CN113855657B - Lycium ruthenicum anthocyanin extract and preparation method of freeze-dried powder - Google Patents
Lycium ruthenicum anthocyanin extract and preparation method of freeze-dried powder Download PDFInfo
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- CN113855657B CN113855657B CN202111272262.XA CN202111272262A CN113855657B CN 113855657 B CN113855657 B CN 113855657B CN 202111272262 A CN202111272262 A CN 202111272262A CN 113855657 B CN113855657 B CN 113855657B
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- lycium ruthenicum
- anthocyanin
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- dried powder
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Abstract
The invention relates to the technical field of lycium ruthenicum anthocyanin extract, products and application thereof, in particular to a preparation method of lycium ruthenicum anthocyanin extract and freeze-dried powder and application thereof in sleep improvement products, which are prepared through the steps of extraction, high-speed centrifugation and ceramic membrane filtration, organic membrane degumming and concentration, simulated moving bed chromatographic separation, low-temperature concentration, freeze-drying and freeze-dried powder preparation. The preparation method of the lycium ruthenicum anthocyanin extract and the freeze-dried powder is suitable for industrial production, and has the advantages of high anthocyanin content, high recovery rate, good product color and no exogenous acidic substance residue. The lycium ruthenicum extract and the freeze-dried powder provided by the invention can obviously prolong the sleep time of mice, improve the sleep incidence rate, shorten the sleep latency and have obvious sleep improving effect. The lycium ruthenicum anthocyanin extract and the freeze-dried powder can be used for functional foods, health-care foods and medicines for improving sleep.
Description
Technical Field
The invention relates to the technical field of lycium ruthenicum anthocyanin extract, products and applications thereof, in particular to a preparation method of lycium ruthenicum anthocyanin extract and freeze-dried powder and application of lycium ruthenicum anthocyanin extract and freeze-dried powder in sleep improvement products.
Background
Lack of exercise, environmental pollution, and exacerbation of social competition have led to an increasing incidence of sleep disorders and related epidemic diseases of low immunity. According to the survey of world health organization, about 27% of people worldwide have sleep disorders, the incidence rate of insomnia of adults in China is as high as 38.2%, and more than 3 hundred million Chinese people have sleep disorders, which have become important health problems of global concern. Research shows that sleep is helpful for enhancing the capability of human leucocytes to resist infection, thereby improving immunity. Chronic sleep disorders often lead to "sub-health states" such as chronic fatigue, anxiety, obesity, hypomnesis, hypoimmunity, etc., which can induce various diseases such as hypertension, diabetes, depression, and tumors. Therefore, improving sleep and immunity plays a key role in conditioning sub-health of human bodies. It is reported that the sub-health population in China exceeds 7 hundred million, and the natural health food/medicine with the effects of improving sleep and enhancing immunity has a rapid rising trend, and has a wide consumption population. At present, the chemical medicament for clinically treating sleep disorder is easy to produce side effects of low safety, residue, dependence and the like after long-term administration. Compared with the traditional Chinese medicine, the natural food and medicine resources are high in safety in improving sleep disorder, drug resistance and dependence are not easy to occur, and besides treatment, the traditional Chinese medicine has conditioning effects, so that the traditional Chinese medicine is more and more favored by patients. In conclusion, research and development of a natural medicine product which is efficient and safe and can improve immunity and sleep has important social value.
Lycium ruthenicum (Lycium ruthenicum Murr.), also called "side Ma" in Tibetan medicine, is perennial shrub of Lycium genus of Solanaceae family, has strong vitality, and can resist salt, cold and drought, and is mainly distributed in Qinghai, xinjiang, ningxia, tibet, northern Shaanxi, gansu and other places in China. The lycium ruthenicum is received in the classical works of Tibetan medicines such as "Jingzhu Ben Cao" and "four-part medical dictionary", and the like, has sweet taste, flat nature and heat clearing and heart fire clearing, and is a plant for both medicine and food. The lycium ruthenicum murr is rich in anthocyanin and alkaloid components, and the anthocyanin components have various physiological functions of resisting inflammation, oxidation, aging, tumors, eyesight and the like, are natural antioxidants and free radical scavengers, and have wide development and application prospects in the industries of medicines, foods, health-care products and cosmetics. The study on the alkaloid components is very few, and the study on the aspects of chemical components, biological activity and the like is basically blank except a few analytical measurement studies.
ZL201010542518.X "preparation method of antioxidant Lycium ruthenicum Murr extract", disclose a method for extracting fresh Lycium ruthenicum Murr fruit with water, grinding with colloid mill, high pressure homogenizing technology, microfiltration ceramic membrane impurity removal, macroporous resin separation, spray drying or freeze drying to prepare Lycium ruthenicum Murr extract; ZL201610548250.8, a method for extracting lycium ruthenicum anthocyanin, discloses a preparation method for extracting lycium ruthenicum anthocyanin by mixing lycium ruthenicum powder with ethanol solution, performing membrane treatment, purifying by macroporous resin, concentrating under reduced pressure and drying.
The existing scheme mainly adopts water or ethanol extraction and macroporous resin adsorption purification for extraction and purification of lycium ruthenicum anthocyanin, and acidic ethanol solution is mainly adopted for extraction and elution in the processing process, so that exogenous acidic substances which are added in the whole extraction, separation and purification, concentration and drying processes cannot be removed, the obtained product contains a large amount of acid, the anthocyanin is dark red (the anthocyanin is blue-purple in a neutral state), the anthocyanin activity is reduced, and meanwhile, the risk of heavy metal chromium pollution is increased in the product due to acidic corrosion in the production process. Colloid mill grinding, high-pressure homogenization, superfine grinding, ultrasonic-microwave reaction extraction, bionic extraction, ultrasonic auxiliary extraction and other pretreatment and extraction equipment are expensive, and industrialization is difficult to implement. In addition, the high temperature of the spray drying process causes degradation or inactivation of the anthocyanin, which is not suitable for the production of lycium ruthenicum anthocyanin. And reports on the study of the anthocyanin activity of lycium ruthenicum are concentrated on the aspects of antioxidation and aging resistance, and reports on the aspect of improving sleep are not yet seen.
