CN102399623A - Method for preparing Cerasus humilis kernel extract - Google Patents
Method for preparing Cerasus humilis kernel extract Download PDFInfo
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Abstract
The invention discloses a method for preparing a Cerasus humilis kernel extract, comprising the following steps: 1) drying Cerasus humilis kernels to let the moisture activity of the Cerasus humilis kernels be 0.10-0.70; 2) crushing until the particle size is 10-120 meshes; 3) under the condition of keeping the moisture activity the same, extracting Cerasus humilis kernel oil; and 4) carrying out separation and extraction on the Cerasus humilis kernel meal with an ethanol aqueous solution having a percentage concentration of 50-95 % to obtain amygdalin and protein from Cerasus humilis kernel. According to the invention, when crushing Cerasus humilis kernels and extracting Cerasus humilis kernel oil, the activity of amygdalase is reduced by controlling the moisture activity; when the separation and extraction of amygdalin and protein from Cerasus humilis kernel, the activity of amygdalase is reduced and excess denature of the protein from Cerasus humilis kernel is prevented by controlling the concentration and operation temperature of ethanol, thus the full utilization of the Cerasus humilis kernel oil, the protein from Cerasus humilis kernel and amygdalin is realized, and the invention lays a foundation for deep processing and comprehensive utilization of Cerasus humilis kernels.
Description
Technical field
The present invention relates to a kind of method of the Ou Liren of preparation extract.
Background technology
Europe Lee (Prunus humilis Bunge) is the rose department cherry genus machaka, is a kind of cold-resistant, drought-enduring, barren-resistant, salt tolerant alkali, adaptable wild fruit tree, is the wild seeds of China's distinctive fruit medicine dual-purpose.Europe Lee mainly is distributed in ground such as Shanxi, Liaoning, Hebei, Shandong, the Inner Mongol, northeast, Shaanxi.In three northern areas of China, in the scope of height above sea level 500-1500m, every 667m2 field planting 500 strains got into the best fruiting period in general the 3rd year, and per mu yield can reach 500-1000kg, produces fruit cycle weak point, and output is high.
The staple of Ou Liren comprises amygdaloside, Europe japanese plum seed oil and Ou Li benevolence albumen.The amygdaloside that contains 2%-5% among the Ou Liren; Amygdaloside has effects such as antitussive and antiasthmatic, antitumor, hypoglycemic and anticoagulation; It has become expelling phlegm for arresting cough agent, complementary cancer therapy drug pharmaceutically commonly used so far; In addition, treat the stagnation of the circulation of vital energy, the dry constipation of intestines, oedema turgor, bronchial asthma, oedema, beriberi, dysuria etc. with it clinically and also obtained good effect.The grease that contains 46%-74% among the Ou Liren, the unsaturated fatty acid content in the grease reaches more than 90%, contains V simultaneously
E, V
A, biologically active substance such as Supraene, sterol.The iodine number of Europe japanese plum seed oil and saponification value and general grease are approaching, but acid number and unsaponifiable matter content are very low, and near the standard of high-grade cooking oil, so the Europe japanese plum seed oil is the very high natural fats and oils of a kind of quality.Ou Liren contains the protein about 30%.The proteic amino acid composition of Ou Liren is close with Semen arachidis hypogaeae protein with Sunlover 10, but Ou Liren albumen glutamic is very high, account for nearly 1/3, far above Semen arachidis hypogaeae protein and Sunlover 10.Proteic composition of amino acid of Ou Liren and teen-age demand percentage are more approaching, and indispensable amino acid total mass mark accounts for 24.0% of total aminoacid massfraction.
People have carried out some researchs to the separation and Extraction of three kinds of staples of Ou Liren.Aspect the separation and Extraction of Europe japanese plum seed oil; Xue Yong etc. adopt normal hexane and methyl alcohol as nonpolar and polar phase; Confirmed that the optimum process condition that diphasic solvent process extracts the Europe japanese plum seed oil is: material alkane is than 1: 5, material alcohol ratio 1: 7, alkali concn 0.10%, determining alcohol 94%, 60 ℃ of temperature and time 4.5h, and this technology has also realized (the Xue Yong that removes of amygdaloside in the Ou Liren grouts when obtaining the Europe japanese plum seed oil; Chen Wei; Cheng Shuan etc. the biphasic solvent lixiviation process extracts the research [J] of Europe japanese plum seed oil. Zhengzhou Engineering College's journal, 2003,24 (1): 20-23).Because methyl alcohol has toxicity, has limited the application of Europe japanese plum seed oil at field of food, Xiao Yongmei etc. combine characteristics and the biphasic solvent leaching method of Ou Liren; Replace methyl alcohol as polar phase with ethanol; The biphasic solvent lixiviation process is extracted the Europe japanese plum seed oil studies, and propose with normal hexane and ethanol as nonpolar and optimum process condition polar phase: alcohol concn 75%, material alcohol than 1: 3, expect that alkane is than 1: 4, time 4h, 40 ℃ of temperature, alkali concn 0.15%, with this understanding; Oil extracting rate is 46.6%; In the dregs of rice VitaminB17 residual volume be 0.44% (Xiao Yongmei, Chen Wei, Wang Duorong etc. hexane-alcohol-water biphasic solvent lixiviation process extracts the research [J] of Europe japanese plum seed oil. Chinese oil; 2004,29 (4): 14-17).The improvement of this method has overcome the residue problem of methyl alcohol, has improved the using value of Europe japanese plum seed oil greatly.Organic solvent residual in Lee's oil of Europe, and Wu Suping etc. (Wu Suping. supercritical CO
