CN103446339A - Preparation method of lycium ruthenicum extract - Google Patents
Preparation method of lycium ruthenicum extract Download PDFInfo
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- CN103446339A CN103446339A CN2013103920773A CN201310392077A CN103446339A CN 103446339 A CN103446339 A CN 103446339A CN 2013103920773 A CN2013103920773 A CN 2013103920773A CN 201310392077 A CN201310392077 A CN 201310392077A CN 103446339 A CN103446339 A CN 103446339A
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Abstract
The invention relates to a preparation method of a lycium ruthenicum extract. The product is prepared from lycium ruthenicum by the processes of fruit selection, cleaning, extraction, centrifugation separation, membrane concentration, vacuum concentration, blending, drying and grinding. The method is used for solving the problems such as frequent loss of procyanidine and residue of organic solvent of a traditional method in producing lycium ruthenicum lozenges. The production method provided by the invention is simple at low cost, the procyanidine extraction rate exceeds 92%, and the prepared product is convenient to carry with high added value and without organic solvent residue.
Description
Technical field
The present invention relates to a kind of preparation method of berry fruit extract, specifically, relate to a kind of preparation method of black Fructus Lycii extract.
Background technology
Black Fructus Lycii (Lycium ruthenicum Murr) is the perennial shrub plant of Solanaceae Lycium.Black Fructus Lycii sweet in the mouth, the property heat of putting down, clear away heart-fire, can nourishing the liver and kidney, replenishing vital essence to improve eyesight, be applicable to soreness of the waist and knees, have a dizzy spell, the symptom such as bleary-eyed, the record black Fructus Lycii such as the classical Four-Volume Medical Code of Tibetan medicine and pharmacology, " Jingzhubencao " cure mainly heart-heat syndrome, heart disease, menoxenia, menolipsis etc." Uigurs medicine will " record Uygur medicine lycium ruthenicum fruit commonly used and root bark treatment calculus of urethra, the tinea scabies, the diseases such as gingiva bleeding gingival hemorrhage, among the peoplely make strengthening by means of tonics and the depressor modern scientific research has confirmed above-mentioned saying, and think that black Fructus Lycii can reduce cholesterol, excited cerebral nerve, strengthen immunologic function, anti-curing cancers, defying age and beauty treatment, black Fructus Lycii extract can promote cellular immune function, strengthen the generation of lymphopoiesis and tumor necrosis factor, interleukin II is had to two-way conciliation effect, energy diabetes-alleviating patient polydipsia polyphagia, disease loses weight.Black Fructus Lycii contains abundant fatty acid, protein, free amino acid, mineral element and polysaccharide etc., is conducive to human body directly absorb, and wherein the content of procyanidin, up to 3.45%, is the plant berry that natural procyanidins content is the highest.Procyanidin is that a class extensively is present in the water colo(u)r in plant, belongs to flavone compound, and anthocyanidin is that human body brings multiple benefit.Fundamentally, anthocyanidin is a kind of strong antioxidant, and it can protect human body to avoid the damage of the harmful substance of free radical.
At present, on market, the utilization of black Fructus Lycii is mainly drunk so that dry fruit is soaked, black Fructus Lycii main active substances-procyanidin is not fully utilized, and does not also develop the product of being convenient to market circulation.
Chinese patent application 201010525734.3 Lycium ruthenicum Murr proanthocyanidin products and preparation method thereof, be by the black Fructus Lycii fresh fruit be raw material through squeezing the juice, ceramic membrane remove impurity, macroporous adsorbent resin filter, spray drying obtains the procyanidin product, there are the shortcomings such as complex process, equipment requirements are higher, spray drying destructible anthocyanidin in this patent application.
Chinese patent application 201010542518.X method for preparing antioxidant lycium ruthenicum extract, through flooding by black Fructus Lycii, colloid mill and high pressure homogenize, remove impurity with microfiltration ceramic membrane again, through macroporous resin separation, spraying or lyophilization, obtain the antioxidation black Fructus Lycii extract, this patent application complex process, equipment requirements are high, spray drying destructible anthocyanidin, lyophilization increase the shortcomings such as cost.