Disclosure of Invention
Based on the technical problems, the invention aims to provide a preparation method of lycium ruthenicum anthocyanin extract and freeze-dried powder and application of the lycium ruthenicum anthocyanin extract and freeze-dried powder in sleep improvement products.
The invention discloses a preparation method of lycium ruthenicum anthocyanin extract and freeze-dried powder, which specifically comprises the following steps:
step 1, an extraction process: crushing the dried lycium ruthenicum, adding deionized water with the volume of 5-10 times, soaking, stirring and extracting for 3-5 times to obtain crude lycium ruthenicum juice; or crushing fresh Lycium ruthenicum Murr, squeezing, extracting residues with water, repeating for 3 times, and mixing filtrates to obtain coarse Lycium ruthenicum Murr juice;
step 2, high-speed centrifugation and ceramic membrane filtration: centrifuging the crude lycium ruthenicum juice obtained in the step 1 by using a centrifugal machine with the rotating speed of 15000-20000 r/min to remove impurities, and clarifying by using a ceramic membrane with the diameter of 50-200 nm to obtain clarified lycium ruthenicum juice;
step 3, degumming and concentrating an organic film: removing pectin, protein and polysaccharide macromolecular substances from the clarified lycium ruthenicum juice obtained in the step 2 through an ultrafiltration organic membrane with the molecular weight cutoff of 50000-100000, adding pure water for cleaning, collecting effluent liquid, and dehydrating and concentrating through the ultrafiltration organic membrane with the molecular weight cutoff of 300-5000 to obtain membrane concentrate;
step 4, simulated moving bed chromatographic separation: adding the membrane concentrate obtained in the step 3 into a simulated moving bed chromatography for separation to obtain a lycium ruthenicum fine anthocyanin separating liquid;
step 5, low-temperature concentration: recovering ethanol from the lycium ruthenicum fine anthocyanin separating liquid obtained in the step 4, and carrying out vacuum low-temperature concentration under the conditions of 10-50 ℃ and vacuum degree of-0.06 MPa to obtain lycium ruthenicum anthocyanin concentrated liquid;
step 6, freeze drying: directly freeze-drying the lycium ruthenicum anthocyanin concentrated solution obtained in the step 5 to obtain a lycium ruthenicum anthocyanin extract;
step 7, preparing freeze-dried powder: and (5) adding auxiliary materials into the lycium ruthenicum anthocyanin concentrated solution obtained in the step (5), stirring and mixing uniformly, and freeze-drying to obtain the lycium ruthenicum anthocyanin freeze-dried powder.
Further, the simulated moving bed separation method in the step 4 is as follows: the simulated moving bed chromatography packed adsorbent is: nonpolar macroporous adsorption resin: d101, D101b, DA-201, DM-301, DM-11, HPD-100, HPD-450, HPD-750, D1400, D1300, D3520, D4006, D4020, HP-20, H-103, H107, X-5, ADS-8, BS-55, BS-65, BS-80, NKA-2, and NKA-9; weak polar macroporous resin: AB-8, DM130, D860021, DS-401, BS-30, CAD-40, and CAD-45; polar macroporous resin: any one or more of ADS-F8, ADS-21, ADS-7, ADS-17, BS-75, BS-45, S-8, NKA-2 and NKA-9, and the flow rate of the adsorption area is 1-2 BV/h; the water washing area is purified water, the dosage of the purified water is 1 to 2 times of the volume of the resin, and the flow rate is 1 to 3BV/h; the desorbent is ethanol solution with the concentration of 5-90 percent, the dosage of the desorbent is 2-4 times of the volume of the resin, and the flow rate is 1-3 BV/h; the resin regeneration solvent is 95% ethanol solution, and the dosage is 1 time of that of the resin; the flow rate is 2-3 BV/h.
Further, in the step 6, freeze drying is carried out by adopting a freeze dryer at the temperature of-50 ℃ to-70 ℃ to obtain the lycium ruthenicum anthocyanin extract.
Further, the auxiliary materials added in the step 7 are one of starch, maltodextrin, fructo-oligosaccharide, galacto-oligosaccharide, lactose, inulin, beta-cyclodextrin, anhydrous glucose, polydextrose, milk powder, calcium citrate, xylitol, sorbitol and D-mannitol, and a freeze dryer is adopted to obtain the freeze-dried powder of lycium ruthenicum anthocyanin under the condition of-50 to-70 ℃.
The invention also protects the lycium ruthenicum anthocyanin extract and the freeze-dried powder prepared by the method, wherein the lycium ruthenicum anthocyanin extract and the freeze-dried powder contain one or more or all of the following chemical components: n-trans-single-foot-amine, (E) -N- (4-Acetamidobutyl) -2- [4, 5-dihydro-2- [3- [2- (4-hydroxy-phenyl) ethyl ] -3-oxo-phenyl ] -3- (4-hydroxy-3-methoxyphenyl) prop-2-enamide, (1S, 2R) -N3- (4-Acetamidobutyl) -1- (3, 4-dihydro-phenyl) -7-hydroxy-N2- (4-hydroxy-phenyl) -6, 8-dimethyl-1, 2-dihydroxy-nano-phenyl-2, 3-dicarboxamide, petunidin3-O- [6-O- (4-O- (4-O-trans- (. Beta. -D-glucopyranoside) -co-L-alpha. -D-glucopyranoside) -alpha. -N-2- (3, 4-hydroxy-phenyl) -7-hydroxy-N2- (4-hydroxy-phenyl) -6, 8-dimethyl-1, 2-hydroxy-phenyl-O-2, 3-O- [6-O- (4-O-trans- (. Beta. -D-glucopyranoside) -alpha. -D-glucopyranoside ] - [ beta ] -N-hydroxy-2- (4-hydroxy-phenyl) -2-hydroxy-methyl ] -phenyl ], N-dihydrocaffeoylspermidine, N-caffeoyl-N-hydrocaffeoylspermidine, N-hydrofaffeoyl-N-caffeoylspermidine, petunidin-3-O- (6-O-p-coumaryl) -rutinoside-5-O-glucoside, malvidin-3-O-rutinoside (cis-p-coumaroyl) -5-O-gIacoside, petuniin-3-O-rutinoside (caffeoyl) -5-O-glucoside and malvidin-3-O-rutinoside (cis-p-coumaroyl) -5-O-gIucoside;
the chemical components are as follows:
further, the anthocyanin extract of lycium ruthenicum and the freeze-dried powder have the anthocyanin content of 0.1-90% and the total alkaloid content of 0.1-90%.