2The discussion [J] of extraction Europe japanese plum seed oil processing condition. oil engineering technology, 2008 (6): 51-53) studied supercritical CO
2The production technique of extraction Europe japanese plum seed oil, this technology oil yield is high, foreign matter content is low, lighter color and can save refining procedures such as underpressure distillation and deodorization.Aspect the proteic separation and Extraction of Ou Liren, use such as Chen Wei alkali extraction and acid precipitation method is extracted Ou Liren albumen, promptly regulates the pH extremely alkaline (pH=9.5) of the Ou Liren dregs of rice powder solution of detoxification earlier with the 1mol/L sodium hydroxide solution; Soluble protein, glucide etc. are dissolved out, utilize centrifugation method to separate then and remove insoluble fiber and residue, adding an amount of 1mol/L hydrochloric acid soln in the dissolved protein soln again; Regulate pH to isoelectric point of protein; Most of protein precipitation is wherein separated out, have only a spot of protein remains to stay in the solution, spinning this moment promptly obtains protein isolates (Chen Wei; Wang Hongyan; Xue Yong etc. proteic extraction of Ou Liren and performance study [J]. Food science, 2005,26 (3): 138-141).Aspect the separation and Extraction of amygdaloside, after Ou Liren carried out high temperature, degreasing etc. and handle, adopt separation and Extraction amygdaloside the grouts of aqueous ethanolic solution after degreasing of 60%-90%.In addition, the Duan Hongdong method that also proposes to adopt wash-out after the resin absorption to the amygdaloside among the Ou Liren separate, extraction and purifying (Duan Hongdong. amygdaloside purification process [P] .200910230090 among a kind of Europe Li Ren).
As stated, people have carried out some researchs to the separation and Extraction of the Central European japanese plum seed oil of Ou Liren, Ou Liren albumen and amygdaloside.The complete utilization of Europe japanese plum seed oil, Europe Lee's albumen and three kinds of compositions of amygdaloside but above research all is unrealized; Only can utilize two kinds of compositions wherein: or utilize Europe japanese plum seed oil and Ou Li benevolence albumen (Ou Liren pulverizes preceding without pyroprocessing), or utilize amygdaloside and Europe japanese plum seed oil (Ou Liren needs through pyroprocessing before pulverizing).This be because, contain amygdalase among the Ou Liren, under the situation of Ou Liren complete form, because the division of labor locellus function of cytolemma and organoid film etc., amygdalase can not had an effect.In case Ou Liren is broken, amygdalase can contact with the substrate amygdaloside, and it is hydrolyzed to glucose, phenyl aldehyde and prussic acid, and is as shown in Figure 1.
In order to extract amygdaloside, Ou Liren need carry out pyroprocessing before pulverizing, to reach the purpose of " enzyme that goes out is protected glycosides ".But pyroprocessing causes the proteic serious sex change of Ou Liren again, has influenced proteic deep development of Ou Liren and utilization.Therefore, how to develop scientific and reasonable, a simple and easy to do processing technology routine, realize the complete utilization of Europe japanese plum seed oil, Ou Liren albumen and amygdaloside, need the difficult problem of solution in having become the Ou Liren intensive processing and having fully utilized badly.
Summary of the invention
The method that the purpose of this invention is to provide a kind of Ou Liren of preparation extract.
A kind of method for preparing the Ou Liren extract provided by the invention comprises the steps:
1) Ou Liren is carried out drying, making the water-activity of said Europe Li Ren is 0.10-0.70, obtains dried Europe Li Ren;
2) be under the condition of 0.10-0.70 in the water-activity that keeps said dried Europe Li Ren, said dried Europe Li Ren be crushed to the 10-120 order, the Ou Liren after obtaining pulverizing;
3) water-activity of the Ou Liren after keeping said pulverizing is under the condition of 0.10-0.70, extracts the Europe japanese plum seed oil among the Ou Liren after the said pulverizing, obtains the said Europe japanese plum seed oil and the Ou Li benevolence dregs of rice;
4) use mass percentage concentration the said Europe Li Ren dregs of rice to be carried out separation and Extraction, obtain amygdaloside and Ou Li benevolence albumen as the aqueous ethanolic solution of 50%-95%; In the said extraction step, temperature is 5-60 ℃;
Said Europe Li Ren extract is selected among a, b and the c three kinds, any two kinds or any one, and wherein, said a is a said step 3) gained Europe japanese plum seed oil, and said b is said step 4) gained amygdaloside, and said c is a said step 4) gained Europe Li Ren albumen.
This method steps 1) in the drying step, drying mode is selected from and dries, at least a in air-dry, oven dry, freeze-drying and the dewatering agent drying.Said oven dry can be normal pressure or vacuum drying, and said normal pressure bake out temperature can be 50 ℃, time and can be 36 hours, and the vacuum tightness of said vacuum drying can be 0.09Mpa, and temperature can be 40 ℃, and the time can be 1.5h; Various freeze drying process commonly used all are suitable for.In the said dewatering agent drying means, dewatering agent is selected from least a in methyl alcohol, ethanol, glycerine, glucose and the salt, preferred alcohol.In this step, the water-activity of Ou Liren can be 0.40-0.60,0.40-0.53,0.40-0.50,0.50-0.60,0.50-0.53 or 0.53-0.60.
Said step 2) in, the water-activity of said dried Europe Li Ren can be 0.40-0.60,0.40-0.53,0.40-0.50,0.50-0.60,0.50-0.53 or 0.53-0.60.