The black Chinese wolfberry fruit industry of Chinese patent application 2013100627418 practical technique, to deceive Fructus Lycii ethanol pre-treatment, divide three 70-90 ℃ of hot water lixiviates to make, it is easily residual that this patent application adopts organic solvent pre-treatment to exist, the shortcomings such as hot water lixiviate destructible anthocyanidin.
All there is certain shortcoming in above-mentioned patent application, and especially the destruction of anthocyanidin is reduced Product Activity.
The present invention has carried out abundant analysis and research in conjunction with extracting method and the application prior art thereof of procyanidin in black Fructus Lycii, and has carried out a large amount of experimentatioies with regard to how improving procyanidin extraction ratio in black Fructus Lycii.
Summary of the invention
The objective of the invention is, in order to solve the black Fructus Lycii extract problem that the procyanidin rapid wear loses in preparation process, provides a kind of preparation method of black Fructus Lycii extract.
The invention provides a kind of production method of black Fructus Lycii extract, the concrete technology step is as follows:
(1) choosing fruit: reject the impurity such as immature fruit, silt, stone in fresh black Fructus Lycii or black Fructus Lycii dry fruit;
(2) clean: the black Fructus Lycii after selected is clean with purified rinse water;
(3) extract: at first in holding the extraction pot of black Fructus Lycii, add by weight 1: the pure water of 10-15, and add the 0.03-0.08% ascorbic acid of black Fructus Lycii weight ratio and the citric acid of 0.1-0.5%, extract at room temperature 25-40min takes out extracting solution; Add 8-12 pure water extract at room temperature 20-35min doubly by the black Fructus Lycii weight ratio again, get extracting solution, merge extracted twice liquid;
(4) centrifugalize: by centrifugalize under turn at 3500-4500/min of extracting solution condition, the feed intake 20-25 extracting solution doubly of weight of the black Fructus Lycii that to obtain solid content be 1.5-5%;
(5) membrance concentration: extracting solution is concentrated through NF membrane, obtain the concentrated solution that solid content is 12-15%;
(6) vacuum concentration: by above-mentioned concentrated solution, at feed temperature, be 45-55 ℃, the Radix osteomelis schwerinais Chinese holly concentrated solution that under vacuum 0.6-0.8Mpa condition, concentrated solid content is 30-35%;
(7) batching: add by weight percentage the starch of 10-15% and the citric acid of 0.1-0.5% in above-mentioned black Fructus Lycii concentrated solution;
(8) drying: above-mentioned gained batching is inserted in vacuum dryer, is 40-50 ℃ in temperature, is dried to water content 3-5% under vacuum 0.5-0.8Mpa condition;
(9) pulverize: by above-mentioned dried crushing material to the 150-200 order;
Drying in step of the present invention (8) can also adopt freeze-drying method to make black Fructus Lycii extract in-45-50 ℃ a condition.
Advantage of the present invention is: production method of the present invention is simple, and cost is low, and the procyanidin extraction rate reached is more than 92%, and the added value of product of preparation is high, and organic solvent-free is residual, has solved that cost is high, the problem of anthocyanidin destructible.
The specific embodiment
Embodiment 1
Selected 100kg black Fructus Lycii dry fruit, clean with purified rinse water, sampling be take catechin as standard substance, adopts hydrochloric acid-vanillin assay to be measured, and recording procyanidin content is 3.4%.
The black Fructus Lycii cleaned up is inserted in extraction pot, add the pure water of 1500kg, the ascorbic acid of 0.03kg and the citric acid of 0.5kg, extract 30min under room temperature and obtain extracting solution 1490kg, take out extracting solution, obtain extracting solution 985kg to extracting 20min under the pure water room temperature that adds 1000kg during black Fructus Lycii extracts the extraction pot of slag again, merge extracted twice liquid 2475kg; By centrifugalize under turn 4000/min of the extracting solution of above-mentioned merging condition, the extracting solution 2413kg that to obtain solid content be 1.5%; Said extracted liquid is concentrated through NF membrane, that to obtain solid content be 15% concentrated solution 240kg; By above-mentioned concentrated solution, at feed temperature, be 50 ℃ again, the Radix osteomelis schwerinais Chinese holly concentrated solution 110kg that under vacuum 0.7Mpa condition, concentrated solid content is 33%; Adding the starch of 11kg and adding during the citric acid of 0.33kg inserts vacuum dryer by weight 0.3% by weight 10% in above-mentioned concentrated solution, in temperature, it is 45 ℃, the black Fructus Lycii extract 53.13kg that under vacuum 0.8Mpa condition, dry moisture is 5%, be crushed to 150 orders packings and get product.