The invention also protects the application of the lycium ruthenicum anthocyanin extract and the freeze-dried powder prepared by the preparation method in improving sleep products; the sleep improving product is food, health food or medicine, specifically, the lycium ruthenicum anthocyanin extract and/or freeze-dried powder are taken as active ingredients, and various dosage forms of medicine are prepared according to any pharmaceutically acceptable carrier, or various foods or health foods are prepared according to any carrier acceptable in food science.
Further, the formulation of the food, the health food or the medicine is powder, tablet or capsule.
Further, the food is a lycium ruthenicum anthocyanin solid beverage, and the health-care food is a lycium ruthenicum anthocyanin tablet candy; the medicine is lycium ruthenicum anthocyanin capsule medicine.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the lycium ruthenicum anthocyanin extract and the freeze-dried powder is suitable for industrial production, the preparation process is green and pollution-free, the anthocyanin content in the prepared extract and freeze-dried powder is high, no exogenous acid is required to be added, the natural properties of the lycium ruthenicum anthocyanin are completely maintained, and harmful substances such as heavy metal and pesticide residues in the raw materials are removed. The prepared lycium ruthenicum anthocyanin extract is subjected to a direct sleep experiment, a barbital sodium subthreshold dose hypnotic experiment, a pentobarbital sodium sleep time prolonging experiment and a barbital sodium sleep latency experiment respectively. Experimental results show that the lycium ruthenicum anthocyanin extract and the freeze-dried powder can obviously prolong the sleep time of mice, improve the sleep incidence rate, shorten the sleep latency period and have obvious effects on improving sleep.
Drawings
FIG. 1 is a diagram showing the chemical constitution of 11 kinds of anthocyanin extracts from Lycium ruthenicum Murr prepared by the method of the present invention;
FIG. 2 is a HPLC chart of the anthocyanin extract of Lycium ruthenicum Murr obtained in example 1 of the present invention;
FIG. 3 is an ion flow chart of HPLC/MS-MS analysis of the anthocyanin extract of Lycium ruthenicum obtained in example 1 of the present invention;
FIG. 4 is a simulated moving bed separation diagram of anthocyanin extract from Lycium ruthenicum Murr obtained in example 1 of the present invention;
FIG. 5 is a graph showing the effect of different dosages of Lycium ruthenicum anthocyanin extract on sleep time of mice according to the present invention;
FIG. 6 is a graph showing the effect of different dosages of Lycium ruthenicum anthocyanin extract on sleep latency in mice.
In the figure, P is less than 0.05 and P is less than 0.01 of a dosage group of 1g crude drug/kg of lycium ruthenicum anthocyanin, a dosage group of 2.5g crude drug/kg of lycium ruthenicum anthocyanin and a dosage group of 5g crude drug/kg of lycium ruthenicum anthocyanin.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The Lycium ruthenicum raw material used in the embodiment of the invention is provided by Qinghai Jin Maiqi biotechnology limited company and purchased from Qinghai Greek Wood market.
Test equipment: CSJ-20 coarse crusher (Jiangyin square round machine Co., ltd.), ZD-LZ-1.5 juicer (Zhongde food machinery Jingjiang Co., ltd.), extraction equipment (Zhejiang temperature Brown mechanical valve Co., ltd.), GQ105B tube centrifuge (Shanghai Pudong Tian centrifugal machine Co., ltd.), PTSX40 butterfly centrifuge (Yixing city ancient cooking machine Co., ltd.), SMB-H-08-A simulated moving bed (Hanbang technology Co., ltd.), GLZ-1B freeze dryer (Shanghai Pudong freeze drying equipment Co., ltd.), SCIENTZ-10 freeze dryer (Ningbo biological technology Co., ltd.), ZPSX tablet press (Shanghai Xiangshan pharmaceutical machinery Co., ltd.), NJP-300 full-automatic capsule filling machine (Rui An Shitian macro pharmaceutical machinery Co., ltd.).
Experimental instrument: spectra Max190 microplate reader (MD Co., USA); bench top high-speed refrigerated centrifuge (Eppendorf 5424R).
Experimental reagent: lycium ruthenicum anthocyanin extract (available from Qinghai Jin Maiqi Biotechnology Co., ltd., lot 20201001); DPPH (sigma company, usa), ascorbate (VC), phenazine Methosulfate (PMS) were all purchased from aladine; reduced coenzyme I (NADH) and Nitrotetrazolium Blue (NBT) were purchased from Biyun Tian; 30% H 2 O 2 Iron sulfate, salicylic acid were all purchased from Tianjin metallocene reagent company; sodium pentobarbital (China medical group Shanghai chemical reagent Co., lot number 20180825).
Animals: kunming mice, SPF grade, department of medicine of West An traffic university laboratory animal center provided, license number: SCXK (Shaanxi) 2018-0001.
