CN111534410A - Preparation method and application of lycium ruthenicum concentrated solution - Google Patents
Preparation method and application of lycium ruthenicum concentrated solution Download PDFInfo
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- CN111534410A CN111534410A CN202010538477.0A CN202010538477A CN111534410A CN 111534410 A CN111534410 A CN 111534410A CN 202010538477 A CN202010538477 A CN 202010538477A CN 111534410 A CN111534410 A CN 111534410A
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
- C12G3/00—Preparation of other alcoholic beverages
- C12G3/04—Preparation of other alcoholic beverages by mixing, e.g. for preparation of liqueurs
- C12G3/05—Preparation of other alcoholic beverages by mixing, e.g. for preparation of liqueurs with health-improving ingredients, e.g. flavonoids, flavones, polyphenols or polysaccharides
- C12G3/055—Preparation of other alcoholic beverages by mixing, e.g. for preparation of liqueurs with health-improving ingredients, e.g. flavonoids, flavones, polyphenols or polysaccharides extracted from plants
Abstract
The invention discloses a preparation method and application of a lycium ruthenicum concentrated solution, and particularly relates to a lycium ruthenicum concentrated solution which is obtained by stirring and extracting 0.15-0.2 times of a malic acid alcohol solution for 5-8 hours, respectively filtering an extracting solution through disc centrifugation, a ceramic membrane and an ultrafiltration membrane, and concentrating through a nanofiltration membrane. The preparation method disclosed by the invention is environment-friendly, simple in process, low in production cost, high in efficiency, short in period, easy to popularize and high in anthocyanin preservation rate of lycium ruthenicum; the prepared lycium ruthenicum concentrated solution has high anthocyanin content and good stability.
Description
Technical Field
The invention relates to the technical field of extraction and separation of plant components, and particularly relates to a preparation method and application of a lycium ruthenicum concentrated solution.
Background
Lycium ruthenicum Murr is a Lycium L of Solanaceae, mature fruits of which are purple black, is a perennial salt-resistant and drought-resistant wild Lycium chinense resource newly discovered in recent years, and is a special wild plant to be developed urgently in northwest China. The lycium ruthenicum murr is an important position in traditional Chinese medicine (Tibetan medicine), the Tibetan medicine is called lycium ruthenicum murr as ' side Ma ', the lycium ruthenicum murr has sweet taste, mild nature and heat clearing effect, mature fruits of the lycium ruthenicum murr are rich in various nutritional ingredients such as protein, lycium ruthenicum polysaccharide, amino acid, vitamin, mineral substances, trace elements and the like, particularly the natural anthocyanin is rich, the anthocyanin content of the natural anthocyanin exceeds fruit juice pigments such as blueberry, cowberry fruit, black currant, mulberry and the like and reaches 3879mg/l00g, the natural wild plant with the highest anthocyanin content is found so far, and the natural wild plant has the reputation of ' king of anthocyanin ' and ' blue goby-shaped hypi. Modern pharmacological research shows that the lycium ruthenicum extract has wide pharmacological effects of reducing blood fat, reducing blood sugar, resisting oxidation, resisting aging and the like, has few toxic and side effects, has far higher medicinal and health-care values than common lycium ruthenicum, has good medical and health-care effects, and is known as 'soft gold', so that the extract can be used for extracting and separating the anthocyanin substances from the lycium ruthenicum, and developing functional foods or serving as raw materials of medicinal and health-care products.
At present, the extraction method of lycium ruthenicum is mostly a solvent extraction mode, most of the extraction methods are ethanol extraction, and the problem of serious loss of effective components in the production process and the application process is caused by the problem that anthocyanin is easy to oxidize in the extraction process.
Therefore, there is a need to develop a method for improving the stability of the production process and the application process.
Disclosure of Invention
The invention aims to provide a preparation method for stable production of lycium ruthenicum concentrated solution, which is environment-friendly, simple in process, low in production cost, short in period and easy to popularize, and effectively reduces the loss of anthocyanin in the production process and the preservation process.
