CN1288162C - Process for extraction refining amygdalin - Google Patents
Process for extraction refining amygdalin Download PDFInfo
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- CN1288162C CN1288162C CN 200410012381 CN200410012381A CN1288162C CN 1288162 C CN1288162 C CN 1288162C CN 200410012381 CN200410012381 CN 200410012381 CN 200410012381 A CN200410012381 A CN 200410012381A CN 1288162 C CN1288162 C CN 1288162C
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- amygdaloside
- amygdalin
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Abstract
The present invention relates to a method for extracting and refining amygdalin, which comprises: vegetables as raw materials rich in amygdalin are pulverized into powder and made into raw material powder; the raw material powder is deoiled and degreased by using CO2 as an extracting agent at the extracting pressure of 15 to 35MPa at the temperature of 31.1 to 60DEG C; CO2 containing vegetable oil and fat is separated at reduced pressure, alcohol is added into slag powder containing the amygdalin according to the solid to liquid ratio of 1:3 to 10, stirred and filtered in a suction mode to obtain suction filter liquid; the suction filter liquid is distilled and dried to obtain a crude product of the amygdalin; the high-purity amygdalin is obtained after the crude product of the amygdalin is dissolved in ethanol, crystallized at a low temperature, filtered and dried. The present invention overcomes the disadvantages of incomplete degreasing, amygdalin decomposition caused by a localized high temperature, etc. in the processes of squeezing and deoiling. Toxic flammable solvents, such as hexane, etc., are not used in the present invention having the advantages of high product purity and simple technology.
Description
Technical field
The present invention relates to a kind of from plant material the method for extracting effective components amygdaloside, be meant the separation and refining method that from Gynocardia odorata R. Br, Europe Lee's seed, almond, peach kernel, extracts amygdaloside especially.
Technical background
Amygdaloside is with a kind of aromatic series cyanogen glycosides, is present in the seed of Flacourtiaceae Gynocardia odorata R. Br, Rosaceae Europe Lee, apricot and peach etc.Discover that amygdaloside is the effective constituent of treatment respiratory system disease, it benumbs inhibition respiratory centre system by slowly discharging prussic acid in vivo, thereby plays the effect of relievining asthma, and is widely used in Chinese traditional treatment, coughs in order to treatment etc.But a large amount of oral Semen Armeniacae Amarums, amygdaloside easily cause serious poisoning, and amygdaloside generates prunasin and almond cyanogen under the synaptase hydrolysis, and almond cyanogen instability is met heat and easily decomposed generation phenyl aldehyde and prussic acid.The intravital cytopigment enzyme of prussic acid and cell pellets ferric iron reacts, and inhibitory enzyme activity causes the histocyte respiration inhibition, even causes death.
Amygdaloside also is a kind of effective constituent for the treatment of cancer, and in the resident of the Pei Ji of island country, the incidence of cancer is very low, this and this state plants a large amount of apricots, often edible its fruit of resident is relevant with seed, and modern medicine study proves that amygdaloside has very strong lethality to cancer cells.The many cancer patientss that comprise western countries often select for use the preparation that contains amygdaloside as medicine.And these preparations have also brought many peculiar curative effects to the patient.Produce the amygdaloside extract and undoubtedly great market is being arranged aspect medicine and the healthcare products.
Nature contains the maximum Flacourtiaceae Gynocardia odorata R. Br of amygdaloside, and its content reaches 6～8%, and amygdaloside content is about 6% in Lee's seed of Europe, and amygdaloside content is about 3.0% in Semen Armeniacae Amarum and the peach kernel.Therefore extract the high purity amygdaloside with these raw materials and have application promise in clinical practice.
At present, the research of relevant amygdaloside extract is less, and CN02100460.9 begins to extract amygdaloside from Semen Armeniacae Amarum squeeze cake, and this method oil removing rate is not high, and the product purity that causes next step alcohol extraction process to obtain is not high; The high temperature extruding makes and produces Semen Armeniacae Amarum enzyme-to-substrate amygdaloside Long contact time and decompose in the while expressing process; CN02146618.1 has reported the method for extracting Europe Lee's oil from Europe Lee's seed raw material, use organic solvent extraction Europe Lee's oil such as hexane, hexane costs an arm and a leg, inflammable and explosive, industrialization safety in production difficulty, and product has higher dissolvent residual, relates to low-carbon alcohol subsequently and extracts amygdaloside, but do not provide concrete technology.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing amygdaloside by supercritical carbon dioxide extraction in conjunction with solvent extraction, crystallization.