In the said step 3) extraction step, process for extracting is selected from organic solvent extraction, supercritical CO
2At least a during fluid extraction extracts with squeezing.In the said organic solvent extracting access method, said organic solvent is selected from least a in normal hexane, hexanaphthene and the vegetables oil extraction solvent, the preferred plant oil extraction solvent, and this vegetables oil extraction solvent is to prepare the gained solvent according to standard GB 16629-2008.The Ou Liren after the said pulverizing and the amount ratio of said organic solvent are 1Kg: 1-7L, preferred 1Kg: 4L.Said supercritical CO
2In the fluid extraction, CO
2Pressure be 20-50MPa, preferred 30MPa, temperature is 35-60 ℃, preferred 40 ℃, the time is 20-200min, preferred 110min.In the said squeezing extracting process, pressure is 20-60MPa, preferred 42MPa, and temperature is 20-65 ℃, preferred 62 ℃.In this step, the water-activity of the Ou Liren after the pulverizing can be 0.40-0.60,0.40-0.53,0.40-0.50,0.50-0.60,0.50-0.53 or 0.53-0.60.
In the said step 4), extract temperature and be preferably 40 ℃, the time is 70-110min, specifically can be 70-80min, 70-90min, 80-90min, 90-110min or 80-110min; In this step, the mass percentage concentration of used aqueous ethanolic solution can be 50-80%, 50-70%, 50-65%, 50-60%, 60-80%, 60-70%, 60-65%, 65-80%, 65-70% or 70-80%;
The step of said separation and Extraction is:
A) the said Europe Li Ren dregs of rice are carried out refluxing extraction in mass percentage concentration is the aqueous ethanolic solution of 50%-95%, collect extracting solution;
B) behind the extracting solution concentrating under reduced pressure that said step a) is obtained; In absolute ethyl alcohol, carry out recrystallization; Obtain said amygdaloside and the bullion that has extracted amygdaloside after the drying, obtain said Europe Li Ren albumen after the bullion vacuum-drying with the intact amygdaloside of said extraction again.
In the step b) concentrating under reduced pressure step of this separation and Extraction, pressure is 20-100kPa, and the time is 20-120min, and temperature is 20-80 ℃; In the said drying step, temperature is 80-140 ℃, and the time is 1-4h; In the said vacuum drying step, vacuum tightness is 50-120kPa, preferred 75-80kPa, and the time is 40-180min, preferred 90-120min, temperature 20-80 ℃, preferred 50-60 ℃.
Because amygdaloside is prone to decomposed (as shown in Figure 1) by amygdalase, therefore, the amygdaloside enzymic activity that reduces in Europe japanese plum seed oil, amygdaloside and the Ou Li benevolence albumen sepn leaching process is to realize the key of three's complete utilization.When Ou Liren pulverizing and the extraction of Europe japanese plum seed oil, to reduce the activity of amygdalase, suitable water-activity is 0.10-0.70 through the control water-activity; Then when amygdaloside and the extraction of Ou Li benevolence albumen sepn, reduce the amygdaloside enzymic activity and prevent the excessive sex change of Ou Liren albumen through control alcohol concn and service temperature, alcohol concn is no more than 65 ℃ for suitable with 50%-95%, service temperature.Method provided by the invention has realized amygdaloside, Europe japanese plum seed oil and the proteic complete utilization of Ou Li benevolence, for Ou Liren intensive processing and comprehensive utilization are laid a good foundation.
Description of drawings
Fig. 1 is the hydrolyzation catalysis effect of amygdalase.
Fig. 2 is the HPLC spectrogram of amygdaloside, and wherein, a is the HPLC spectrogram of amygdaloside standard model, and b is the HPLC spectrogram of embodiment 1 preparation gained amygdaloside.
Fig. 3 is a used typical curve when measuring amygdaloside purity with the HPLC method.
Embodiment
Below in conjunction with specific embodiment the present invention is described further, but the present invention is not limited to following examples.Following method is ordinary method if no special instructions.Said measuring method is ordinary method if no special instructions.Among the following embodiment, the Europe japanese plum seed oil all adopts the Suo Shi extraction process to measure, and amygdaloside all adopts high effective liquid chromatography for measuring, and Ou Liren albumen all adopts nitrogen determination to measure.The testing conditions of used performance liquid chromatography is all as follows when wherein, measuring amygdaloside: chromatographic column: SunfireTMC18 (250mm * 4.6mm, 5 μ m); Moving phase: the mixed solution that the first alcohol and water gets with 30: 70 mixings of volume ratio; Flow velocity: 1ml/min; Detect wavelength: 210nm; Column temperature: 30 ℃; Sample size: 10 μ l; Separating size: 1.2nm, used typical curve is as shown in Figure 3, and regression equation is y=8946.4x-30118, and y is a peak area, and x is an amygdaloside concentration, unit is μ g/ml, coefficient R
2=0.9998.