Example 1
The preparation method of the lycium ruthenicum anthocyanin extract specifically comprises the following steps:
step 1, an extraction process: crushing 30Kg of dried lycium ruthenicum, putting the crushed dried lycium ruthenicum into 200L extraction equipment, adding deionized water with the volume of 5-10 times, soaking, stirring and extracting for 3-5 times to obtain crude lycium ruthenicum juice;
step 2, high-speed centrifugation and ceramic membrane filtration: centrifuging the crude lycium ruthenicum juice obtained in the step 1 by using a high-speed centrifuge with the rotating speed of 20000r/min to remove impurities, and clarifying by using a 50nm ceramic membrane to obtain about 800L of clarified lycium ruthenicum juice;
step 3, degumming and concentrating an organic film: removing pectin, protein and polysaccharide macromolecular substances from the clarified lycium ruthenicum juice obtained in the step 2 through an ultrafiltration organic membrane with the molecular weight cutoff of 50000, adding pure water with the volume of 3-5 times for cleaning, collecting effluent liquid, and dehydrating and concentrating through the ultrafiltration organic membrane with the molecular weight cutoff of 300 to obtain about 15L of membrane concentrate;
step 4, simulated moving bed chromatographic separation: adding the membrane concentrate obtained in the step 3 into a simulated moving bed chromatography for separation to obtain 250L lycium ruthenicum fine anthocyanin separating liquid; the simulated moving bed separation method comprises the following steps: the simulated moving bed chromatography packed adsorbent is: the simulated moving bed chromatography packed adsorbent is: HPD-100: DM130: ADS-21=2:2:1 mixed resin, and the flow rate of the adsorption zone is 1-2 BV/h; the water washing area is purified water, the dosage of the purified water is 1.5 times of the volume of the resin, and the flow rate is 2BV/h; the desorbing agent is 30-60% ethanol solution, the dosage of the desorbing agent is 3 times of the volume of the resin, and the flow rate is 1-2 BV/h; the resin regeneration solvent is 95% ethanol solution, and the dosage is 1 time of that of the resin; the flow rate is 2-3 BV/h;
step 5, low-temperature concentration: recovering ethanol from the fine anthocyanin separating liquid of lycium ruthenicum obtained in the step 4, and concentrating at a low temperature under vacuum at 10 ℃ and a vacuum degree of-0.06 MPa to obtain about 25Kg of anthocyanin concentrated liquid of lycium ruthenicum;
step 6, freeze drying: and (3) directly freeze-drying the lycium ruthenicum anthocyanin concentrated solution obtained in the step (5) at the temperature of-50 to-70 ℃ by adopting a freeze dryer to obtain about 1.2Kg of lycium ruthenicum anthocyanin extract.
The anthocyanin content in the lycium ruthenicum anthocyanin extract is measured to be 56.0% by a pH differential method, and the total alkaloid content is measured to be 5.5% by a spectrophotometry.
The anthocyanin extract of Lycium ruthenicum has 92.9% of scavenging capacity to organic free radical (DPPH. Cndot.) and to superoxide anion (O. Cndot.) 2 The scavenging capacity of (-) free radical was 86.6%, and the scavenging capacity of P-hydroxyl free radical (. OH) was 96.3%.
The extract contains chemical components 1,2, 3,4, 5, 6, 7, 8, 9, 10 and 11, and has structural formula shown in figure 1.
Example 2
The preparation method of the lycium ruthenicum anthocyanin extract specifically comprises the following steps:
step 1, an extraction process: crushing 32Kg of dried lycium ruthenicum, putting the crushed dried lycium ruthenicum into 200L extraction equipment, adding deionized water with the volume of 5-10 times, soaking, stirring and extracting for 3-5 times to obtain crude lycium ruthenicum juice;
step 2, high-speed centrifugation and ceramic membrane filtration: centrifuging the crude lycium ruthenicum juice obtained in the step 1 by using a high-speed centrifuge with the rotating speed of 20000r/min to remove impurities, and clarifying by using a 100nm ceramic membrane to obtain about 800L of clarified lycium ruthenicum juice;
step 3, degumming and concentrating an organic film: removing pectin, protein and polysaccharide macromolecular substances from the clarified lycium ruthenicum juice obtained in the step 2 through an ultrafiltration organic membrane with the molecular weight cutoff of 100000, adding pure water with the volume of 3-5 times for cleaning, collecting effluent liquid, and dehydrating and concentrating through the ultrafiltration organic membrane with the molecular weight cutoff of 5000 to obtain about 15L of membrane concentrate;
step 4, simulated moving bed chromatographic separation: adding the membrane concentrate obtained in the step 3 into a simulated moving bed chromatography for separation to obtain 260L lycium ruthenicum fine anthocyanin separating liquid; the simulated moving bed separation method comprises the following steps: the simulated moving bed chromatography packed adsorbent is: the simulated moving bed chromatography packed adsorbent is: AB-8 macroporous resin, the flow rate of an adsorption area is 1-2 BV/h; the water washing area is purified water, the dosage of the purified water is 1.5 times of the volume of the resin, and the flow rate is 2BV/h; the desorbing agent is 30-60% ethanol solution, the dosage of the desorbing agent is 3 times of the volume of the resin, and the flow rate is 1-2 BV/h; the resin regeneration solvent is 95% ethanol solution, and the dosage is 1 time of that of the resin; the flow rate is 2-3 BV/h;
step 5, low-temperature concentration: recovering ethanol from the fine anthocyanin separating liquid of lycium ruthenicum obtained in the step 4, and concentrating at a low temperature under the condition of 50 ℃ and a vacuum degree of-0.06 MPa to obtain about 22Kg of anthocyanin concentrated liquid of lycium ruthenicum;
step 6, freeze drying: and (3) directly freeze-drying the lycium ruthenicum anthocyanin concentrated solution obtained in the step (5) at the temperature of-50 to-70 ℃ by adopting a freeze dryer to obtain about 0.69Kg of lycium ruthenicum anthocyanin extract.
The anthocyanin content in the lycium ruthenicum anthocyanin extract is 88.6% by a pH differential method, and the total alkaloid content is 0.12% by a spectrophotometry.
The anthocyanin extract of Lycium ruthenicum has 92.9% of scavenging capacity to organic free radical (DPPH. Cndot.) and to superoxide anion (O. Cndot.) 2 The scavenging capacity of (-) free radical was 86.6%, and the scavenging capacity of P-hydroxyl free radical (. OH) was 96.3%.
The extract contains chemical components 4, 8, 9, 10 and 11, and has a structural formula shown in figure 1.
