CN1500794A - Rose hip general extract and producing technology thereof - Google Patents

Rose hip general extract and producing technology thereof Download PDF

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Publication number
CN1500794A
CN1500794A CNA021525595A CN02152559A CN1500794A CN 1500794 A CN1500794 A CN 1500794A CN A021525595 A CNA021525595 A CN A021525595A CN 02152559 A CN02152559 A CN 02152559A CN 1500794 A CN1500794 A CN 1500794A
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China
Prior art keywords
rose hip
controlled
liquid
ethanol
leaf
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Pending
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CNA021525595A
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Chinese (zh)
Inventor
姚德坤
***
姚德利
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GREAT XINGAN MOUNTAINS LINGEBEI ORGANIC FOOD CO Ltd
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GREAT XINGAN MOUNTAINS LINGEBEI ORGANIC FOOD CO Ltd
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Priority to CNA021525595A priority Critical patent/CN1500794A/en
Publication of CN1500794A publication Critical patent/CN1500794A/en
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Abstract

The present invention is the technological process of producing dahurian rose fruit total extractive with dahurian rose fruit as material and the dahurian rose fruit total extractive including dahurian rose fruit saponin, dahurian rose fruit flavone and methyl pyranyl glucogallate. The production process of dahurian rose fruit total extractive includes the steps of crushing dahurian rose fruit, reflux extraction of the fruit powder, decoction of dahurian rose leaf and stem, concentration, adsorption, desorption, re-concentration and spary drying.