1) Ou Liren 100g is carried out drying with the drying in the sun method, making the water-activity of this Ou Liren is 0.70, obtains dried Europe Li Ren;
According to the Suo Shi extraction process to measuring as the Europe japanese plum seed oil among the Ou Liren of raw material; Adopt high effective liquid chromatography for measuring to measuring as the amygdaloside among the Ou Liren of raw material; According to nitrogen determination to measuring as the albumen among the Ou Liren of raw material; Can know that wherein grease, amygdaloside and proteic quality percentage composition are respectively 39.8%, 3.45% and 28.6%;
2) under the water-activity that keeps the dried Europe Li Ren of step 1) gained is 0.70 condition, should be crushed to 10 orders by dried Europe Li Ren, the Ou Liren 97.1g after obtaining pulverizing;
3) keeping step 2) water-activity of Ou Liren after gained is pulverized is under 0.70 the condition, the Europe japanese plum seed oil among the Ou Liren after under 50 ℃, should pulverizing with organic solvent extraction obtains Europe japanese plum seed oil 38.8g and Ou Li benevolence dregs of rice 57.9g; Used organic solvent is a normal hexane; This step 2) Ou Liren after gained is pulverized and the amount ratio of organic solvent-normal hexane are 1Kg: 4L;
Measure according to insoluble impurities Determination on content and GB/T5538-2005 animal-plant oil peroxide value in transparency, smell, flavour identification method, GB/T 5528-2005 Vegetable oil lipoprotein moisture and volatile matter content determination, GB/T 5530-2005 animal-plant oil acid number and the acid test of GB/T 5525-2008 Vegetable oil lipoprotein, the GB/T 15688-2008 animal-plant oil; Europe japanese plum seed oil to after the refining detects; The gained result is as follows: this Europe japanese plum seed oil clear; The quality percentage composition of moisture and volatile matter content is 0.07%; The quality percentage composition of insoluble impurities is 0.04%; Acid number (KOH) is 0.37mg/g, and peroxide value is 0.31mmol/kg.
4) using mass percentage concentration is that 60% aqueous ethanolic solution carries out separation and Extraction to the step 3) gained Europe Li Ren dregs of rice, obtains amygdaloside 2.80g and Ou Li benevolence albumen (Ou Liren protein concentrate) 43.3g, the extraction of completion Ou Liren;
The concrete steps of this separation and Extraction are:
A) the step 3) gained Europe Li Ren dregs of rice are carried out refluxing extraction in mass percentage concentration is 60% aqueous ethanolic solution, collect extracting solution; In this extraction step, temperature is 40 ℃, and the time is 90min;
B) behind the extracting solution concentrating under reduced pressure that step a) is obtained (pressure is 20kPa, and the time is 120min, and temperature is 20 ℃); Add an amount of absolute ethyl alcohol; After room temperature left standstill crystallization 24h, (amount ratio that room temperature leaves standstill crystallization step gained crystal and absolute ethyl alcohol was 1Kg: 20L), and with behind the absolute ethanol washing to carry out recrystallization at 10 ℃ with absolute ethyl alcohol again; Obtain amygdaloside 2.80g and the bullion that has extracted amygdaloside after 2 hours in 120 ℃ of dryings again; Obtain Ou Liren albumen (Ou Liren protein concentrate) 43.3g after will having extracted the bullion vacuum-drying (vacuum tightness is 80kPa, and be 120min time of drying, and temperature is 60 ℃) of amygdaloside again.
By on can know that this method gained Semen Armeniacae Amarum extract is step 3) gained Europe japanese plum seed oil, step 4) gained amygdaloside and Ou Li benevolence albumen (Ou Liren protein concentrate).
Method according to this embodiment provides is carried out the extraction of Ou Liren, and the extraction yield of Europe japanese plum seed oil and amygdaloside is respectively 97.49% and 81.16%.
Step 4) gained amygdaloside is detected with performance liquid chromatography, and the gained result is as shown in Figure 2, and the purity of this amygdaloside is 96.1%.
Measuring method according to moisture in nitrogen determination, soxhlet extraction and the GB/T 5009.3-2010 food; Respectively step 4) gained Europe Li Ren albumen (Ou Liren protein concentrate) is detected; The gained result is as follows: proteic quality percentage composition is 66.1% in this Ou Liren albumen (Ou Liren protein concentrate); The quality percentage composition of fat is 0.6%, and the quality percentage composition of moisture is 7.2%.
1) with Ou Liren 100g with 20mL dewatering agent dewatering of ethanol, making the water-activity of Ou Liren is 0.53, obtains dried Europe Li Ren;
According to the Suo Shi extraction process to measuring as the Europe japanese plum seed oil among the Ou Liren of raw material; Adopt high effective liquid chromatography for measuring to measuring as the amygdaloside among the Ou Liren of raw material; According to nitrogen determination to measuring as the albumen among the Ou Liren of raw material; Can know that wherein grease, amygdaloside and proteic quality percentage composition are respectively 39.8%, 3.45% and 28.6%;
2) under the water-activity that keeps the dried Europe Li Ren of step 1) gained is 0.53 condition, should be crushed to 120 orders by dried Europe Li Ren, the Ou Liren 95.26g after obtaining pulverizing;
3) keeping step 2) water-activity of Ou Liren after gained is pulverized is under 0.53 the condition, under 42 ℃, to use supercritical CO
2The method of fluid extraction is extracted the Europe japanese plum seed oil among the Ou Liren after this pulverizing, obtains Europe japanese plum seed oil 38.6g and Ou Li benevolence dregs of rice 56.56g; This supercritical CO
2In the fluid extraction step, CO
2Pressure be 30MPa, temperature is 40 ℃, the time is 110min.
Measure according to insoluble impurities Determination on content and GB/T5538-2005 animal-plant oil peroxide value in transparency, smell, flavour identification method, GB/T 5528-2005 Vegetable oil lipoprotein moisture and volatile matter content determination, GB/T 5530-2005 animal-plant oil acid number and the acid test of GB/T 5525-2008 Vegetable oil lipoprotein, the GB/T 15688-2008 animal-plant oil; Europe japanese plum seed oil to after the refining detects; The gained result is as follows: this Europe japanese plum seed oil clear; The quality percentage composition of moisture and volatile matter content is 0.07%; The quality percentage composition of insoluble impurities is 0.03%; Acid number (KOH) is 0.86mg/g, and peroxide value is 0.33mmol/kg.