Example 3
The preparation method of the lycium ruthenicum anthocyanin extract specifically comprises the following steps:
step 1, an extraction process: crushing 35Kg of dried lycium ruthenicum, putting the crushed dried lycium ruthenicum into 200L extraction equipment, adding deionized water with the volume of 5-10 times, soaking, stirring and extracting for 3-5 times to obtain crude lycium ruthenicum juice;
step 2, high-speed centrifugation and ceramic membrane filtration: centrifuging the crude lycium ruthenicum juice obtained in the step 1 by using a high-speed centrifuge with the rotating speed of 20000r/min to remove impurities, and clarifying by using a 200nm ceramic membrane to obtain the clarified lycium ruthenicum juice with the volume of 870L;
step 3, degumming and concentrating an organic film: removing pectin, protein and polysaccharide macromolecular substances from the clarified lycium ruthenicum juice obtained in the step 2 through an ultrafiltration organic membrane with the molecular weight cutoff of 50000, adding pure water with the volume of 3-5 times for cleaning, collecting effluent liquid, and dehydrating and concentrating through the ultrafiltration organic membrane with the molecular weight cutoff of 1000 to obtain about 17L of membrane concentrate;
step 4, simulated moving bed chromatographic separation: adding the membrane concentrate obtained in the step 3 into a simulated moving bed chromatography for separation to obtain 280L lycium ruthenicum fine anthocyanin separating liquid; the simulated moving bed separation method comprises the following steps: the simulated moving bed chromatography packed adsorbent is: the simulated moving bed chromatography packed adsorbent is: AB-8: NKA-9=1:1 mixed resin, and the flow rate of the adsorption zone is 1-2 BV/h; the water washing area is purified water, the dosage of the purified water is 1.5 times of the volume of the resin, and the flow rate is 2BV/h; the desorbent is 20-50% ethanol solution, the dosage of the desorbent is 3 times of the volume of the resin, and the flow rate is 1-2 BV/h; the resin regeneration solvent is 95% ethanol solution, and the dosage is 1 time of that of the resin; the flow rate is 2-3 BV/h;
step 5, low-temperature concentration: recovering ethanol from the fine anthocyanin separating liquid of lycium ruthenicum obtained in the step 4, and concentrating at a low temperature under vacuum at 20 ℃ and a vacuum degree of-0.06 MPa to obtain about 26Kg of anthocyanin concentrated liquid of lycium ruthenicum;
step 6, freeze drying: and (3) directly freeze-drying the lycium ruthenicum anthocyanin concentrated solution obtained in the step (5) at the temperature of-50 to-70 ℃ by adopting a freeze dryer to obtain about 1.26Kg of lycium ruthenicum anthocyanin extract.
The anthocyanin content in the lycium ruthenicum anthocyanin extract is measured to be 32.6% by a pH differential method, and the total alkaloid content is measured to be 18.2% by a spectrophotometry.
The anthocyanin extract of Lycium ruthenicum has 82.3% of scavenging capacity to organic free radical (DPPH. Cndot.) and to superoxide anion (O. Cndot.) 2 The scavenging capacity of (-) free radical was 75.6%, and the scavenging capacity of OH free radical (. OH) was 82.9%.
The extract contains chemical components 1,2, 3,4, 5, 6, 7, 8, 9, 10 and 11, and has structural formula shown in figure 1.
Example 4
The preparation method of the lycium ruthenicum anthocyanin extract specifically comprises the following steps:
step 1, an extraction process: crushing 150Kg of fresh lycium ruthenicum murr, squeezing, extracting residues by adding 200L of water each time, repeating for 3 times, and combining the filtrates to obtain about 750L of crude lycium ruthenicum murr juice;
step 2, high-speed centrifugation and ceramic membrane filtration: centrifuging the crude lycium ruthenicum juice obtained in the step 1 by using a butterfly centrifuge with the rotation speed of 15000r/min to remove impurities, and clarifying by using a 50nm ceramic membrane to obtain approximately 850L of clarified lycium ruthenicum juice;
step 3, degumming and concentrating an organic film: removing pectin, protein and polysaccharide macromolecular substances from the clarified lycium ruthenicum juice obtained in the step 2 through an ultrafiltration organic membrane with the molecular weight cutoff of 50000, adding pure water with the volume of 3-5 times for cleaning, collecting effluent liquid, and dehydrating and concentrating through the ultrafiltration organic membrane with the molecular weight cutoff of 5000 to obtain about 13L of membrane concentrate;
step 4, simulated moving bed chromatographic separation: adding the membrane concentrate obtained in the step 3 into a simulated moving bed chromatography for separation to obtain 180L of lycium ruthenicum fine anthocyanin separating liquid; the simulated moving bed separation method comprises the following steps: the simulated moving bed chromatography packed adsorbent is: the simulated moving bed chromatography packed adsorbent is: DS-401: BS-75=1:2 mixed resin, and the flow rate of an adsorption zone is 1-2 BV/h; the water washing area is purified water, the dosage of the purified water is 1.5 times of the volume of the resin, and the flow rate is 2BV/h; the desorbent is ethanol solution with 15-45% and the dosage is 3 times of the volume of the resin, and the flow rate is 1-2 BV/h; the resin regeneration solvent is 95% ethanol solution, and the dosage is 1 time of that of the resin; the flow rate is 2-3 BV/h;
step 5, low-temperature concentration: recovering ethanol from the fine anthocyanin separating liquid of lycium ruthenicum obtained in the step 4, and concentrating at a low temperature under the vacuum degree of-0.06 MPa at 25 ℃ to obtain about 15Kg of anthocyanin concentrated liquid of lycium ruthenicum;
step 6, freeze drying: and (3) directly freeze-drying the lycium ruthenicum anthocyanin concentrated solution obtained in the step (5) at the temperature of-50 to-70 ℃ by adopting a freeze dryer to obtain about 0.46Kg of lycium ruthenicum anthocyanin extract.
The anthocyanin content in the lycium ruthenicum anthocyanin extract is 15.2% by a pH differential method, and the total alkaloid content is 75.6% by a spectrophotometry.
Lycium ruthenicum anthocyanin extractionThe scavenging capacity of the substance for organic radicals (DPPH. Cndot.) was 77.8%, for superoxide anions (. Cndot.O) 2 The scavenging capacity of (-) free radical was 66.5%, and the scavenging capacity of p-hydroxy free radical (. OH) was 82.3%.
The extract contains chemical components 1,2, 3,4, 5, 6, 7, 8, 9, 10 and 11, and has structural formula shown in figure 1.