Description

Rose hip general extractive and production technology thereof
The present invention relates to a kind of production technology of rose hip general extractive and the rose hip general extractive (rose hip saponin, rose hip flavones, glucopyanosyl base methyl gallate) that obtains of method thus.
Rose hip is a rosaceous plant, be Rosa bella again, thorn rose rose, formal name used at school ROSadavurica is born in the hillside shrubbery, in the shaw, river bank and forest land, the florescence 6-7 month, the fruit phase 8-9 month, national storage capacity surely belongs to the forest zone, Daxing'an Mountainrange than horn of plenty, and owing to be to be grown in the forest zone, non-environmental-pollution almost detects this fruit through science and has invigorating the spleen and regulate the flow of vital energy effects such as nourishing blood for regulating menstruation, be rich in multiple biological activity, its main chemical compositions is multiple triterpenic acid, flavones and glucopyanosyl base methyl gallate, silver section glucoside etc.
Purpose of the present invention: being to provide a kind of fruit with rose hip, stem, leaf is raw material, produces the novel method of rose hip general extractive.
Another object of the present invention: be to provide a kind of rose hip general extractive of producing by production method of the present invention (rose hip saponin, rose hip flavones, glucopyanosyl base methyl gallate).
By the production technique of extraction and absorption, and mass-produce rose hip general extractive by this technology with pharmaceutical use.
Advantage of the present invention;
1, the rose hip general extractive was used extraction using alcohol in the past, and acid-alkali treatment and post layer separate, but are not suitable for suitability for industrialized production.
2, terpene acid, flavones, alkaloid and gallic acid extraction process have been done a large amount of cut-and-try works, select alcohol reflux for use, concentrating under reduced pressure is selected the isolating method of macroporous resin for use, with flavones in the extract, phenol one-tenth, alkaloid, amino acid are controlling index, adopt the high-efficient liquid phase color popularize law to detect, can obtain the rose hip general extractive of quality and stable yield, yield is 0.05-0.07%, and the total extract effective component content is more than 25%.
3, rose hip is very abundant at the Daxing'an Mountainrange reserves, and year storage capacity has great exploitation and is worth more than 100,000 tons.
4, with the rose hip general extractive of explained hereafter of the present invention, the effective component content height improves 15 percentage points than common process, and production cost reduces 1/3 than common process, therefore has business development and is worth.
The present invention relates to a kind of method of utilizing rose hip to produce the rose hip general extractive, may further comprise the steps:
1, pulverize:
(1) get ripe rose hip, with its fragmentation, grinding particle size is controlled at about 60 orders with crusher, becomes the fruit powder.
(2) get rose hip footpath leaf (tip 15cm) and be cut into medicine section about 15mm.
2, fruit powder refluxing extraction
With the fruit powder that the epimere operation has been pulverized, be loaded in the multi-function extractor with 95% alcohol reflux 10 times, each 1.5h-2h, solvent consumption be 8-10 doubly, extracting liquid filtering, merging filtrate is called A liquid.
Stem, the fried extraction of leaf place multi-function extractor with stem, leaf,, filter then decocting under 80 ℃ of conditions about 2h with 8 times water, and filter residue decocts about 3h with 5 times water again, merge decoction filtrate then and are called B liquid.
3, concentrate: A liquid and the merging of B liquid are concentrated, reclaim the ethanol temperature simultaneously and be controlled at about 60 ℃, striking point is 30 degree Beaume, does not have the alcohol flavor.
4, absorption: concentrated solution is added the suitable quantity of water dilution, suction filtration, filtrate is added on the macroporous absorption post of having handled well adsorbs, and rate of adsorption is controlled at 4BV/h, till saturated.
5, various solvent is washed the macroporous absorption post, and desorption rate is controlled at 4BV/V just can wash the inhomogeneity Chemical Composition.
(1) washing: wash with water earlier, can wash polysaccharide, monose, tannin, oligose this moment.Prevent that with thin layer inspection inspection saponin from washing.Sugar: with 2-Cai phenol strong sulfuric acid response, acidic component detects with 1% to C13 ethanol liquid.
Whether (2) 30% ethanol are washed, and the washing back washes saponin with 30% above ethanol, detect saponin with thin layer and wash.
(3) 70% ethanol are washed: after washing, 30% alcohol washes flavones with 70% aqueous solution again, and behind the phenol thing, amino acid, flavones reacts with hydrochloric acid one iron powder, and 1%, Alcl3 ethanol liquid, amino acid ninhydrin reaction.
