CN107789383A - A kind of extraction process of Huanghua Pear branches and leaves extract - Google Patents

A kind of extraction process of Huanghua Pear branches and leaves extract Download PDF

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Publication number
CN107789383A
CN107789383A CN201610833359.6A CN201610833359A CN107789383A CN 107789383 A CN107789383 A CN 107789383A CN 201610833359 A CN201610833359 A CN 201610833359A CN 107789383 A CN107789383 A CN 107789383A
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CN
China
Prior art keywords
extraction
huanghua pear
raw material
extract solution
extraction process
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Pending
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CN201610833359.6A
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Chinese (zh)
Inventor
周伟
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Hunan Haiji Pharmaceutical Co Ltd
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Hunan Haiji Pharmaceutical Co Ltd
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Priority to CN201610833359.6A priority Critical patent/CN107789383A/en
Publication of CN107789383A publication Critical patent/CN107789383A/en
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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)
    • A61K36/48Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • 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
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • 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
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • 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
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

Abstract

A kind of extraction process of Huanghua Pear branches and leaves extract, comprises the following steps:Raw material removal of impurities, cleaning, crush;Raw material after crushing carry out the extraction of repeated ultrasonic ripple and merge extract solution;Using 0.1um ceramic membrane filter;Ultrafiltration is carried out successively using the multiple milipore filters of 10000~100000 middle-molecular-weihydroxyethyls from large to small, trapped fluid is standby, permeate is handled with the milipore filter of next molecular weight, the permeate of last time is concentrated to give concentrate with NF membrane or reverse osmosis membrane, trapped fluid containing pigment is discarded, remaining trapped fluid mixes with concentrate produces target product.The present invention makes full use of existing raw material, extraction is abundant and will not cause destruction and the fragrance loss of functional component, make coloured product and better quality after going depigmentation and heavy metal ion, using more fine and extensive, extract fully simultaneously, extraction time is short, reduces production cost, production technology is simplified, suitable for industrialized production.