4) using mass percentage concentration is that 80% aqueous ethanolic solution carries out separation and Extraction to the step 3) gained Europe Li Ren dregs of rice, obtains amygdaloside 2.52g and Ou Li benevolence albumen (Ou Liren protein concentrate) 42.56g, the extraction of completion Ou Liren;
The concrete steps of this separation and Extraction are:
A) the step 3) gained Europe Li Ren dregs of rice are carried out refluxing extraction in mass percentage concentration is 80% aqueous ethanolic solution, collect extracting solution; In this extraction step, temperature is 40 ℃, and the time is 110min.
B) behind the extracting solution concentrating under reduced pressure that step a) is obtained (pressure is 100kPa, and the time is 20min, and temperature is 50 ℃); Add an amount of absolute ethyl alcohol, after room temperature left standstill crystallization 24h, (amount ratio that room temperature leaves standstill crystallization step gained crystal and absolute ethyl alcohol was 1Kg: 20L) to carry out recrystallization at 10 ℃ with absolute ethyl alcohol again; And with behind the absolute ethanol washing; Obtain amygdaloside 2.45g after 2 hours and extracted the bullion of amygdaloside in 120 ℃ of dryings again, (vacuum tightness is 50kPa will to have extracted the bullion vacuum-drying of amygdaloside again; Be 180min time of drying, and temperature is 80 ℃) after obtain Ou Liren albumen (Ou Liren protein concentrate) 42.56g.
By on can know that this method gained Semen Armeniacae Amarum extract is step 3) gained Europe japanese plum seed oil, step 4) gained amygdaloside and Ou Li benevolence albumen (Ou Liren protein concentrate).
Method according to this embodiment provides is carried out the extraction of Ou Liren, and the extraction yield of its Central European japanese plum seed oil and amygdaloside is respectively 96.98% and 73.04%.
Step 4) gained amygdaloside is detected with performance liquid chromatography, and gained spectrogram and Fig. 2 do not have substantive difference, and the purity of this amygdaloside is 95.8%.
Measuring method according to moisture in nitrogen determination, soxhlet extraction and the GB/T 5009.3-2010 food; Respectively step 4) gained Europe Li Ren albumen (Ou Liren protein concentrate) is detected; The gained result is as follows: proteic quality percentage composition is 67.2% in this Ou Liren albumen (Ou Liren protein concentrate); The quality percentage composition of fat is 0.91%, and the quality percentage composition of moisture is 9.1%.
Embodiment 3,
1) Ou Liren 100g is carried out drying with freeze dried method, making the water-activity of Ou Liren is 0.40, obtains dried Europe Li Ren; In this step of freeze drying, make material pre-freeze to-40 ℃ earlier, the open vacuum pump makes vacuum tightness carry out the vacuum-freeze-dry operation at 20-40Pa then, when temperature of charge during near room temperature freeze-drying accomplish.
According to the Suo Shi extraction process to measuring as the Europe japanese plum seed oil among the Ou Liren of raw material; Adopt high effective liquid chromatography for measuring to measuring as the amygdaloside among the Ou Liren of raw material; According to nitrogen determination to measuring as the albumen among the Ou Liren of raw material; Can know that wherein grease, amygdaloside and proteic quality percentage composition are respectively 39.8%, 3.45% and 28.6%;
2) under the water-activity that keeps the dried Europe Li Ren of step 1) gained is 0.40 condition, dried Europe Li Ren is crushed to 60 orders, the Ou Liren 94.68g after obtaining pulverizing;
3) keeping step 2) water-activity of Ou Liren after gained is pulverized is under 0.40 the condition, the Europe japanese plum seed oil among the Ou Liren after 55 ℃ are extracted this with the method for squeezing down and pulverize obtains Europe japanese plum seed oil 35.0g and Ou Li benevolence dregs of rice 59.46g; In this squeezing extraction step, pressure is 42Mpa, and the time is 60min.
Measure according to insoluble impurities Determination on content and GB/T5538-2005 animal-plant oil peroxide value in transparency, smell, flavour identification method, GB/T 5528-2005 Vegetable oil lipoprotein moisture and volatile matter content determination, GB/T 5530-2005 animal-plant oil acid number and the acid test of GB/T 5525-2008 Vegetable oil lipoprotein, the GB/T 15688-2008 animal-plant oil; Europe japanese plum seed oil to after the refining detects; The gained result is as follows: this Europe japanese plum seed oil clear; The quality percentage composition of moisture and volatile matter content is 0.06%; The quality percentage composition of insoluble impurities is 0.07%; Acid number (KOH) is 0.62mg/g, and peroxide value is 0.36mmol/kg.
4) using mass percentage concentration is that 70% aqueous ethanolic solution carries out separation and Extraction to the step 3) gained Europe Li Ren dregs of rice, obtains amygdaloside 2.24g and Ou Li benevolence albumen (Ou Liren protein concentrate) 43.42g, the extraction of completion Ou Liren;
The concrete steps of this separation and Extraction are:
A) the step 3) gained Europe Li Ren dregs of rice are carried out refluxing extraction in mass percentage concentration is 70% aqueous ethanolic solution, collect extracting solution; In this extraction step, temperature is 40 ℃, and the time is 80min.