Example 5
The preparation method of the lycium ruthenicum anthocyanin extract specifically comprises the following steps:
step 1, an extraction process: crushing 180Kg of fresh lycium ruthenicum murr, squeezing juice, extracting residues by adding 200L of water each time, repeating for 3 times, and combining filtrate to obtain 830L of crude lycium ruthenicum murr juice;
step 2, high-speed centrifugation and ceramic membrane filtration: centrifuging the crude lycium ruthenicum juice obtained in the step 1 by using a butterfly centrifuge with the rotation speed of 15000r/min to remove impurities, and clarifying by using a 50nm ceramic membrane to obtain about 950L of clarified lycium ruthenicum juice;
step 3, degumming and concentrating an organic film: removing pectin, protein and polysaccharide macromolecular substances from the clarified lycium ruthenicum juice obtained in the step 2 through an ultrafiltration organic membrane with the molecular weight cutoff of 50000, adding pure water with the volume of 3-5 times for cleaning, collecting effluent liquid, and dehydrating and concentrating through the ultrafiltration organic membrane with the molecular weight cutoff of 5000 to obtain about 18L of membrane concentrate;
step 4, simulated moving bed chromatographic separation: adding the membrane concentrate obtained in the step 3 into a simulated moving bed chromatography for separation to obtain 80L lycium ruthenicum fine anthocyanin separating liquid; the simulated moving bed separation method comprises the following steps: the simulated moving bed chromatography packed adsorbent is: the simulated moving bed chromatography packed adsorbent is: NKA-2 resin, the flow rate of the adsorption area is 1-2 BV/h; the water washing area is purified water, the dosage of the purified water is 1.5 times of the volume of the resin, and the flow rate is 2BV/h; the desorbent is ethanol solution with the concentration of 5-25 percent, the dosage of the desorbent is 3 times of the volume of the resin, and the flow rate is 1-2 BV/h; the resin regeneration solvent is 95% ethanol solution, and the dosage is 1 time of that of the resin; the flow rate is 2-3 BV/h;
step 5, low-temperature concentration: recovering ethanol from the fine anthocyanin separating liquid of lycium ruthenicum obtained in the step 4, and concentrating at a low temperature under vacuum at 30 ℃ and a vacuum degree of-0.06 MPa to obtain about 8Kg of anthocyanin concentrated liquid of lycium ruthenicum;
step 6, freeze drying: and (3) directly freeze-drying the lycium ruthenicum anthocyanin concentrated solution obtained in the step (5) at the temperature of-50 to-70 ℃ by adopting a freeze dryer to obtain about 0.22Kg of lycium ruthenicum anthocyanin extract.
The anthocyanin content in the lycium ruthenicum anthocyanin extract is 3.2% by a pH differential method, and the total alkaloid content is 89.2% by a spectrophotometry.
The anthocyanin extract of Lycium ruthenicum has 62.8% of scavenging capacity to organic free radical (DPPH. Cndot.) and scavenging capacity to superoxide anion (O. Cndot.) 2 The scavenging capacity of (-) free radical was 56.5%, and the scavenging capacity of P-hydroxyl free radical (. OH) was 72.6%.
The extract contains chemical components 1,2, 3,4, 5, 6, 7, 8 and 10, and has structural formula shown in figure 1.
Example 6
The preparation method of the lycium ruthenicum anthocyanin freeze-dried powder specifically comprises the following steps:
step 1, an extraction process: crushing 40Kg of dried lycium ruthenicum, putting the crushed dried lycium ruthenicum into 200L extraction equipment, adding deionized water with the volume of 5-10 times, soaking, stirring and extracting for 3-5 times to obtain crude lycium ruthenicum juice;
step 2, high-speed centrifugation and ceramic membrane filtration: centrifuging the crude lycium ruthenicum juice obtained in the step 1 by using a high-speed centrifuge with the rotation speed of 20000r/min to remove impurities, and clarifying by using a 50nm ceramic membrane to obtain 960L clarified lycium ruthenicum juice;
step 3, degumming and concentrating an organic film: removing pectin, protein and polysaccharide macromolecular substances from the clarified lycium ruthenicum juice obtained in the step 2 through an ultrafiltration organic membrane with the molecular weight cutoff of 50000, adding pure water with the volume of 3-5 times for cleaning, collecting effluent liquid, and dehydrating and concentrating through the ultrafiltration organic membrane with the molecular weight cutoff of 5000 to obtain about 20L of membrane concentrate;
step 4, simulated moving bed chromatographic separation: adding the membrane concentrate obtained in the step 3 into a simulated moving bed chromatography for separation to obtain 320L lycium ruthenicum fine anthocyanin separating liquid; the simulated moving bed separation method comprises the following steps: the simulated moving bed chromatography packed adsorbent is: the simulated moving bed chromatography packed adsorbent is: HP750: d860021: ADS-7=1: 1:1 mixing resin, wherein the flow rate of an adsorption zone is 1-2 BV/h; the water washing area is purified water, the dosage of the purified water is 1.5 times of the volume of the resin, and the flow rate is 2BV/h; the desorbent is 20-50% ethanol solution, the dosage of the desorbent is 3 times of the volume of the resin, and the flow rate is 1-2 BV/h; the resin regeneration solvent is 95% ethanol solution, and the dosage is 1 time of that of the resin; the flow rate is 2-3 BV/h;
step 5, low-temperature concentration: recovering ethanol from the fine anthocyanin separating liquid of lycium ruthenicum obtained in the step 4, and concentrating at a low temperature under the vacuum degree of-0.06 MPa at 35 ℃ to obtain about 28Kg of anthocyanin concentrated liquid of lycium ruthenicum;
step 6, preparing freeze-dried powder: adding 10Kg of lactose into the lycium ruthenicum anthocyanin concentrated solution obtained in the step 5, stirring and mixing uniformly to obtain about 38Kg of anthocyanin lactose mixed solution, and freeze-drying at the temperature of-50 to-70 ℃ by adopting a freeze dryer to obtain about 12.5Kg of lycium ruthenicum anthocyanin freeze-dried powder.
The anthocyanin content in the freeze-dried lycium ruthenicum anthocyanin powder is measured by a pH differential method to be 8.6%, and the total alkaloid content is measured by a spectrophotometry to be 1.8%.
The Lycium ruthenicum anthocyanin lyophilized powder has 75.4% of scavenging ability to organic free radical (DPPH. Cndot.) and scavenging ability to superoxide anion (O) 2 The scavenging capacity of (-) free radical was 65.6%, and the scavenging capacity of p-hydroxy free radical (. OH) was 68.5%.
HPLC-MS/MS analysis shows that the freeze-dried powder of lycium ruthenicum anthocyanin contains chemical components 1,2, 3,4, 5, 6, 7, 8, 9 and 10, and the structural formula is shown in figure 1.