Get at random finished product 100 grams, take catechin as standard substance, adopting hydrochloric acid-vanillin assay to record procyanidin content is 5.9%, through measuring and calculating, by this implementation method, can make the extraction rate reached 92.9% of procyanidin in black Fructus Lycii.
Embodiment 2
Selected 100kg black Fructus Lycii dry fruit, clean with purified rinse water, sampling be take catechin as standard substance, adopts hydrochloric acid-vanillin assay to be measured, and recording procyanidin content is 3.43%.
The black Fructus Lycii cleaned up is inserted in extraction pot, add the pure water of 1000kg, the ascorbic acid of 0.08kg and the citric acid of 0.1kg, extract 40min under room temperature and obtain extracting solution 960kg, take out extracting solution, obtain extracting solution 1100kg to extracting 35min under the pure water room temperature that adds 1200kg during black Fructus Lycii extracts the extraction pot of slag again, merge extracted twice liquid 2060kg; By centrifugalize under turn 4500/min of the extracting solution of above-mentioned merging condition, the extracting solution 1620kg that to obtain solid content be 5%; Said extracted liquid is concentrated through NF membrane, that to obtain solid content be 14% concentrated solution 540kg; By above-mentioned concentrated solution, at feed temperature, be 55 ℃ again, the Radix osteomelis schwerinais Chinese holly concentrated solution 160kg that under vacuum 0.8Mpa condition, concentrated solid content is 35%; Adding the starch of 24kg and adding during the citric acid of 0.8kg inserts vacuum dryer by weight 0.5% by weight 15% in above-mentioned concentrated solution, in temperature, it is 50 ℃, the dry black Fructus Lycii extract 91kg that obtains moisture 4% under vacuum 0.6Mpa condition, be crushed to 200 orders packings and get product.
Get at random finished product 100 grams, take catechin as standard substance, adopting hydrochloric acid-vanillin assay to record procyanidin content is 3.5%, through measuring and calculating, by this implementation method, can make the extraction rate reached 92.85% of procyanidin in black Fructus Lycii.
Embodiment 3
Selected 100kg black Fructus Lycii dry fruit, clean with purified rinse water, sampling be take catechin as standard substance, adopts hydrochloric acid-vanillin assay to be measured, and recording procyanidin content is 3.38%.
The black Fructus Lycii cleaned up is inserted in extraction pot, add the pure water of 1300kg, the ascorbic acid of 0.05kg and the citric acid of 0.3kg, extract 25min under room temperature and obtain extracting solution 1285kg, take out extracting solution, obtain extracting solution 780kg to extracting 30min under the pure water room temperature that adds 800kg during black Fructus Lycii extracts the extraction pot of slag again, merge extracted twice liquid 2065kg; By centrifugalize under turn 3500/min of the extracting solution of above-mentioned merging condition, the extracting solution 2010kg that to obtain solid content be 3%; Said extracted liquid is concentrated through NF membrane, that to obtain solid content be 12% concentrated solution 503kg; By above-mentioned concentrated solution, at feed temperature, be 45 ℃ again, the Radix osteomelis schwerinais Chinese holly concentrated solution 168kg that under vacuum 0.6Mpa condition, concentrated solid content is 30%; Adding the starch of 21.8kg and adding during the citric acid of 0.168kg inserts vacuum dryer by weight 0.1% by weight 13% in above-mentioned concentrated solution, in temperature, it is 40 ℃, the dry black Fructus Lycii extract 85.8kg that obtains moisture 3% under vacuum 0.5Mpa condition, be crushed to 170 orders packings and get product.
Get at random finished product 100 grams, take catechin as standard substance, adopting hydrochloric acid-vanillin assay to record procyanidin content is 3.7%, through measuring and calculating, by this implementation method, can make the extraction rate reached 92.85% of procyanidin in black Fructus Lycii.