The invention also aims to provide the lycium ruthenicum concentrated solution with high anthocyanin preservation rate.
The invention also aims to provide application of the lycium ruthenicum in preparing the compound wine.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
A preparation method of Lycium ruthenicum Murr concentrated solution comprises the following steps:
extracting Lycium ruthenicum Murr with 0.15-0.2 times of malic acid alcoholic solution under stirring for 5-8 hr to obtain Lycium ruthenicum Murr extractive solution; and (3) respectively performing disc centrifugation, ceramic membrane filtration and ultrafiltration membrane filtration on the extracting solution, and concentrating by using a nanofiltration membrane to obtain the lycium ruthenicum concentrated solution.
In the preferred embodiment of the present invention, the extraction conditions of lycium ruthenicum are as follows: adding Lycium ruthenicum Murr medicinal material into an alcohol solution 8-15 times of the medicinal material and 50% -60% in concentration, adding malic acid 0.15-0.2 times of the medicinal material into the alcohol solution, and stirring and extracting at 50-60 ℃ for 5-8 hours to obtain Lycium ruthenicum Murr extract.
In the preferred embodiment of the invention, the parameters of the centrifugation of the lycium ruthenicum extract are that the disc centrifugation rotating speed is more than or equal to 3000r/min, and the centrifugate is collected; the filtering parameters of the ceramic membrane are that the aperture of the ceramic membrane is less than or equal to 0.1um, the filtering operation temperature is less than or equal to 50 ℃, and the permeate is collected; the ultrafiltration membrane filtration parameters are that the cut-off molecular weight of the ultrafiltration membrane is less than or equal to 100000, the ultrafiltration temperature is less than or equal to 45 ℃, and the permeate is collected.
In the preferred embodiment of the invention, the lycium ruthenicum ultrafiltration permeate is finally concentrated by a nanofiltration membrane to remove alcohol and most of malic acid, the concentration parameters of the nanofiltration membrane are that the molecular weight cut-off of the nanofiltration membrane is less than or equal to 500, the nanofiltration temperature is less than or equal to 45 ℃, and the concentration is concentrated to the crude drug concentration of 0.3-0.4Kg/L, and the trapped fluid is collected to obtain the lycium ruthenicum concentrated solution.
The invention provides a lycium ruthenicum concentrated solution which is prepared by adopting the preparation method of the lycium ruthenicum concentrated solution.
In the preferred embodiment of the invention, the concentrated lycium ruthenicum murr solution has an anthocyanin preservation rate of over 96% through three-month stability experiment investigation.
The invention provides application of the lycium ruthenicum concentrated solution in production of compound wine.
In the preferred embodiment of the invention, the Lycium ruthenicum Murr concentrated solution is applied to the compound wine at a crude drug concentration of 0.01-0.05 g/ml.
Compared with the prior art, the preparation method of the lycium ruthenicum concentrated solution is environment-friendly, simple in process, low in production cost, high in efficiency, short in period, easy to popularize and high in anthocyanin preservation rate of the lycium ruthenicum; the prepared lycium ruthenicum concentrated solution has high anthocyanin content and good stability.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation process flow of the lycium ruthenicum concentrated solution in the embodiment is shown in fig. 1, and specifically includes:
first, preparation method
(1) Extraction: adding 1000g of lycium ruthenicum murr medicinal material into 10L of 50% alcohol solution, adding 160g of malic acid into the alcohol solution, and stirring and extracting at 50 ℃ for 6 hours to obtain lycium ruthenicum murr extract.
(2) Centrifuging: centrifuging the extractive solution with a disc centrifuge at a rotation speed of 3000r/min or more, and collecting the centrifugate.
(3) Ceramic membrane filtration: the disk centrifugate is filtered by a ceramic membrane to collect the permeate, the aperture of the ceramic membrane is less than or equal to 0.1um, and the filtering operation temperature is less than or equal to 50 ℃.
(4) And (3) ultrafiltration membrane filtration: filtering the ceramic membrane filtrate with ultrafiltration membrane to collect the filtrate, wherein the cut-off molecular weight of the ultrafiltration membrane is less than or equal to 100000, and the ultrafiltration temperature is less than or equal to 45 ℃.