Purpose of the present invention realizes by following scheme:
(1). the plant material that will be rich in amygdaloside is ground into 10-40 purpose meal, is prepared into raw material powder;
(2). with the raw material powder extractor of packing into, with food-class CO
2For carrying out grease to raw material powder, extraction agent removes, control extracting pressure 15～35MPa, and temperature is at 31.1～60 ℃; The carbonic acid gas that contains Vegetable oil lipoprotein flows out from the extractor top, enters the separator decompression separation and removes separating pressure 4～10MPa, 10～80 ℃ of separation temperatures;
(3). the ground-slag that contains amygdaloside is emitted from the separator bottom, adds edible ethanol by solid-to-liquid ratio 1: 3～10 in ground-slag, stirs, and suction filtration gets suction filtration liquid;
(4). suction filtration liquid gets the amygdaloside crude product through distillation, drying;
(5). in ethanol, low temperature crystallization gets the high purity amygdaloside behind the filtration drying with the amygdaloside dissolving crude product.
The aforesaid plant material that contains amygdaloside is Gynocardia odorata R. Br, Europe Lee's seed, almond or peach kernel etc.
In aforesaid (4) step solvent seasoning is common drying, vacuum-drying, spraying drying etc.
Also can use the ultrasonic wave means in aforesaid (5) step dissolution process, promote dissolving fast.
Can also directly adopt ultrasonic dissolution in aforesaid (5) step crystallization filtration drying, normal temperature leaves standstill filtration drying.
The present invention has following advantage:
(1) amygdaloside is a polar material, is not dissolved in the supercritical carbon dioxide fluid.Supercritical carbon dioxide fluid can more fully remove the fat-soluble component in the raw material.And the milling process degreasing is unclean, and residual fat-soluble composition can enter solution along with the extraction using alcohol process, and product purity is descended.Compare supercritical CO with traditional solvent
2Be green solvent, operational condition gentleness, no fire hazard free from environmental pollution, on-the-spot.
(2) contain synaptase in the plant seed simultaneously, the extruding that squeezing produces in the skimming processes and localized hyperthermia can promote contacting and reaction of synaptase and amygdaloside, cause the reduction of amygdaloside yield, and supercritical CO
2Fluid medium has gentle operational condition and higher extraction efficiency, and service temperature is low, and the extraction time is short, and the material form is constant before and after the extraction, and synaptase is in lower active condition all the time, and the amygdaloside composition in the raw material does not decompose substantially.
Embodiment
Example 1:
Get Europe Lee's seed, be ground into the 10-40 order, take by weighing raw material 200 grams, put and pass through supercritical CO in the extractor
2Carry out de-oiling behind the fluid extraction, extracting pressure 30MPa, 40 ℃ of extraction temperature, separating pressure 8MPa, 50 ℃ of separation temperatures are after 4 hours, ground-slag is drawn off by the extractor bottom, add 1200 milliliters of ethanol, divide three extractions, each 400 milliliters, merging filtrate, decompression recycling ethanol be to an amount of, 65 ℃ of vacuum-drying 3 hours, get pale brown look extract 11 grams, measuring content through the HPLC method is 55%.
Get extract 3 grams of being carried, add the small amount of ethanol dissolution filter, placed 4 ℃ of refrigerators then static 10 hours, separate out white crystals, filter, wash after drying with small amount of ethanol, get 1.3 grams, detect through HPLC, content reaches 98.0%.
Example 2:
Get Europe Lee's seed, put shearing pulverizer and be ground into the 20-40 order, take by weighing raw material 200 grams, put and pass through supercritical CO in the extractor
2Carry out de-oiling behind the fluid extraction, extracting pressure 20MPa, 60 ℃ of extraction temperature, separating pressure 9MPa, 70 ℃ of separation temperatures are after 6 hours, ground-slag is drawn off by the extractor bottom, add 1200 milliliters of ethanol, divide three extractions, each 400 milliliters, merging filtrate, decompression recycling ethanol be to an amount of, dry 3 hours of 65 ℃ of vacuum-drying, get pale brown look extract 12 grams, measuring content through the HPLC method is 50%.
The extract carried 4 grams add the small amount of ethanol ultrasonic dissolution, under the normal temperature static 1 hour then, filter white crystals, drying, 1.6 grams, detect through HPLC, content reaches 92.3%.
Example 3:
Get the Semen Armeniacae Amarum seed, put shearing pulverizer and be ground into the 20-40 order, take by weighing raw material 200 grams, put and pass through supercritical CO in the extractor
2Carry out de-oiling behind the fluid extraction, extracting pressure 32MPa, 50 ℃ of extraction temperature, separating pressure 5Mpa, 30 ℃ of separation temperatures are after 4 hours, ground-slag is drawn off by the extractor bottom, add 1500 milliliters of ethanol, divide three extractions, each 500 milliliters, merging filtrate, decompression recycling ethanol be to an amount of, 65 ℃ of vacuum-drying 3 hours, get pale brown look extract 5.5 grams, measuring content through the HPLC method is 60%.