Description

A kind of extraction process of Huanghua Pear branches and leaves extract
Technical field
The present invention relates to technical field of plant extraction, and in particular to a kind of extraction process of Huanghua Pear branches and leaves extract.
Background technology
Huanghua Pear is Papilionaceae Dalbergia arbor, and its timber is first-class furniture good timber, and its root heartwood is good town Pain agent, knife wound bleeding is controlled, at present mainly heartwood, other parts untapped application, but chrysanthemum of the Huanghua Pear as medicinal ingredient The branches of pears, leaf, seed and the leftover pieces of timber processing at source have use habit, and as Huanghua Pear seed is used for nti-freckle, branches and leaves are decocted It is used to wash hair after water, there is the function such as anti-dandruff, antipruritic, chrysanthemum pears leaf can then makes one with tealeaves compounding composition trophism health protection tea Health-care efficacy is obtained in drinking tea.
For plant extracts using increasingly extensively in the industries such as cosmetics, medicine and food, chrysanthemum Fructus Pyri extract is same at present Sample has very big market prospects, but the system of chrysanthemum Fructus Pyri extract is carried out according to the conventional common method extracted and separated It is standby, then often exist and extract insufficient, to obtain extract color depth, heavy metal ion content is high so that what application was limited Phenomenon, and it is at most that the active ingredient in plant is extracted by modes such as thermophilic digestions that plant extracts is applied at present, it is this Extracting mode is simple to operate, not high to equipment requirement, but is easy to the active ingredient destroyed in plant, causes volatile aroma to damage Lose, and existing ultrasonic technology accelerates extraction with that can promote plant thin broken wall, without high temperature, does not destroy some in plant The function composition of thermally labile, facile hydrolysis or oxidation characteristic, and the characteristics of security is good, and operation is simple, energy consumption is low, and And functional component includes active ingredient and the molecular weight such as the relatively large polysaccharide of molecular weight and protein in Huanghua Pear extract solution The active ingredients such as less flavones, the molecular weight ranges of the organic pigment in Huanghua Pear are generally 20000~50000, heavy metal Ion equimolecular quantity then scope typically below 100, if therefore ultrasonic assistant can be combined extract, and according to molecular size range Different principles, using membrane separation technique, reach high efficiency extraction, impurity elimination, remove harmful heavy metal ions and Fractional Collections is different The purpose of functional component, make product more fine and extensive in sector applications such as foods and cosmetics.
The content of the invention
Technical problem solved by the invention is to provide a kind of extraction process of Huanghua Pear branches and leaves extract, to solve to carry on the back The branch of the Huanghua Pear mentioned in scape technology, leaf, seed and the leftover pieces of timber processing solve Huanghua Pear and carried using insufficient Insufficient, high temperature functional component is extracted during taking, pigment and beavy metal impurity, which are not separated and removed, to be influenceed subsequently should The problem of using.
Technical problem solved by the invention is realized using following technical scheme:
A kind of extraction process of Huanghua Pear branches and leaves extract, comprises the following steps:
1) pre-treatment:Raw material are cleaned, clean, crushed;
2) ultrasonic wave extraction:Raw material after crushing are added in ultrasonic wave extraction equipment, solid-liquid ratio is arranged to 1: (5~ 10), extracted under normal temperature in a manner of water extraction or alcohol extracting and extract solution filtered to obtain after 30~60min, same condition repeat extraction 1~ 4 times, merge extract solution;
3) refined filtration:Extract solution passes through 0.1um ceramic membrane filter, takes permeate to obtain refined filtration liquid;
4) ultrafiltration:3) refined filtration liquid is entered successively using the multiple milipore filters of 10000~100000 middle-molecular-weihydroxyethyls from large to small in Row ultrafiltration, trapped fluid is standby, and permeate is handled with the milipore filter of next molecular weight, the permeate nanofiltration of last time Film or reverse osmosis membrane are concentrated to give concentrate, and the trapped fluid containing pigment is discarded, and remaining trapped fluid mixes with concentrate produces mesh Mark product.
In the present invention, 100,000,50,000 and 20,000 milipore filter is respectively adopted to refined filtration liquid ultrafiltration successively in 3) in the ultrafiltration, its In the filtered solutions of 20,000 milipore filters be concentrated to give concentrate with NF membrane or reverse osmosis membrane, merge the retention of concentrate and 50,000 milipore filters Liquid produces target product.
In the present invention, the NF membrane molecular weight is preferably 300~500.
In the present invention, the raw material include one in the leftover pieces after branch, leaf, seed and the trunk processing of Huanghua Pear Kind is several.
In the present invention, the alcohol extracting is using one or more of addition powder in methanol, ethanol, acidic ethanol, acidic methanol Extracted in raw material after broken, the acidic ethanol or acidic methanol using sulfuric acid, hydrochloric acid, phosphoric acid, lactic acid, citric acid, One or more progress acidity adjustments in oxalic acid.