B) behind the extracting solution concentrating under reduced pressure that step a) is obtained (pressure is 60kPa, and the time is 70min, and temperature is 70 ℃); Add an amount of absolute ethyl alcohol; After room temperature left standstill crystallization 24h, (amount ratio that room temperature leaves standstill crystallization step gained crystal and absolute ethyl alcohol was 1Kg: 20L), and with behind the absolute ethanol washing to carry out recrystallization at 10 ℃ with absolute ethyl alcohol again; Behind 120 ℃ of dry 2h, obtain amygdaloside 2.06g and the bullion that has extracted amygdaloside again; Obtain Ou Liren albumen (Ou Liren protein concentrate) 43.42g after will having extracted the bullion vacuum-drying (vacuum tightness is 120kPa, and be 40min time of drying, and temperature is 20 ℃) of amygdaloside again.
By on can know that this method gained Semen Armeniacae Amarum extract is step 3) gained Europe japanese plum seed oil, step 4) gained amygdaloside and Ou Li benevolence albumen (Ou Liren protein concentrate).
Method according to this embodiment provides is carried out the extraction of Ou Liren, and its Central European japanese plum seed oil and amygdaloside extraction yield are respectively 87.9% and 64.9%.
Step 4) gained amygdaloside is detected with performance liquid chromatography, and gained spectrogram and Fig. 2 do not have substantive difference, and the purity that can know this amygdaloside is 95.7%.
Measuring method according to moisture in nitrogen determination, soxhlet extraction and the GB/T 5009.3-2010 food; Respectively step 4) gained Europe Li Ren albumen (Ou Liren protein concentrate) is detected; The gained result is as follows: proteic quality percentage composition is 65.8% in this Ou Liren albumen (Ou Liren protein concentrate); The quality percentage composition of fat is 0.79%, and the quality percentage composition of moisture is 8.6%.
Embodiment 4,
1) Ou Liren 100g is carried out drying with the method for oven dry, making the water-activity of this Ou Liren is 0.60, obtains dried Europe Li Ren; In this baking step, temperature is 50 ℃, and the time is 36h;
According to the Suo Shi extraction process to measuring as the Europe japanese plum seed oil among the Ou Liren of raw material; Adopt high effective liquid chromatography for measuring to measuring as the amygdaloside among the Ou Liren of raw material; According to nitrogen determination to measuring as the albumen among the Ou Liren of raw material; Can know that wherein grease, amygdaloside and proteic quality percentage composition are respectively 39.8%, 3.45% and 28.6%;
2) under the water-activity that keeps the dried Europe Li Ren of step 1) gained is 0.60 condition, should be crushed to 80 orders by dried Europe Li Ren, the Ou Liren 96.12g after obtaining pulverizing;
3) keeping step 2) water-activity of Ou Liren after gained is pulverized is under 0.60 the condition, under 40 ℃, to use supercritical CO
2The method of fluid extraction is extracted the Europe japanese plum seed oil among the Ou Liren after this pulverizing, obtains Europe japanese plum seed oil 38.9g and Ou Li benevolence dregs of rice 57.02g; This supercritical CO
2In the fluid extraction step, CO
2Pressure be 30MPa, temperature is 40 ℃, the time is 110min.
Measure according to insoluble impurities Determination on content and GB/T5538-2005 animal-plant oil peroxide value in transparency, smell, flavour identification method, GB/T 5528-2005 Vegetable oil lipoprotein moisture and volatile matter content determination, GB/T 5530-2005 animal-plant oil acid number and the acid test of GB/T 5525-2008 Vegetable oil lipoprotein, the GB/T 15688-2008 animal-plant oil; Europe japanese plum seed oil to after the refining detects; The gained result is as follows: this Europe japanese plum seed oil clear; The quality percentage composition of moisture and volatile matter content is 0.05%; The quality percentage composition of insoluble impurities is 0.04%; Acid number (KOH) is 0.71mg/g, and peroxide value is 0.33mmol/kg.
4) using mass percentage concentration is that 50% aqueous ethanolic solution carries out separation and Extraction to the step 3) gained Europe Li Ren dregs of rice, obtains amygdaloside 2.39g and Ou Li benevolence albumen (Ou Liren protein concentrate) 43.73g, the extraction of completion Ou Liren;
The concrete steps of this separation and Extraction are:
A) the step 3) gained Europe Li Ren dregs of rice are carried out refluxing extraction in mass percentage concentration is 50% aqueous ethanolic solution, collect extracting solution; In this extraction step, temperature is 40 ℃, and the time is 70min.
B) (pressure is 100kPa to the extracting solution concentrating under reduced pressure that step a) is obtained; Time is 20min; Temperature is 20 ℃) after, an amount of absolute ethyl alcohol added, after room temperature leaves standstill crystallization 24h; (amount ratio that room temperature leaves standstill crystallization step gained crystal and absolute ethyl alcohol is 1Kg: 20L) to carry out recrystallization at 10 ℃ with absolute ethyl alcohol again; And with behind the absolute ethanol washing, obtain amygdaloside 2.39g after 2 hours and extracted the bullion of amygdaloside in 120 ℃ of dryings again, (vacuum tightness is 80kPa will to have extracted the bullion vacuum-drying of amygdaloside again; Be 120min time of drying, and temperature is 60 ℃) after obtain Ou Liren albumen (Ou Liren protein concentrate) 43.73g.