Get extract 4 grams of being carried, add the small amount of ethanol dissolution filter, place 4 ℃ to leave standstill then 10 hours, separate out white crystals, filter, wash after drying with small amount of ethanol, get 1.8 grams, detect through HPLC, content reaches 95.4%
Embodiment 4:
Get peach kernel and put shearing pulverizer and be ground into the 10-40 order, take by weighing raw material 300 grams, put and pass through supercritical CO in the extractor
2Carry out de-oiling behind the fluid extraction, extracting pressure 25MPa, 35 ℃ of extraction temperature, separating pressure 5MPa, 20 ℃ of separation temperatures are after 4 hours, ground-slag is drawn off by the extractor bottom, add 900 milliliters of ethanol, divide three extractions, each 300 milliliters, merging filtrate, decompression recycling ethanol be to an amount of, pours into behind the white disk 65 ℃ of dryings of vacuum drier 3 hours, get pale brown look extract 5.8 grams, measuring content through the HPLC method is 58%.
Get extract 4 grams of being carried, add the small amount of ethanol dissolution filter, place 4 ℃ to leave standstill then 10 hours, separate out white crystals, filter, wash after drying with small amount of ethanol, get 2.1 grams, detect through HPLC, content reaches 93.0%.
Claims (3)
1, a kind of method of extracting refining amygdaloside is characterized in that comprising the steps:
(1). the plant material that will be rich in amygdaloside is ground into 10-40 purpose meal, is prepared into raw material powder;
(2). with the raw material powder extractor of packing into, with food-class CO
2For carrying out grease to raw material powder, extraction agent removes, control extracting pressure 15～35MPa, and temperature is at 31.1～60 ℃; The carbonic acid gas that contains Vegetable oil lipoprotein flows out from the extractor top, enters the separator decompression separation and removes separating pressure 4～10MPa, 10～80 ℃ of separation temperatures;
(3). the ground-slag that contains amygdaloside is emitted from the separator bottom, adds edible ethanol by solid-to-liquid ratio 1: 3～10 in ground-slag, stirs, and suction filtration gets suction filtration liquid;
(4). suction filtration liquid gets the amygdaloside crude product through distillation, drying;
(5). in ethanol, low temperature crystallization gets the high purity amygdaloside behind the filtration drying with the amygdaloside dissolving crude product.
2, the method for claim 1 is characterized in that the described plant material that contains amygdaloside is Gynocardia odorata R. Br, Europe Lee's seed, almond or peach kernel.
3, the method for claim 1 is characterized in that also using ultrasonic wave in described (5) step dissolution process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012381 CN1288162C (en) | 2004-07-02 | 2004-07-02 | Process for extraction refining amygdalin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012381 CN1288162C (en) | 2004-07-02 | 2004-07-02 | Process for extraction refining amygdalin |
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| CN1594340A CN1594340A (en) | 2005-03-16 |
| CN1288162C true CN1288162C (en) | 2006-12-06 |
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| CN 200410012381 Expired - Fee Related CN1288162C (en) | 2004-07-02 | 2004-07-02 | Process for extraction refining amygdalin |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1879724B (en) * | 2006-05-10 | 2010-05-12 | 西北师范大学 | A method for preparing blood fat-reducing natural product |
| CN101362782B (en) * | 2008-08-26 | 2011-09-14 | 山西百利士生物科技有限公司 | Extraction method of amygdalin |
| CN101768194B (en) * | 2009-12-31 | 2013-07-24 | 西北大学 | Method for extracting amygdalin and albumen powder from Amygdalus pedunculata pall. oil residues |
| CN102234298A (en) * | 2010-04-23 | 2011-11-09 | 华东理工大学 | Method for extracting and purifying amygdalin from peach seeds |
| CN102399622B (en) * | 2010-09-09 | 2013-01-23 | 北京市农林科学院 | Method for preparing bitter almond extract product |
| CN102399623B (en) * | 2010-09-09 | 2013-05-08 | 北京市农林科学院 | Method for preparing Cerasus humilis kernel extract |
| CN101967426A (en) * | 2010-10-15 | 2011-02-09 | 王朝臣 | Preparation process and system for ultrasonic reinforced supercritical CO2 extraction of tussah pupa oil |
| CN102850371A (en) * | 2012-09-25 | 2013-01-02 | 南京泽朗农业发展有限公司 | Method for preparing ryanodine |
| CN103214529A (en) * | 2013-05-10 | 2013-07-24 | 浙江省农业科学院 | Method for extracting amygdalin from kernel of red bayberry fruit |
| CN107927696A (en) * | 2017-11-20 | 2018-04-20 | 广东聿津食品有限公司 | A kind of preparation method of black pepper essential oil |
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