6, concentrate: above-mentioned 30% pure washing lotion and 70% pure washing lotion are mixed, carry out cryoconcentration then, reclaim ethanol simultaneously, temperature is controlled at about 60 ℃-80 ℃ when concentrating, and striking point is 20 Baumes.
7, spraying drying: the concentrated solution behind the above-mentioned recovery ethanol is carried out drying, and inlet temperature is controlled at 160-190 ℃, and temperature out is controlled at 60-80 ℃, and air-pressure controlling is at 0.045mpa, and pure liquid detects.Get pale or white powder, be the rose hip general extractive, its index is as follows:
9, packing: the good powdery rose hip of drying general extractive is carried out metering packing.
The invention still further relates to the rose hip general extractive (rose hip saponin, rose hip flavones, glucopyanosyl base methyl gallate) that obtains by production method of the present invention.
According to the present invention, by the rose hip general extractive that production method of the present invention obtains, its effective component content is between 25%-95%.Rose hip general extractive effective ingredient of the present invention refer to rose hip saponin, rose hip flavones, glucopyanosyl base methyl gallate one of them or all, its index is as follows:
1. contain the rose hip saponin, phenolic substance, flavones etc. are mixed with effective constituent and account for this product 25-95%.
2. yield is 0.06%
3. water ratio is :≤5%
Below implement profit with the best and further specify the present invention:
1, pulverize:
A) get ripe rose hip 100kg, its broken grinding particle size is controlled at about 60 orders, become the fruit powder with crusher.
B) get rose hip footpath leaf (tip 15cm) 100kg and be cut into medicine section about 15mm.
2, fruit powder refluxing extraction
With the fruit powder 100kg that the epimere operation has been pulverized, be loaded in the multi-function extractor with 95% alcohol reflux 10 times, each 1.5h-2h, solvent consumption be 8-10 doubly, extracting liquid filtering, merging filtrate is called A liquid.
3, stem, the fried extraction of leaf
100kg stem, leaf are placed multi-function extractor, decoct 2h with 8 times water under 80 ℃ of conditions, filter then, filter residue decocts 3h again with 5 times water, merges decoction filtrate then and is called B liquid.
4, concentrate: A liquid and B liquid are merged amount to 1000kg and concentrate, reclaim the ethanol temperature simultaneously and be controlled at about 60 ℃, striking point is 30 degree Beaume, does not have the alcohol flavor.
5, absorption: concentrated solution is added the suitable quantity of water dilution, suction filtration, filtrate is added on the macroporous absorption post of having handled well adsorbs, and rate of adsorption is controlled at 4BV/h.
6, wash the macroporous absorption post with various solvent, till saturated, just can wash the inhomogeneity Chemical Composition.
A) washing: wash with water earlier, can wash polysaccharide when last, monose, tannin, oligose.Prevent that with approaching to examine to order saponin from washing.Sugar: with 2-Cai phenol strong sulfuric acid response, acidic component detects with 1% to C13 ethanol liquid.
B) 30% ethanol is washed: the washing back washes saponin with 30% above ethanol, detects saponin with thin layer and whether washes the about 500kg of this alcohol washing lotion.
70% ethanol is washed: after washing, 30% alcohol washes flavones with 70% aqueous solution again, and behind the phenol thing, amino acid, flavones reacts with hydrochloric acid one iron powder, and 1%, Acl3 ethanol liquid, amino acid terpene three acid-responss, the about 500kg of this alcohol washing lotion.
7, concentrate: above-mentioned 30% pure washing lotion and 70% pure washing lotion are mixed, amount to 1000kg, carry out cryoconcentration then, reclaim ethanol simultaneously, temperature is controlled at about 60 ℃-80 ℃ when concentrating, and concentrated fusing point is 20 Baumes, and this concentrated solution is approximately 200kg.
8, spraying drying: the 200kg concentrated solution behind the above-mentioned recovery ethanol is carried out drying, and inlet temperature is controlled at 160-190 ℃, and temperature out is controlled at 60-80 ℃, and air-pressure controlling detects at 0.045mp alcohol liquid.Get light yellow or white powder, be the rose hip general extractive, its index is as follows:
9, packing: with the good powdery rose hip of drying general extractive metering packing into.The finished product that obtained by production method of the present invention are that its quality index of rose hip general extractive (rose hip saponin, rose hip flavones, glucopyanosyl base methyl gallate) is as follows:
1, physical and chemical index:
Color and luster: faint yellow, shallow white
Shape: Powdered
Solvability: be dissolved in water fully
Purity: do not have precipitation, inclusion-free
Rose hip general extractive effective ingredient (rose hip saponin, rose hip flavones, glucopyanosyl base methyl gallate) content: 25%-95%
Moisture % :≤5
Ash content % :≤0.05
Arsenic (As) % :≤0.0001
Plumbous (Pb) % :≤0.0003
2, microbiological indicator:
Total plate count:<100/g
Mould:<100/g
Salmonellas: must not detect
Intestinal bacteria: must not detect