By on can know that this method gained Semen Armeniacae Amarum extract is step 3) gained Europe japanese plum seed oil, step 4) gained amygdaloside and Ou Li benevolence albumen (Ou Liren protein concentrate).
Method according to this embodiment provides is carried out the extraction of Ou Liren, and the extraction yield of its Central European japanese plum seed oil and amygdaloside is respectively: 97.7% and 69.3%.
Step 4) gained amygdaloside is detected with performance liquid chromatography, and gained spectrogram and Fig. 2 do not have substantive difference, and the purity that can know this amygdaloside is 95.3%.
Measuring method according to moisture in nitrogen determination, soxhlet extraction and the GB/T 5009.3-2010 food; Respectively step 4) gained Europe Li Ren albumen (Ou Liren protein concentrate) is detected; The gained result is as follows: proteic quality percentage composition is 65.4% in this Ou Liren albumen (Ou Liren protein concentrate); The quality percentage composition of fat is 0.81%, and the quality percentage composition of moisture is 9.1%.
Embodiment 5,
1) Ou Liren 100g is carried out drying with the method for vacuum drying, making the water-activity of this Ou Liren is 0.50, obtains dried Europe Li Ren; In this vacuum drying step, vacuum tightness is 0.09Mpa, and temperature is 40 ℃, and the time is 1.5h;
According to the Suo Shi extraction process to measuring as the Europe japanese plum seed oil among the Ou Liren of raw material; Adopt high effective liquid chromatography for measuring to measuring as the amygdaloside among the Ou Liren of raw material; According to nitrogen determination to measuring as the albumen among the Ou Liren of raw material; Can know that wherein grease, amygdaloside and proteic quality percentage composition are respectively 39.8%, 3.45% and 28.6%;
2) under the water-activity that keeps the dried Europe Li Ren of step 1) gained is 0.50 condition, should be crushed to 50 orders by dried Europe Li Ren, the Ou Liren 95.18g after obtaining pulverizing;
3) keeping step 2) water-activity of Ou Liren after gained is pulverized is under 0.50 the condition, the Europe japanese plum seed oil among the Ou Liren after under 50 ℃, should pulverizing with organic solvent extraction obtains Europe japanese plum seed oil 38.5g and Ou Li benevolence dregs of rice 56.57g; Used organic solvent is the vegetables oil extraction solvent; This step 2) Ou Liren after gained is pulverized and the amount ratio of organic solvent vegetables oil extraction solvent are 1Kg: 4L;
Measure according to insoluble impurities Determination on content and GB/T5538-2005 animal-plant oil peroxide value in transparency, smell, flavour identification method, GB/T 5528-2005 Vegetable oil lipoprotein moisture and volatile matter content determination, GB/T 5530-2005 animal-plant oil acid number and the acid test of GB/T 5525-2008 Vegetable oil lipoprotein, the GB/T 15688-2008 animal-plant oil; Europe japanese plum seed oil to after the refining detects; The gained result is as follows: this Europe japanese plum seed oil clear; The quality percentage composition of moisture and volatile matter content is 0.08%; The quality percentage composition of insoluble impurities is 0.07%; Acid number (KOH) is 0.72mg/g, and peroxide value is 0.37mmol/kg.
4) using mass percentage concentration is that 65% aqueous ethanolic solution carries out separation and Extraction to the step 3) gained Europe Li Ren dregs of rice, obtains amygdaloside 2.55g and Ou Li benevolence albumen (Ou Liren protein concentrate) 42.88g, the extraction of completion Ou Liren;
The concrete steps of this separation and Extraction are:
A) the step 3) gained Europe Li Ren dregs of rice are carried out refluxing extraction in mass percentage concentration is 65% aqueous ethanolic solution, collect extracting solution; In this extraction step, temperature is 40 ℃, and the time is 80min.
B) behind the extracting solution concentrating under reduced pressure that step a) is obtained (pressure is 60kPa, and the time is 70min, and temperature is 50 ℃); Add an amount of absolute ethyl alcohol; After room temperature left standstill crystallization 24h, (amount ratio that room temperature leaves standstill crystallization step gained crystal and absolute ethyl alcohol was 1Kg: 20L), and with behind the absolute ethanol washing to carry out recrystallization at 10 ℃ with absolute ethyl alcohol again; Obtain amygdaloside 2.55g and the bullion that has extracted amygdaloside after 2 hours in 120 ℃ of dryings again; Obtain Ou Liren albumen (Ou Liren protein concentrate) 42.88g after will having extracted the bullion vacuum-drying (vacuum tightness is 80kPa, and be 120min time of drying, and temperature is 60 ℃) of amygdaloside again.
By on can know that this method gained Semen Armeniacae Amarum extract is step 3) gained Europe japanese plum seed oil, step 4) gained amygdaloside and Ou Li benevolence albumen (Ou Liren protein concentrate).
Method according to this embodiment provides is carried out the extraction of Ou Liren, and the extraction yield of its Central European japanese plum seed oil and amygdaloside is respectively: 96.7% and 73.9%.
Step 4) gained amygdaloside is detected with performance liquid chromatography, and gained spectrogram and Fig. 2 do not have substantive difference, and the purity that can know this amygdaloside is 96.1%.
Measuring method according to moisture in nitrogen determination, soxhlet extraction and the GB/T 5009.3-2010 food; Respectively step 4) gained Europe Li Ren albumen (Ou Liren protein concentrate) is detected; The gained result is as follows: proteic quality percentage composition is 66.7% in this Ou Liren albumen (Ou Liren protein concentrate); The quality percentage composition of fat is 0.73%, and the quality percentage composition of moisture is 8.2%.