In the present invention, the ultrasonic wave extraction is to add the raw material after crushing in ultrasonic wave extraction equipment, solid-liquid ratio 1: 5 is arranged to, filters to obtain extract solution after extracting 45min under normal temperature in a manner of water extraction, same condition repeats extraction and closed afterwards three times And extract solution.
In the present invention, the ultrasonic wave extraction is to add the raw material after crushing in ultrasonic wave extraction equipment, solid-liquid ratio 1: 5 is arranged to, filters to obtain extract solution after extracting 45min under normal temperature in a manner of 80% ethanol extracts, same condition repeats to carry Take and merge extract solution afterwards three times.
Beneficial effect:A kind of extraction process of Huanghua Pear branches and leaves extract of the present invention, makes full use of Huanghua Pear Leftover pieces after branch, leaf, seed and trunk processing carry out effective component extracting, and the various pieces of Huanghua Pear have been carried out fully Utilize, avoid the waste of raw material, while repeatedly fully extracted using ultrasonic wave after the raw material crushing of the present invention, without height Temperature operation, the function composition of thermally labile in Huanghua Pear, facile hydrolysis or oxidation characteristic is not destroyed, and security is good, operation letter It is single it is easy, energy consumption is low, by extract solution by refined filtration, ultrafiltration and concentration, by the color in extract solution while reservation function composition Element and heavy metals removal, and each trapped fluid and last concentrate can merge use and can also be used separately in the present invention, from And make the follow-up application of extract solution more it is fine and extensively.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below Specific embodiment is closed, the present invention is expanded on further.
Specific embodiment 1
1) 100kg Huanghua Pear impurity removings are taken, fine powder are ground into after cleaning, after all trunk processing of Huanghua Pear raw material Leftover pieces, by the raw material input ultrasonic extraction device after crushing, add 500L water ultrasonic extraction 45min, collect extract solution, the 2nd, 3 extractions respectively add 500L water ultrasonic extraction 45min again, merge gained extract solution three times;
2) extract solution 1) is obtained into refined filtration liquid with 0.1 μm of ceramic membrane filter.
3) ultrafiltration 2) will be carried out with the milipore filter of molecular weight 100,000,50,000,20,000 successively, collects 50,000 molecular weight trapped fluids, and The permeate of 20,000 molecular weight is concentrated to give concentrate with the NF membrane of 300 molecular weight, merges trapped fluid and concentrate is obtained and finally produced Product.
Specific embodiment 2
1) 100kg Huanghua Pear impurity removings are taken, fine powder is ground into after cleaning, are put into ultrasonic extraction device, Huanghua Pear is former Expect for Huanghua Pear seed, add 800L water ultrasonic extraction 30min, collect extract solution, the 2nd, 3 extraction is again respectively plus 500L water ultrasounds carry 45min is taken, collects and merges extract solution.
2) extract solution 1) is obtained into refined filtration liquid with 0.1 μm of ceramic membrane filter.
3) ultrafiltration 2) will be carried out with the milipore filter of molecular weight 100,000,50,000,20,000 successively, wherein the permeate of 20,000 molecular weight Concentrated with reverse osmosis membrane, collect 50,000 molecular weight trapped fluids and reverse osmosis membrane concentrate respectively as final product.
Specific embodiment 3
1) 100kg Huanghua Pear impurity removings are taken, fine powder is ground into after cleaning, are put into ultrasonic extraction device, Huanghua Pear is former Branch, leaf, seed random combine in material, add 500L80% ethanol (interior plus 3% citric acid) ultrasonic extraction 45min, collect extraction Liquid, the 2nd, 3 extraction respectively add 500L water ultrasonic extraction 45min, collect and merge extract solution again.
2) extract solution 1) is obtained into refined filtration liquid with 0.1 μm of ceramic membrane filter.
3) refined filtration liquid in 2) is subjected to ultrafiltration with the milipore filter of molecular weight 100,000,50,000,20,000 successively, wherein 20,000 molecular weight Permeate concentrated with the NF membranes of 300 molecular weight, 50,000 molecular weight trapped fluids and nanofiltration concentrate in collecting 3), produce most Finished product.
Specific embodiment 4
1) 100kg Huanghua Pear impurity removings are taken, fine powder is ground into after cleaning, are put into ultrasonic extraction device, Huanghua Pear is former Expect for Huanghua Pear leaf, add 1000L80% EtOH Sonicates to extract 60min, collect extract solution, the 2nd, 3,4 extraction again respectively plus 500L water ultrasonic extraction 45min, collect extract solution.
2) extract solution 1) is obtained into refined filtration liquid with 0.1 μm of ceramic membrane filter.
3) ultrafiltration 2) will be carried out with the milipore filter of molecular weight 100,000,50,000,20,000 successively, wherein the permeate of 20,000 molecular weight Concentrate is concentrated to give with the NF membrane of 300 molecular weight, collects 50,000 molecular weight trapped fluids and concentrate respectively and respectively as final Product uses.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (7)