Claims (8)

  1. A kind of rose hip general extractive production technology and the rose hip general extractive (rose hip saponin, rose hip flavones, glucopyanosyl base methyl gallate) that obtains of method thus.It is characterized in that:
    1, pulverize:
    (1) get ripe rose hip, with its fragmentation, grinding particle size is controlled at about 60 orders with crusher, and it is standby to become the fruit powder.
    (2) it is standby to get the medicine section that is cut into about 15mm in rose hip footpath leaf (tip 15cm).
  2. 2, fruit powder refluxing extraction
    With 95% alcohol reflux fruit powder 10 times, each 1.5h-2h, solvent consumption be 8-10 times of fruit powder, extracting liquid filtering, and merging filtrate is called A liquid.
  3. 3, stem, the fried extraction of leaf
    Stem, leaf are placed multi-function extractor, decocting under 80 ℃ of conditions about 2-4h with 8 times of water to the cauline leaf volume, filtration then, filter residue decocts about 3-5h with 5 times water again, merges decoction filtrate then and is called B liquid.
  4. 4, concentrate: A liquid and the merging of B liquid are concentrated, and temperature is controlled at about 60 ℃-80 ℃, and striking point is 30 degree Beaume, does not have the alcohol flavor.
  5. 5, absorption: concentrated solution is added the suitable quantity of water dilution, suction filtration, filtrate is added on macroporous adsorbent resin (commercially available) post of having handled well adsorbs, and rate of adsorption is controlled at 4-5BV/h, till saturated.
  6. 6, desorb:
    (1) washing: wash with water earlier, can wash polysaccharide, monose, tannin, oligose this moment.
    (2) 30% ethanol are washed: the washing back washes the rose hip saponin with 30% above ethanol.
    (3) 70% ethanol are washed: wash flavones with 70% ethanolic soln again after 30% alcohol is washed.
  7. 7, concentrate: 30% pure washing lotion and 70% pure washing lotion mixing back are concentrated, and temperature is controlled at about 60 ℃-80 ℃, and striking point is 20 Baumes.
  8. 8, spraying drying: concentrated solution is carried out drying, and inlet temperature is controlled at 160-190 ℃, and temperature out is controlled at 60-80 ℃, and air-pressure controlling is at 0.045mpa.Get shallow white or buff powder, be the rose hip general extractive, metering packing dispatches from the factory then.
CNA021525595A 2002-11-18 2002-11-18 Rose hip general extract and producing technology thereof Pending CN1500794A (en)

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Application Number Priority Date Filing Date Title
CNA021525595A CN1500794A (en) 2002-11-18 2002-11-18 Rose hip general extract and producing technology thereof

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CN1500794A true CN1500794A (en) 2004-06-02

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102796066A (en) * 2012-08-31 2012-11-28 云南民族大学 Flavone compound and preparation method and application thereof
CN104069209A (en) * 2014-06-12 2014-10-01 陕西辉胜新兴农业科技发展有限公司 Preparation method of wild rosa xanthina fruit crude general flavone for treating coronary heart disease and hyperlipidaemia
CN104126833A (en) * 2014-06-30 2014-11-05 吉林化工学院 Rosa davurica functional beverage preparation method
CN105997702A (en) * 2016-07-05 2016-10-12 上海相宜本草化妆品股份有限公司 Dahurian rose fruit extract and application thereof
CN104147179B (en) * 2014-06-30 2017-05-10 吉林化工学院 Wild rose hip effervescent tablet and preparation method thereof
CN106975076A (en) * 2017-04-14 2017-07-25 青岛市第三人民医院 A kind of pepsin coating tablet containing Chinese medical extract
CN113461747A (en) * 2021-07-12 2021-10-01 吉林化工学院 New compound with hypoglycemic activity in 2 rosa davurica fruits and preparation method thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102796066A (en) * 2012-08-31 2012-11-28 云南民族大学 Flavone compound and preparation method and application thereof
CN102796066B (en) * 2012-08-31 2014-09-03 云南民族大学 Flavone compound and preparation method and application thereof
CN104069209A (en) * 2014-06-12 2014-10-01 陕西辉胜新兴农业科技发展有限公司 Preparation method of wild rosa xanthina fruit crude general flavone for treating coronary heart disease and hyperlipidaemia
CN104126833A (en) * 2014-06-30 2014-11-05 吉林化工学院 Rosa davurica functional beverage preparation method
CN104126833B (en) * 2014-06-30 2015-08-19 吉林化工学院 A kind of preparation method of rose hip functional beverage
CN104147179B (en) * 2014-06-30 2017-05-10 吉林化工学院 Wild rose hip effervescent tablet and preparation method thereof
CN105997702A (en) * 2016-07-05 2016-10-12 上海相宜本草化妆品股份有限公司 Dahurian rose fruit extract and application thereof
CN106975076A (en) * 2017-04-14 2017-07-25 青岛市第三人民医院 A kind of pepsin coating tablet containing Chinese medical extract
CN113461747A (en) * 2021-07-12 2021-10-01 吉林化工学院 New compound with hypoglycemic activity in 2 rosa davurica fruits and preparation method thereof
CN113461747B (en) * 2021-07-12 2023-02-03 吉林化工学院 2 compounds with hypoglycemic activity in rose hip

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