(5) Concentrating a nanofiltration membrane: concentrating the filtrate of the ultrafiltration membrane by using a nanofiltration membrane, collecting trapped fluid, removing alcohol and most malic acid, wherein the trapped molecular weight of the nanofiltration membrane is less than or equal to 500, the nanofiltration temperature is less than or equal to 45 ℃, and the final volume of the trapped fluid is constant volume of 300ml, thus obtaining the concentrated solution of lycium ruthenicum. The anthocyanin purity is 20.5% through drying detection, and the total loss rate in the production process is 9.1%.
Second, application
The concentrated solution is applied to a prepared wine to prepare 1000ml of wine body, and the prepared wine is prepared by taking 800ml of wine, adding 90ml of lycium ruthenicum concentrated solution, adding 15g of xylitol, using white spirit wine base to regulate the volume to 16% vol, adding water to a constant volume of 1000ml, uniformly stirring, standing for 15 days under the conditions of shade, cool and light-proof, and filtering. The stability experiment investigation of the wine body for 3 months proves that the anthocyanin preservation rate is 98%.
Example 2
First, preparation method
(1) Extraction: 1000g of lycium ruthenicum murr medicinal material is added into 15L of 50% alcohol solution, 200g of malic acid is added into the alcohol solution, and stirring extraction is carried out at 50 ℃ for 8 hours to obtain lycium ruthenicum murr extract.
(2) Centrifuging: centrifuging the extractive solution with a disc centrifuge at a rotation speed of 3000r/min or more, and collecting the centrifugate.
(3) Ceramic membrane filtration: the disk centrifugate is filtered by a ceramic membrane to collect the permeate, the aperture of the ceramic membrane is less than or equal to 0.1um, and the filtering operation temperature is less than or equal to 50 ℃.
(4) And (3) ultrafiltration membrane filtration: filtering the ceramic membrane filtrate with ultrafiltration membrane to collect the filtrate, wherein the cut-off molecular weight of the ultrafiltration membrane is less than or equal to 100000, and the ultrafiltration temperature is less than or equal to 45 ℃.
(5) Concentrating a nanofiltration membrane: concentrating the filtrate of the ultrafiltration membrane by using a nanofiltration membrane, collecting trapped fluid, removing alcohol and most malic acid, wherein the trapped molecular weight of the nanofiltration membrane is less than or equal to 500, the nanofiltration temperature is less than or equal to 45 ℃, and the final volume of the trapped fluid is constant volume of 300ml, thus obtaining the concentrated solution of lycium ruthenicum. The anthocyanin purity is 18.3% through drying detection, and the total loss rate in the production process is 11.7%.
Second, application
The concentrated solution is applied to a prepared wine to prepare 1000ml of wine body, and the prepared wine is prepared by taking 600ml of wine, adding 90ml of lycium ruthenicum concentrated solution, adding 15g of xylitol, using white spirit wine base to regulate the volume to 18% vol, adding water to a constant volume of 1000ml, uniformly stirring, standing for 15 days under the conditions of shade, cool and light-proof, and filtering. The stability experiment of the wine body for 3 months proves that the anthocyanin preservation rate is 96.22 percent.
Comparative example 1
First, preparation method
(1) Extraction: taking 10kg of lycium ruthenicum murr medicinal material, adding 60% ethanol, extracting at 60 ℃ for 3 times, each time for two hours, adding 150L of 60% ethanol for the first time, adding 100L of 60% ethanol for the second time and the third time respectively, and combining the three extracting solutions to obtain the lycium ruthenicum murr extracting solution.
(2) Centrifuging: centrifuging the extractive solution with a disc centrifuge at a rotation speed of 3000r/min or more, and collecting the centrifugate.
(3) Ceramic membrane filtration: the disk centrifugate is filtered by a ceramic membrane to collect the permeate, the aperture of the ceramic membrane is less than or equal to 0.1um, and the filtering operation temperature is less than or equal to 50 ℃.
