CN101768194B

CN101768194B - Method for extracting amygdalin and albumen powder from Amygdalus pedunculata pall. oil residues

Info

Publication number: CN101768194B
Application number: CN 200910254652
Authority: CN
Inventors: 申烨华; 李聪; 张应龙; 李冰; 范云玺
Original assignee: Northwest University
Current assignee: Northwest University
Priority date: 2009-12-31
Filing date: 2009-12-31
Publication date: 2013-07-24
Anticipated expiration: 2029-12-31
Also published as: CN101768194A

Abstract

The invention discloses a method for extracting amygdalin and albumen powder from Amygdalus pedunculata pall. oil residues, which comprises the following steps of: (1) extracting amygdalin by adopting Amygdalus pedunculata pall. oil residues as raw materials with a solvent backflow method and recrystallizing a rough product to obtain a pure product; (2) extracting albumen from the residues after the amygdalin is extracted by using an alkali dissolving and acid precipitating method; drying and then obtaining the albumen powder. The extracted oil residues are used as the raw materials, the amygdalin is refluxed and extracted, the albumen is extracted by using the alkali dissolving and acid precipitating method, and products of the amygdalin and the albumen powder can be obtained; and the utilization of the Amygdalus pedunculata pall. oil residues organically combines desert control and the comprehensive development of the products and has wide development prospect.

Description

The Amygdalus pedunculata dregs of fat extract the method for Vitamin B17 and protein powder

Technical field

The present invention relates to a kind of method of from the Amygdalus pedunculata dregs of fat, extracting Vitamin B17 and protein powder.

Background technology

Amygdalus pedunculata has another name called fruit or seed of Szechwan Cherry (Amygdalus pcdunculata Pall.), it is the machaka of Rosaceae Amygdalus, because the desert is flooded and artificial destruction, distribute scattered and day by day the disappearance, 1992 version " Inner Mongol rare or endangered species collection of illustrative plates " Amygdalus pedunculata has been classified as the secondary threatened plant.Amygdalus pedunculata is as outside checking winds and fixing drifting sand, and its kernel oleaginousness is 45%～58%, can make it become the first-selected seeds of administering northern Desert Area development woody oleiferous plants base.Amygdalus pedunculata mainly in desert and the plantation of desertification area, away from three-waste pollution source, city, is subjected to the pollution of chemical fertilizer and agricultural chemicals etc. hardly, can develop into organic edible oil.In addition, the Amygdalus pedunculata kernel oil expression back dregs of fat are rich in Vitamin B17 and protein.

Vitamin B17 (amygdalin, amygdalin Amygdalins, almond cyanogen-β-gentiobioside), belong to aromatic series cyanogen glucoside, widely distributed in vegitabilia, wherein the content with rosaceous plant (apricot, peach, Lee) seed is the highest, and structural formula is benzene hydroxyl second cyanogen-β-D-glucose-6-β-D-glycoside, and its hydrolysis under the effect of glucosaccharases such as synaptase and prunase generates wild cherry skin glucoside and almond cyanogen, latter's instability is met heat and is easily decomposed generation phenyl aldehyde and prussic acid (HCN).Mostly external in recent years research is to concentrate on oncology pharmacology research, toxicity test research and other purposes.Vitamin B17 has antimutagenic effect, can reduce the quantity of the micronucleus polychromatic erythrocyte that is caused by Sulpyrine, Metronidazole plain BP.98 99, mitomycin etc.; Vitamin B17 also has the effect of the diabetes that prevention and treatment antitumour drug alloxan cause.Vitamin B17 is now as a kind of composition of treatment dental plaque medicine, produces to be a kind of preparation.The phenyl aldehyde that the Vitamin B17 hydrolysis generates is through benzoic condensation enzyme effect generation st-yrax, and st-yrax has analgesic activity, so it is bitter to remove slight illness with Semen Armeniacae Amarum treatment advanced liver cancer, and anodyne is obeyed in even not using of having.

Protein powder is a kind of rich in proteins, carbohydrate, multivitamin and mineral substance, has the very product formulation of high nutritive value, mainly is that the dregs of fat after extracting oil from oil crops are produced.Extracting method commonly used has organic solvent precipitation method, chemical coagulation process, cold method, alkali extraction and acid precipitation method etc.Organic solvent precipitation method and chemical coagulation process reclaim the proteic while at the adding chemical reagent, introduce new pollution, and cost increases.The shortcoming of cold method maximum is exactly that extraction yield is low.The alkali extraction and acid precipitation method is low because of cost, and the protein powder that obtains is Powdered, and is dry fine and smooth, is faint yellow, so application is more extensive.Studying more is to produce peanut protein powder from peanut, and is applied in the processing of numerous food product as the Food Quality modifying agent.