1. a kind of extraction process of Huanghua Pear branches and leaves extract, it is characterised in that comprise the following steps:
1) pre-treatment:Raw material are cleaned, clean, crushed;
2) ultrasonic wave extraction:Raw material after crushing are added in ultrasonic wave extraction equipment, solid-liquid ratio is arranged to 1: (5~10), Extract solution is filtered to obtain after extracting 30~60min in a manner of water extraction or alcohol extracting under normal temperature, same condition repeats extraction 1~4 time, Merge extract solution;
3) refined filtration:Extract solution passes through 0.1um ceramic membrane filter, takes permeate to obtain refined filtration liquid;
4) ultrafiltration:3) refined filtration liquid is surpassed successively using the multiple milipore filters of 10000~100000 middle-molecular-weihydroxyethyls from large to small in Filter, trapped fluid is standby, and permeate is handled with the milipore filter of next molecular weight, the permeate NF membrane of last time or Reverse osmosis membrane is concentrated to give concentrate, and the trapped fluid containing pigment is discarded, and remaining trapped fluid mixes with concentrate produces target production Thing.
A kind of 2. extraction process of Huanghua Pear branches and leaves extract according to claim 1, it is characterised in that the ultrafiltration point Not Cai Yong 100,000,50,000 and 20,000 milipore filter to refined filtration liquid ultrafiltration successively in 3), wherein the filtered solution NF membrane of 20,000 milipore filters Or reverse osmosis membrane is concentrated to give concentrate, the trapped fluid for merging concentrate and 50,000 milipore filters produces target product.
A kind of 3. extraction process of Huanghua Pear branches and leaves extract according to claim 1 or 2, it is characterised in that the nanofiltration Membrane molecule amount is 300~500.
A kind of 4. extraction process of Huanghua Pear branches and leaves extract according to claim 1 or 2, it is characterised in that the former material Material includes the one or more in the leftover pieces after branch, leaf, seed and the trunk processing of Huanghua Pear.
A kind of 5. extraction process of Huanghua Pear branches and leaves extract according to claim 1 or 2, it is characterised in that the alcohol extracting Extracted in raw material after being crushed using one or more of additions in methanol, ethanol, acidic ethanol, acidic methanol, institute Acidic ethanol or acidic methanol are stated using one or more progress acidity in sulfuric acid, hydrochloric acid, phosphoric acid, lactic acid, citric acid, oxalic acid Regulation.
A kind of 6. extraction process of Huanghua Pear branches and leaves extract according to claim 1 or 2, it is characterised in that the ultrasound Ripple is extracted as adding the raw material after crushing in ultrasonic wave extraction equipment, and solid-liquid ratio is arranged to 1: 5, under normal temperature in a manner of water extraction Extract solution is filtered to obtain after extraction 45min, same condition repeats extraction and merges extract solution afterwards three times.
A kind of 7. extraction process of Huanghua Pear branches and leaves extract according to claim 1 or 2, it is characterised in that the ultrasound Ripple is extracted as adding the raw material after crushing in ultrasonic wave extraction equipment, and solid-liquid ratio is arranged to 1: 5, with 80% ethanol under normal temperature The mode of extraction filters to obtain extract solution after extracting 45min, and same condition repeats extraction and merges extract solution afterwards three times.
CN201610833359.6A 2016-09-01 2016-09-01 A kind of extraction process of Huanghua Pear branches and leaves extract Pending CN107789383A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101659794A (en) * 2009-09-27 2010-03-03 广西山云生化科技有限公司 New process for extracting high-purity gardenia yellow pigment by membrane separation and purification technology
CN103773820A (en) * 2012-10-22 2014-05-07 东北林业大学 Method for extracting, separating and purifying isoflavone active components biochanin A and genistein from dalbergia odorifera T.Chen leaves
CN105497101A (en) * 2015-12-16 2016-04-20 张家界立功旅游农业发展有限公司 Method for extracting kinds of combined extract from blueberry stems and leaves

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101659794A (en) * 2009-09-27 2010-03-03 广西山云生化科技有限公司 New process for extracting high-purity gardenia yellow pigment by membrane separation and purification technology
CN103773820A (en) * 2012-10-22 2014-05-07 东北林业大学 Method for extracting, separating and purifying isoflavone active components biochanin A and genistein from dalbergia odorifera T.Chen leaves
CN105497101A (en) * 2015-12-16 2016-04-20 张家界立功旅游农业发展有限公司 Method for extracting kinds of combined extract from blueberry stems and leaves

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
黄丽容等: ""AB-8大孔吸附树脂纯化降香总黄酮的工艺研究"", 《广东药学院学报》 *

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Application publication date: 20180313

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