Embodiment 4
Selected 100kg black Fructus Lycii dry fruit, clean with purified rinse water, sampling be take catechin as standard substance, adopts hydrochloric acid-vanillin assay to be measured, and recording procyanidin content is 3.38%.
The black Fructus Lycii cleaned up is inserted in extraction pot, add the pure water of 1300kg, the ascorbic acid of 0.05kg and the citric acid of 0.3kg, extract 25min under room temperature and obtain extracting solution 1285kg, take out extracting solution, obtain extracting solution 780kg to extracting 30min under the pure water room temperature that adds 800kg during black Fructus Lycii extracts the extraction pot of slag again, merge extracted twice liquid 2065kg; By centrifugalize under turn 3500/min of the extracting solution of above-mentioned merging condition, the extracting solution 2010kg that to obtain solid content be 3%; Said extracted liquid is concentrated through NF membrane, that to obtain solid content be 12% concentrated solution 503kg; By above-mentioned concentrated solution, at feed temperature, be 45 ℃ again, the Radix osteomelis schwerinais Chinese holly concentrated solution 168kg that under vacuum 0.6Mpa condition, concentrated solid content is 30%; Adding the starch of 21.8kg and adding during the citric acid of 0.168kg inserts freeze drying equipment by weight 0.1% by weight 13% in above-mentioned concentrated solution, the dry black Fructus Lycii extract 85.8kg that obtains moisture 4% under-45 ℃ of conditions, be crushed to 170 orders packings and get product.
Get at random finished product 100 grams, take catechin as standard substance, adopting hydrochloric acid-vanillin assay to record procyanidin content is 3.7%, through measuring and calculating, by this implementation method, can make the extraction rate reached 92.85% of procyanidin in black Fructus Lycii.
Embodiment 5
The black Fructus Lycii concentrated solution prepared under condition similarly to Example 4 can obtain the black Fructus Lycii extract 85kg of moisture 3% in lyophilization under-55 ℃ of conditions, is crushed to 170 order packings and gets product.
Claims (3)
1. the preparation method of a black Fructus Lycii extract is characterized in that the processing step of described method is as follows:
(1) choosing fruit: reject the impurity such as immature fruit, silt, stone in fresh black Fructus Lycii or black Fructus Lycii dry fruit;
(2) clean: the black Fructus Lycii after selected is clean with purified rinse water;
(3) extract: at first in holding the extraction pot of black Fructus Lycii, add by weight 1: the pure water of 10-15, and add the 0.03-0.08% ascorbic acid of black Fructus Lycii weight ratio and the citric acid of 0.1-0.5%, extract at room temperature 25-40min takes out extracting solution; Add 8-12 pure water extract at room temperature 20-35min doubly by the black Fructus Lycii weight ratio again, get extracting solution, merge extracted twice liquid;
(4) centrifugalize: by centrifugalize under turn at 3500-4500/min of extracting solution condition, the feed intake 20-25 extracting solution doubly of weight of the black Fructus Lycii that to obtain solid content be 1.5-5%;
(5) membrance concentration: extracting solution is concentrated through NF membrane, obtain the concentrated solution that solid content is 12-15%;
(6) vacuum concentration: by above-mentioned concentrated solution, at feed temperature, be 45-55 ℃, the Radix osteomelis schwerinais Chinese holly concentrated solution that under vacuum 0.6-0.8Mpa condition, concentrated solid content is 30-35%;
(7) batching: add by weight percentage the starch of 10-15% and the citric acid of 0.1-0.5% in above-mentioned black Fructus Lycii concentrated solution;
(8) drying: above-mentioned gained batching is inserted in vacuum dryer, is 40-50 ℃ in temperature, is dried to water content 3-5% under vacuum 0.5-0.8Mpa condition;
(9) pulverize: above-mentioned dried crushing material to 150-200 order packing is got product.