Example 7
The preparation method of the lycium ruthenicum anthocyanin freeze-dried powder specifically comprises the following steps:
step 1, an extraction process: crushing 200Kg of fresh lycium ruthenicum murr, squeezing juice, extracting residues by adding 220L of water each time, repeating for 3 times, and combining filtrate to obtain about 900L of crude lycium ruthenicum murr juice;
step 2, high-speed centrifugation and ceramic membrane filtration: centrifuging the crude lycium ruthenicum juice obtained in the step 1 by using a butterfly centrifuge with the rotation speed of 15000r/min to remove impurities, and clarifying by using a 50nm ceramic membrane to obtain about 950L of clarified lycium ruthenicum juice;
step 3, degumming and concentrating an organic film: removing pectin, protein and polysaccharide macromolecular substances from the clarified lycium ruthenicum juice obtained in the step 2 through an ultrafiltration organic membrane with the molecular weight cutoff of 50000, adding pure water with the volume of 3-5 times for cleaning, collecting effluent liquid, and dehydrating and concentrating through the ultrafiltration organic membrane with the molecular weight cutoff of 5000 to obtain about 22L of membrane concentrate;
step 4, simulated moving bed chromatographic separation: adding the membrane concentrate obtained in the step 3 into a simulated moving bed chromatography for separation to obtain 120L lycium ruthenicum fine anthocyanin separating liquid; the simulated moving bed separation method comprises the following steps: the simulated moving bed chromatography packed adsorbent is: the simulated moving bed chromatography packed adsorbent is: CAD-40: BS-45=1:1 mixed resin, and the flow rate of an adsorption zone is 1-2 BV/h; the water washing area is purified water, the dosage of the purified water is 1.5 times of the volume of the resin, and the flow rate is 2BV/h; the desorbent is an ethanol solution with the concentration of 15-40 percent, the dosage of the desorbent is 3 times of the volume of the resin, and the flow rate is 1-2 BV/h; the resin regeneration solvent is 95% ethanol solution, and the dosage is 1 time of that of the resin; the flow rate is 2-3 BV/h;
step 5, low-temperature concentration: recovering ethanol from the fine anthocyanin separating liquid of lycium ruthenicum obtained in the step 4, and concentrating at a low temperature under the vacuum degree of-0.06 MPa at 40 ℃ to obtain about 22Kg of anthocyanin concentrated liquid of lycium ruthenicum;
step 6, preparing freeze-dried powder: and (3) adding 15Kg of fructo-oligosaccharide into the concentrated solution of the lycium ruthenicum anthocyanin obtained in the step (5), stirring and uniformly mixing to obtain about 37Kg of mixed solution of the anthocyanin and the fructo-oligosaccharide, and freeze-drying at the temperature of-50 to-70 ℃ by adopting a freeze dryer to obtain about 16.5Kg of freeze-dried powder of the lycium ruthenicum anthocyanin.
The anthocyanin content in the freeze-dried lycium ruthenicum anthocyanin powder is 5.5 percent by a pH differential method, and the total alkaloid content is 3.2 percent by a spectrophotometry.
The Lycium ruthenicum anthocyanin lyophilized powder has 70.6% of scavenging capacity to organic free radical (DPPH. Cndot.) and scavenging capacity to superoxide anion (O) 2 (-) self-primingThe radical scavenging capacity was 61.2%, and the p-hydroxyl radical (. OH) scavenging capacity was 65.8%.
HPLC-MS/MS analysis shows that the freeze-dried powder of lycium ruthenicum anthocyanin contains chemical components 1,2, 3,4, 5, 6, 7, 8, 9 and 10, and the structural formula is shown in figure 1.
Example 8
The anthocyanin extract of Lycium ruthenicum has effect of improving sleep of mice.
Experimental model for injecting sodium pentobarbital into abdominal cavity of mouse
160 healthy male KM mice are selected, the weight of the healthy male KM mice is 20+/-2 g, the healthy male KM mice are randomly grouped according to the weight, and the healthy male KM mice are respectively a solvent control group, a lycium ruthenicum anthocyanin 1, a lycium ruthenicum anthocyanin 2 and a crude drug/kg dose group, wherein the total dose is 4 groups, and the total dose is 40 groups. The mice of the administration group are subjected to intragastric administration of lycium ruthenicum anthocyanin according to dosage, the mice of the solvent control group are subjected to intragastric administration of equal volume of double distilled water, and continuous intragastric administration is carried out for 30 days once daily. After the last administration for 1h, 10 mice of each group are respectively subjected to a direct sleep experiment, a barbital sodium subthreshold dose hypnotic experiment, a pentobarbital sodium sleep time experiment and a barbital sodium sleep latency experiment, and the experimental environment is kept at a quiet constant temperature.
(1) Direct sleep experiment
After the last administration of the experiment for 1h, each group of mice is observed to enter a sleep state within 60min, and the mice are considered to enter sleep after the disappearance of the regular reflection of the mice exceeds 1min, and the regular reflection of the mice is restored to be awake. The number of mice falling asleep and the time to fall asleep were counted for each group.
(2) Barbital sodium subthreshold dose hypnotic experiments
After the last administration of the experiment for 1 hour, each group of mice was intraperitoneally injected with pentobarbital sodium at a maximum sub-threshold hypnotic dose of 45mg/kg, the number of mice with the disappearance of 30min of the eversion regular reflection exceeding 1min was recorded, and the sleep occurrence rate was calculated, and the sleep occurrence rate = the number of mice falling asleep/the total number of mice of each group x 100%.
(3) Experiment for prolonging sleeping time of pentobarbital sodium
After the last administration of 1h, each group of mice was intraperitoneally injected with 300mg/kg of pentobarbital sodium, the time from the injection of pentobarbital sodium until the disappearance of the eversion of the mice was recorded, and the sleep latency of each group of mice was compared.
All data are as followsData statistical analysis was performed using SPSS16.0 software and group comparisons were performed using t-test.
Experimental results
TABLE 1 Effect of Lycium ruthenicum anthocyanin extract on sleep Rate in mice
The effect of different doses of lycium ruthenicum anthocyanin extract on the sleep latency of mice (see figures 5 and 6 for details). 1g crude drug/kg dose group of lycium ruthenicum anthocyanin A, 2.5g crude drug/kg dose group of lycium ruthenicum anthocyanin B, and 5g crude drug/kg dose group of lycium ruthenicum anthocyanin C, wherein P is less than 0.05 and P is less than 0.01.