When administering desertification, with the desertification regional development is the edible oil base, and set up the industrial chain of plant resources comprehensive utilization, plantation, industrialization development and suitability for industrialized production are organically combined, will make in the desertification control process and produce considerable economic, form sand industry, realize the Sustainable development of desertification treatment, and expand the land resources utilized of China, will have important society, ecology and economic benefit.

Summary of the invention

The purpose of this invention is to provide a kind of method of extracting Vitamin B17 and protein powder from the Amygdalus pedunculata dregs of fat, this method has realized the comprehensive utilization to the dregs of fat, has increased the economic development value of the dregs of fat.

Implementation procedure of the present invention is as follows:

Extracting the method for Vitamin B17 and protein powder in a kind of Amygdalus pedunculata dregs of fat, is raw material with the Amygdalus pedunculata dregs of fat, and the solvent refluxing method is extracted Vitamin B17, and crude product promptly gets pure product through recrystallization; Residue extracts albumen with the alkali extraction and acid precipitation method again after extracting Vitamin B17, obtains the protein powder product after the drying.

Extracting the described solvent of Vitamin B17 is methyl alcohol or dehydrated alcohol, and recrystallisation solvent is 92～97% ethanol or dehydrated alcohol; The alkaline solution of regulator solution pH is 0.1～1mol/l NaOH, KOH or its carbonate (Na ₂CO ₃, K ₂CO ₃) solution, acid solution is 0.1～1mol/l HCl, HNO ₃Or H ₂SO ₄Solution.

The contriver attempts using different recrystallisation solvents, and the Vitamin B17 purity that 95% ethanol primary crystallization obtains is 95.93%, and the crystal that is white in color.The Vitamin B17 purity that the dehydrated alcohol primary crystallization obtains has only 67.23%, and is micro-yellow powder.Use the pH of different acid-base solution regulator solutions, little to proteic extraction yield influence.

Concrete extracting method comprises the steps:

(1) the Amygdalus pedunculata dregs of fat and ethanol or methyl alcohol are extracted Vitamin B17 according to solid-liquid ratio (1: 6)～(1: 30) g/ml, extract 50～80 ℃ of temperature;

(2) extract end back filtered while hot, obtain filtrate and filter cake;

(3) filtrate decompression concentrate to reclaim solvent, and crude product through 92～97% ethyl alcohol recrystallizations three times, is dried to constant weight again, promptly gets the pure product of Vitamin B17;

(4) behind the filtration cakes torrefaction, press solid-liquid ratio (1: 10)～(1: 30) g/ml and add distilled water, the pH value is transferred to 8.0～12.0,, leave standstill the back suction filtration, collect filtrate and filter cake then 20～60 ℃ of extractions with 0.1～1mol/L NaOH, KOH or its carbonate solution;

(5) use 0.1～1mol/LHCl, HNO again ₃Or H ₂SO ₄Solution transfers to 3.0～6.0 with filtrate pH value, leave standstill, centrifugal, press solid-liquid ratio (1: 5)～(1: 100) g/ml and add distilled water, return adjust pH to neutral with 0.1～1mol/L NaOH, KOH or its carbonate solution again, stirring is redissolved precipitation, promptly gets the protein powder product after the vacuum lyophilization.

Through Institute of Analysis of Northwest University and spectrum Buddhist nun test center Vitamin B17, protein powder product are detected, the Vitamin B17 product purity reaches more than 98%, satisfies market-oriented needs.Protein content is 95.79% in the protein powder, belongs to high protein powder (protein content is more than 80%).Contain 18 seed amino acids that exist in the plant, total amino acid content is 82.44g/100g.Wherein 8 kinds of human bodies can not synthetic indispensable amino acid (Methionin, tryptophane, methionine(Met), leucine, Isoleucine, phenylalanine, Threonine and Xie Ansuan) total amount be 21.68g/100g, account for 26.30% (seeing Table 1) of total amino acid content.In addition, the Amygdalus pedunculata protein powder also contains the mineral element of multiple needed by human such as Ca, Mg, P, Fe, K, does not contain Cd, As, Pb (seeing Table 2).