2. the preparation method of a kind of black Fructus Lycii extract according to claim 1 is characterized in that the selection process step of described method is as follows:
(1) choosing fruit: reject the impurity such as immature fruit, silt, stone in fresh black Fructus Lycii or black Fructus Lycii dry fruit;
(2) clean: the black Fructus Lycii after selected is clean with purified rinse water;
(3) extract: at first in holding the extraction pot of black Fructus Lycii, add by weight 1: the pure water of 13-15, and add the 0.05-0.08% ascorbic acid of black Fructus Lycii weight ratio and the citric acid of 0.3-0.5%, extract at room temperature 25-30min takes out extracting solution; Add 8-10 pure water extract at room temperature 20-30mmin doubly by the black Fructus Lycii weight ratio again, get extracting solution, merge extracted twice liquid;
(4) centrifugalize: by centrifugalize under turn at 4000-4500/min of extracting solution condition, obtain the extracting solution that solid content is 3-5%;
(5) membrance concentration: extracting solution is concentrated through NF membrane, obtain the concentrated solution that solid content is 12-14%;
(6) vacuum concentration: by above-mentioned concentrated solution, at feed temperature, be 45-50 ℃, the Radix osteomelis schwerinais Chinese holly concentrated solution that under vacuum 0.7-0.8Mpa condition, concentrated solid content is 30-33%;
(7) batching: add by weight percentage the starch of 10-13% and the citric acid of 0.3-0.5% in above-mentioned black Fructus Lycii concentrated solution;
(8) drying: above-mentioned gained batching is inserted in vacuum dryer, is 40-45 ℃ in temperature, is dried to water content 3-4% under vacuum 0.6-0.8Mpa condition;
(9) pulverize: above-mentioned dried crushing material to 150-170 order packing is got product.
3. the preparation method of a kind of black Fructus Lycii extract according to claim 1 and 2, is characterized in that, the vacuum drying in the described drying means also freeze-drying method of available-45～-50 ℃ condition replaces.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104248036A (en) * | 2014-09-19 | 2014-12-31 | 青海诺蓝杞生物科技开发有限公司 | Lycium ruthenicum Murr procyanidine effervescent tablet and production method thereof |
| CN105166933A (en) * | 2015-10-28 | 2015-12-23 | 青海尤尼克生物技术有限公司 | Composition containing Chinese wolfberry fruit extract and fruit ferment and preparation method thereof |
| CN107198240A (en) * | 2017-07-12 | 2017-09-26 | 青岛大学 | The combined extraction method of plurality of active ingredients in black fruit fructus lycii |
| CN109833238A (en) * | 2017-11-27 | 2019-06-04 | 重庆戴贺李生物科技有限公司 | A kind of extracting method of black fruit fructus lycii active matter used for cosmetic |
| CN111534410A (en) * | 2020-06-13 | 2020-08-14 | 劲牌有限公司 | Preparation method and application of lycium ruthenicum concentrated solution |
| CN115530369A (en) * | 2022-08-24 | 2022-12-30 | 可菲生物科技有限公司 | Preparation method for preparing mixed extract by using lycium ruthenicum murr and shaddock peel |
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| CN1258512A (en) * | 1998-12-28 | 2000-07-05 | 启东市天和生物制品有限公司 | Lycium chinense glycopeptide and its production process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104248036A (en) * | 2014-09-19 | 2014-12-31 | 青海诺蓝杞生物科技开发有限公司 | Lycium ruthenicum Murr procyanidine effervescent tablet and production method thereof |
| CN105166933A (en) * | 2015-10-28 | 2015-12-23 | 青海尤尼克生物技术有限公司 | Composition containing Chinese wolfberry fruit extract and fruit ferment and preparation method thereof |
| CN107198240A (en) * | 2017-07-12 | 2017-09-26 | 青岛大学 | The combined extraction method of plurality of active ingredients in black fruit fructus lycii |
| CN109833238A (en) * | 2017-11-27 | 2019-06-04 | 重庆戴贺李生物科技有限公司 | A kind of extracting method of black fruit fructus lycii active matter used for cosmetic |
| CN111534410A (en) * | 2020-06-13 | 2020-08-14 | 劲牌有限公司 | Preparation method and application of lycium ruthenicum concentrated solution |
| CN115530369A (en) * | 2022-08-24 | 2022-12-30 | 可菲生物科技有限公司 | Preparation method for preparing mixed extract by using lycium ruthenicum murr and shaddock peel |
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Application publication date: 20131218 |