Claims (10)
1. a method for preparing the Ou Liren extract comprises the steps:
1) Ou Liren is carried out drying, making the water-activity of said Europe Li Ren is 0.10-0.70, obtains dried Europe Li Ren;
2) water-activity of the Ou Liren after keeping said drying and dehydrating is under the condition of 0.10-0.70, said dried Europe Li Ren is crushed to the 10-120 order, the Ou Liren after obtaining pulverizing;
3) water-activity of the Ou Liren after keeping said pulverizing is under the condition of 0.10-0.70, extracts the Europe japanese plum seed oil among the Ou Liren after the said pulverizing, obtains the said Europe japanese plum seed oil and the Ou Li benevolence dregs of rice;
4) use mass percentage concentration the said Europe Li Ren dregs of rice to be carried out separation and Extraction, obtain amygdaloside and Ou Li benevolence albumen as the aqueous ethanolic solution of 50%-95%; In the said extraction step, temperature is 5-65 ℃;
Said Europe Li Ren extract is selected among a, b and the c three kinds, any two kinds or any one, and wherein, said a is a said step 3) gained Europe japanese plum seed oil, and said b is said step 4) gained amygdaloside, and said c is a said step 4) gained Europe Li Ren albumen.
2. method according to claim 1 is characterized in that: in the said step 1) drying step, drying mode is selected from and dries, at least a in air-dry, oven dry, freeze-drying and the dewatering agent drying.
3. method according to claim 2 is characterized in that: in the said dewatering agent drying means, dewatering agent is selected from least a in methyl alcohol, ethanol, glycerine, glucose and the salt; The amount ratio of said dewatering agent and said Europe Li Ren is 0.04-0.5L: 1Kg.
4. method according to claim 3 is characterized in that: said dewatering agent is an ethanol; The amount ratio of said dewatering agent and said Europe Li Ren is 0.16L: 1Kg.
5. according to the arbitrary described method of claim 1-4, it is characterized in that: in the said step 3), extract and be selected from organic solvent extraction, supercritical CO
2At least a in fluid extraction and the squeezing extraction.
6. method according to claim 5; It is characterized in that: in the said step 3) organic solvent extraction; Said organic solvent is selected from least a in normal hexane, hexanaphthene and the vegetables oil extraction solvent, and the Ou Liren after the said pulverizing and the amount ratio of said organic solvent are 1Kg: 1-7L;
Said step 3) supercritical CO
2In the fluid extraction, CO
2Pressure be 20-50MPa, temperature is 35-60 ℃, the time is 20-200min;
In the said step 3) squeezing extraction, pressure is 20-60MPa, and temperature is 20-65 ℃;
In the said step 4), the mass percentage concentration of said aqueous ethanolic solution is 60%, and in the said refluxing extraction step, temperature is 40 ℃, and the time is 70-110min.
7. method according to claim 6 is characterized in that: in the said step 3) organic solvent extraction, said organic solvent is the vegetables oil extraction solvent, and the Ou Liren after the said pulverizing and the amount ratio of said organic solvent are 1Kg: 4L;
Said step 3) supercritical CO
2In the fluid extraction, CO
2Pressure be 30MPa, temperature is 40 ℃, the time is 110min;
In the said step 3) squeezing extraction, pressure is 42MPa, and temperature is 55 ℃.
8. according to the arbitrary described method of claim 1-7, it is characterized in that: in the said step 4), the step of said separation and Extraction is:
A) the said Europe Li Ren dregs of rice are carried out refluxing extraction in mass percentage concentration is the aqueous ethanolic solution of 50%-95%, collect extracting solution;
B) behind the extracting solution concentrating under reduced pressure that said step a) is obtained; In absolute ethyl alcohol, carry out recrystallization; Obtain said amygdaloside and the bullion that has extracted amygdaloside after the drying, obtain said Europe Li Ren albumen after the bullion vacuum-drying with the intact amygdaloside of said extraction again.
9. method according to claim 8 is characterized in that: in the said step b) concentrating under reduced pressure step, pressure is 20-100kPa, and the time is 20-120min, and temperature is 20-80 ℃; In the said drying step, temperature is 80-140 ℃, and the time is 1-4 hour; In the said vacuum drying step, vacuum tightness is 50-120kPa, preferred 75-80kPa, and the time is 40-180min, preferred 90-120min, temperature 20-80 ℃, preferred 50-60 ℃.
10. method according to claim 9 is characterized in that: in the said step b) vacuum drying step, vacuum tightness is 75-80kPa, and the time is 90-120min, and temperature is 50-60 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1594340A (en) * | 2004-07-02 | 2005-03-16 | 中国科学院山西煤炭化学研究所 | Process for extraction refining amygdalin |
| CN101362782A (en) * | 2008-08-26 | 2009-02-11 | 山西百利士生物科技有限公司 | Extraction method of amygdalin |
| CN101704853A (en) * | 2009-11-13 | 2010-05-12 | 段洪东 | Extraction and purification method of amygdalin in Cerasus humilis kernel |
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| CN1594340A (en) * | 2004-07-02 | 2005-03-16 | 中国科学院山西煤炭化学研究所 | Process for extraction refining amygdalin |
| CN101362782A (en) * | 2008-08-26 | 2009-02-11 | 山西百利士生物科技有限公司 | Extraction method of amygdalin |
| CN101704853A (en) * | 2009-11-13 | 2010-05-12 | 段洪东 | Extraction and purification method of amygdalin in Cerasus humilis kernel |
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