) fructus hippophae is cleaned, drained and clayed into power;
2) add ethanol solution and vegetable oil, ultrasonic extraction for a period of time, obtain extract solution after filtering;
3) by extract solution liquid separation, water alcohol phase is obtained;
4) water alcohol phase is dried into powder, the total seabuckthorn flavone as purified, wherein,
It is 40%-70% that ethanol solution concentration is added in step 2), and the amount of the ethanol solution of addition adds 3-8 for every gram of fructus hippophae The ethanol solution of milliliter,
The amount that vegetable oil is added in step 2) adds 1-1.5 milliliter vegetable oil for each gram of fructus hippophae.
2. total seabuckthorn flavone purifying technique according to claim 1, it is characterised in that the time of ultrasonic extraction in step 2) For 40-60 minutes.
3. total seabuckthorn flavone purifying technique according to claim 1, it is characterised in that the temperature of drying is in step 4) 40-60℃。
4. the total seabuckthorn flavone of the total seabuckthorn flavone purifying technique purification according to claim any one of 1-3.
CN201410844325.8A 2014-12-25 2014-12-25 A kind of total seabuckthorn flavone purifying technique Expired - Fee Related CN104490956B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1451658A (en) * 2003-05-20 2003-10-29 傅建熙 Method for extracting seabuckthorn fruit total flavonoids by three-solvent system
CN102308987A (en) * 2011-06-27 2012-01-11 新疆科宇科技有限公司 Production method for extracting glucoside type seabuckthorn flavones from sea-buckthorn leaf

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1451658A (en) * 2003-05-20 2003-10-29 傅建熙 Method for extracting seabuckthorn fruit total flavonoids by three-solvent system
CN102308987A (en) * 2011-06-27 2012-01-11 新疆科宇科技有限公司 Production method for extracting glucoside type seabuckthorn flavones from sea-buckthorn leaf

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
微波辅助提取沙棘总黄酮的工艺研究;冯纪南等;《安徽农业科学》;20111231(第26期);15952-15954 *

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