(4) And (3) concentrating under reduced pressure: and (3) carrying out reduced pressure concentration on the ceramic membrane filtrate by using a scraper concentrator, controlling the temperature to be less than or equal to 55 ℃ in the concentration process, keeping the final volume constant to 30L, detecting the purity of the anthocyanin to be 12% by drying, and keeping the total loss rate of the production process to be 15.53%.
Second, application
The concentrated solution is applied to a prepared wine to prepare 1000ml of wine body, and the prepared wine is prepared by taking 800ml of wine, adding 90ml of lycium ruthenicum concentrated solution, adding 15g of xylitol, using white spirit wine base to regulate the volume to 16% vol, adding water to a constant volume of 1000ml, uniformly stirring, standing for 15 days under the conditions of shade, cool and light-proof, and filtering. The stability test of the wine body for 3 months proves that the anthocyanin preservation rate is 88%.
Experimental results prove that the lycium ruthenicum concentrated solution with high anthocyanin content and good stability can be prepared only by the specific extraction process, and when the process parameters are beyond the range of the invention, the anthocyanin content and the stability are both lower.
The method can effectively prepare the lycium ruthenicum concentrated solution with high anthocyanin content and good stability, and the applied compound wine has high anthocyanin storage rate, good stability and excellent effect. The above-mentioned embodiments only express the embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. A preparation method of a lycium ruthenicum concentrated solution is characterized by comprising the following steps:
extracting Lycium ruthenicum Murr with 0.15-0.2 times of malic acid alcoholic solution under stirring for 5-8 hr to obtain Lycium ruthenicum Murr extractive solution; and (3) respectively performing disc centrifugation, ceramic membrane filtration and ultrafiltration membrane filtration on the extracting solution, and concentrating by using a nanofiltration membrane to obtain the lycium ruthenicum concentrated solution.
2. The preparation method according to claim 1, wherein the lycium ruthenicum extraction conditions are as follows: adding Lycium ruthenicum Murr medicinal material into an alcohol solution 8-15 times of the medicinal material and 50% -60% in concentration, adding malic acid 0.15-0.2 times of the medicinal material into the alcohol solution, and stirring and extracting at 50-60 ℃ for 5-8 hours to obtain Lycium ruthenicum Murr extract.
3. The preparation method according to claim 1, wherein the centrifugation parameter of the lycium ruthenicum extract is that the disc centrifugation rotating speed is more than or equal to 3000r/min, and the centrifugate is collected; the filtering parameters of the ceramic membrane are that the aperture of the ceramic membrane is less than or equal to 0.1um, the filtering operation temperature is less than or equal to 50 ℃, and the permeate is collected; the ultrafiltration membrane filtration parameters are that the cut-off molecular weight of the ultrafiltration membrane is less than or equal to 100000, the ultrafiltration temperature is less than or equal to 45 ℃, and the permeate is collected.
4. The preparation method according to claims 1-3, wherein the Lycium ruthenicum Murr ultrafiltration permeate is finally concentrated by a nanofiltration membrane to remove alcohol and most of malic acid, the nanofiltration membrane concentration parameter is that the nanofiltration membrane cut-off molecular weight is less than or equal to 500, the nanofiltration temperature is less than or equal to 45 ℃, the concentration is carried out until the crude drug concentration is 0.3-0.4Kg/L, and the trapped fluid is collected to obtain the Lycium ruthenicum Murr concentrated solution.
5. Lycium ruthenicum concentrate prepared by the preparation method of any one of claims 1 to 4.
6. The Lycium ruthenicum Murr concentrate of claim 5, wherein the concentrated Lycium ruthenicum Murr concentrate has an anthocyanin preservation rate of more than 96% through three-month stability experiment examination.
7. Use of the Lycium ruthenicum concentrate of claim 5 or 6 in the manufacture of a wine blend.
8. The use of claim 7, wherein the Lycium ruthenicum Murr concentrate is used in the formulated wine at a crude drug concentration of 0.01-0.05/ml.
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