Experimental results show that the lycium ruthenicum anthocyanin can obviously prolong the sleep time of mice, improve the sleep incidence rate, shorten the sleep latency and have remarkable effects on improving sleep.
The results show that in the direct sleep experiment, the number of the sleeping mice in the solvent control group and the black fruit Chinese wolfberry anthocyanin 1, 2.5 and 5g crude drug/kg dose group is 0, namely the black fruit Chinese wolfberry anthocyanin has no direct sleep induction effect, meets the requirements in the implementation manual of the technical specifications for health food inspection and evaluation, and can be used for evaluating other sleep improvement effects; in the pentobarbital sodium hypnotic experiment, compared with a solvent control group, the incidence of sleep of mice in the middle and high-dose groups of lycium ruthenicum anthocyanin is obviously improved (see table 1 for details); the high, medium and low doses of lycium ruthenicum anthocyanin can obviously prolong the sleeping time, and the sleeping latency of the medium and high dose group is obviously shortened.
Example 9
Lycium ruthenicum anthocyanin solid beverage and food
The freeze-dried powder of lycium ruthenicum anthocyanin prepared in example 6 is added with 21% of maltodextrin, 0.3% of sodium carboxymethyl cellulose and 4% of sucrose or xylitol, and the mixture is uniformly mixed by a CH-200 groove type mixer, and granulated by a conventional method to obtain the lycium ruthenicum anthocyanin solid beverage.
Example 10
Lycium ruthenicum anthocyanin tablet candy health food
22% of maltitol or xylitol or aspartame or stevioside, 13% of microcrystalline cellulose and 5% of magnesium stearate are added into the freeze-dried lycium ruthenicum anthocyanin powder prepared in the example 6, the mixture is uniformly mixed by a CH-200 groove type mixer, the dry granulation is carried out, and tabletting treatment (the pressure is 40-60 KN) is carried out by a ten-punch tablet press (ZPSX), so that the tabletting candy is obtained.
Example 11
Lycium ruthenicum anthocyanin capsule medicine
Adding 35-45% lactose or pregelatinized starch, 2% magnesium stearate, 5% talcum powder or micro powder silica gel into the lycium ruthenicum anthocyanin extract obtained in example 1 or the lycium ruthenicum anthocyanin freeze-dried powder prepared in example 6, uniformly mixing by using a CH-200 groove type mixer, granulating by a dry method, and filling by using an NJP-300 capsule filling machine to obtain capsules.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. The preparation method of the lycium ruthenicum anthocyanin extract is characterized by comprising the following steps of: the method specifically comprises the following steps:
step 1, an extraction process: crushing 30Kg of dried lycium ruthenicum, putting the crushed dried lycium ruthenicum into 200L extraction equipment, adding deionized water with the volume of 5-10 times, soaking, stirring and extracting for 3-5 times to obtain crude lycium ruthenicum juice;
step 2, high-speed centrifugation and ceramic membrane filtration: centrifuging the crude lycium ruthenicum juice obtained in the step 1 by using a high-speed centrifuge with the rotating speed of 20000r/min to remove impurities, and clarifying by using a 50nm ceramic membrane to obtain clarified lycium ruthenicum juice;
step 3, degumming and concentrating an organic film: removing pectin, protein and polysaccharide macromolecular substances from the clarified lycium ruthenicum juice obtained in the step 2 through an ultrafiltration organic membrane with the molecular weight cutoff of 50000, adding pure water with the volume of 3-5 times for cleaning, collecting effluent liquid, and dehydrating and concentrating through the ultrafiltration organic membrane with the molecular weight cutoff of 300 to obtain membrane concentrate;
step 4, simulated moving bed chromatographic separation: adding the membrane concentrate obtained in the step 3 into a simulated moving bed chromatography for separation to obtain a lycium ruthenicum fine anthocyanin separating liquid; the simulated moving bed separation method comprises the following steps: the simulated moving bed chromatography packed adsorbent is: HPD-100: DM130: ADS-21=2:2:1 mixed resin, and the flow rate of the adsorption zone is 1-2 BV/h; the water washing area is purified water, the dosage of the purified water is 1.5 times of the volume of the resin, and the flow rate is 2BV/h; the desorbing agent is 30-60% ethanol solution, the dosage of the desorbing agent is 3 times of the volume of the resin, and the flow rate is 1-2 BV/h; the resin regeneration solvent is 95% ethanol solution, and the dosage is 1 time of that of the resin; the flow rate is 2-3 BV/h;
step 5, low-temperature concentration: recovering ethanol from the fine anthocyanin separating liquid of lycium ruthenicum obtained in the step 4, and concentrating at a low temperature under the condition of 10 ℃ and a vacuum degree of-0.06 MPa to obtain a anthocyanin concentrated liquid of lycium ruthenicum;
step 6, freeze drying: and (3) directly freeze-drying the lycium ruthenicum anthocyanin concentrated solution obtained in the step (5) at the temperature of-50 to-70 ℃ by adopting a freeze dryer to obtain the lycium ruthenicum anthocyanin extract.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101991709A (en) * | 2010-11-09 | 2011-03-30 | 中国科学院西北高原生物研究所 | Method for preparing antioxidant lycium ruthenicum extract |
| CN109574979A (en) * | 2018-12-28 | 2019-04-05 | 中国科学院西北高原生物研究所湖州高原生物资源产业化创新中心 | A kind of black fruit fructus lycii blue anthocyanidin and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101991709A (en) * | 2010-11-09 | 2011-03-30 | 中国科学院西北高原生物研究所 | Method for preparing antioxidant lycium ruthenicum extract |
| CN109574979A (en) * | 2018-12-28 | 2019-04-05 | 中国科学院西北高原生物研究所湖州高原生物资源产业化创新中心 | A kind of black fruit fructus lycii blue anthocyanidin and preparation method thereof |
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| Lycium ruthenicum studies: molecular biology, phytochemistry and pharmacology;WANG, Hanqing等;《Food Chemistry》;20170805;第240卷;第759-766页 * |
| 崔大方、闫平.黑果枸杞.《认识中国植物 西北分册》.广东科技出版社,2018, * |
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