Amino acid is formed and content (g/100g) in table 1 protein powder

Annotate: " * " is indispensable amino acid

Micronutrient levels in table 2 protein powder (μ g/g)

The contriver finds that the extraction order of Vitamin B17 and protein powder is extremely important.If adopt the alkali extraction and acid precipitation method to extract albumen earlier, change of configuration can take place in then naturally occurring Vitamin B17, influences its effect.And under optimum process condition, adopt the alcohol reflux Vitamin B17 earlier, and adopt the alkali extraction and acid precipitation method to extract albumen again, gained Vitamin B17 maintenance native conformation and purity are higher, and total recovery is 43.07%.Protein content is higher in the protein powder, and total recovery is 41.52%, and nutritive ingredient-amino acid and mineral element content are abundant.

Advantage of the present invention:

Use the oil expression back dregs of fat to be raw material, first refluxing extraction Vitamin B17 adopts the alkali extraction and acid precipitation method to extract albumen again, can obtain Vitamin B17, protein powder product; The utilization of the Amygdalus pedunculata dregs of fat will administer the desert and the product comprehensive exploitation organically combines, and has vast potential for future development.

Description of drawings

Fig. 1 is for extracting Vitamin B17 and preparation protein powder process flow sheet.

Embodiment

As shown in Figure 1, in the 250ml three-necked bottle of reflux condensing tube, mechanical stirrer is housed, add the 15g Amygdalus pedunculata dregs of fat, dehydrated alcohol 150ml is heated with stirring to 70 ℃, continues about 60min.Extract and finish the back filtered while hot, obtain filtrate and filter cake.Filtrate decompression is concentrated into the dried crude product that obtains.

Press solid-liquid ratio and add 95% ethanol at 1: 20, heating for dissolving, room temperature leave standstill the 24h crystallization.Filter, filter cake is through 105 ℃ of dryings, and the Vitamin B17 product purity is 95.93%, uses 95% alcohol crystal 2 times again, and the Vitamin B17 product purity can reach more than 98%, and total recovery is 43.07%.

To carry filter cake natural air drying behind the Vitamin B17, accurately take by weighing 10.00g powder (protein content 49.28%) in the 500ml beaker, add distilled water at 1: 15 by solid-to-liquid ratio, with 0.5mol/l NaOH solution the pH value is transferred to 9.0, extract 30min 40 ℃ of stirred in water bath then, leave standstill the back suction filtration, collect filtrate and filter cake.Protein content is 11.32mg/ml in the Xylene Brilliant Cyanine G method mensuration extracting solution, and extraction rate of protein is 57.43%.Transfer to about 4.5 with the pH value of 0.5mol/l HCl solution again extracting solution.Leave standstill 30min, the centrifugal 10min of whizzer 5000r/m presses solid-liquid ratio and adds distilled water at 1: 10, returns adjust pH to 7.0 with 0.5mol/l NaOH solution again, stirs precipitation is redissolved, and promptly gets the protein powder product after the vacuum lyophilization.The protein powder total recovery is 41.52%, and protein content is 95.79%.

Claims

1. the Amygdalus pedunculata dregs of fat extract the method for Vitamin B17 and protein powder, it is characterized in that comprising the steps:

(1) the Amygdalus pedunculata dregs of fat and ethanol or methyl alcohol are extracted Vitamin B17 according to solid-liquid ratio 1:6 ~ 1:30 g/ml, extract 50 ~ 80 ℃ of temperature;

(2) extract end back filtered while hot, obtain filtrate and filter cake;

(3) filtrate decompression concentrates and reclaims solvent, and crude product through 92～97% ethyl alcohol recrystallizations, is dried to constant weight again, promptly gets the pure product of Vitamin B17;

(4) behind the filtration cakes torrefaction, press solid-liquid ratio 1:10 ~ 1:30 g/ml and add distilled water, the pH value is transferred to 8.0 ~ 12.0,, leave standstill the back suction filtration, collect filtrate and filter cake then 20 ~ 60 ℃ of extractions with 0.1 ~ 1mol/L NaOH or KOH solution;

(5) use 0.1 ~ 1mol/L HCl, HNO again ₃Or H ₂SO ₄Solution transfers to 3.0 ~ 6.0 with filtrate pH value, leaves standstill, centrifugal, presses solid-liquid ratio 1:5 ~ 1:100 g/ml and adds distilled water, uses 0.1 ~ 1mol/L NaOH or KOH solution to return adjust pH to neutral again, stirs precipitation is redissolved, and promptly gets protein powder after the vacuum lyophilization.