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CN106083796A - A kind of extracting method of vaccinium oxycoccus pigment - Google Patents

A kind of extracting method of vaccinium oxycoccus pigment Download PDF

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Publication number
CN106083796A
CN106083796A CN201610441777.0A CN201610441777A CN106083796A CN 106083796 A CN106083796 A CN 106083796A CN 201610441777 A CN201610441777 A CN 201610441777A CN 106083796 A CN106083796 A CN 106083796A
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vaccinium oxycoccus
oxycoccus pigment
extract
supernatant
solution
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仇颖莹
张明
王龙
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/58Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
    • C07D311/60Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
    • C07D311/62Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00Dyes of natural origin prepared from natural sources, e.g. vegetable sources

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention discloses the extracting method of a kind of vaccinium oxycoccus pigment, belong to field of natural organic chemistry.The present invention is with blue berry as raw material, and crushing and beating, is that 40% ethanol solution is as extracting solution with mass fraction, and add cellulase, extract under ultrasonic wave added, then be performing centrifugal separation on, precipitation repeats to extract once, after united extraction liquid concentrates, passes through high-pressure pulse electric, promote the dissolution of vaccinium oxycoccus pigment, increase the vaccinium oxycoccus pigment stripping quantity of extracting solution, then through absorption with macroporous adsorbent resin, alcohol is washed, concentrate, lyophilization, thus obtain vaccinium oxycoccus pigment extracting method.Example proves, the present invention operates controlled, and method is unique, decreases production cost, pollution-free so that the vaccinium oxycoccus pigment extraction ratio up to more than 80% prepared, high purity more than 75%, has higher value medical health care and broader practical application area.

Description

A kind of extracting method of vaccinium oxycoccus pigment
Technical field
The invention discloses the extracting method of a kind of vaccinium oxycoccus pigment, belong to field of natural organic chemistry.
Background technology
Anthocyanidin also known as anthocyanidin, is the water-soluble natural pigment that is widely present in plant of a class, belongs to flavonoid Thing, it is anthocyanin after being combined with glycosidic bond with glucide, is a kind of natural antioxidant.Owing to anthocyanidin is unstable Fixed, mainly exist with anthocyanin in plant.
Anthocyanidin is as a kind of natural food colour, safe and nontoxic, aboundresources, and has certain nutrition and pharmacology Effect, has huge application potential at aspects such as food, cosmetic, medicine.Anthocyanidin is that the nutrition of the defying age of pure natural is mended Filling agent, research proves mankind nowadays and finds maximally effective antioxidant, is the maximally effective antioxidant of current nature.With Time have research title can vision enhancing, anti-eye strain;Delay cranial nerve old and feeble.Anthocyanidin contained by blue berry is current all plants In anthocyanidin, function is the most excellent, range of application is the widest, and side effect is minimum, is also the kind that price is the most expensive.Anthocyanidin content reaches The blueberry extract price of 25% is 5~6 times that content reaches the Semen Vitis viniferae extract of 95%, it is seen that its value free from worldly cares.Blue berry Root, stem, leaf, peel, sarcocarp all contain anthocyanidin, and is present in the vacuole of blue berry cell.
Research to the extraction of anthocyanidin at present mainly has water to carry or organic solvent extraction, supercritical fluid extraction Deng.Traditional water carry or solvent extraction method exist due to the too high structure that can destroy anthocyanidin of temperature, affect its biological activity and The problems such as productivity reduction;Although modern supercritical extraction extraction ratio is high, but because of apparatus expensive, is not suitable for industrialized production.
Strong in order to solve blue berry Seasonal Harvest, and it is difficult to storage, unsalable blue berry had both caused huge because rotting Economic loss, the problem polluting again environment, what the present invention provided a kind of high-efficiency and economic extracts vaccinium oxycoccus pigment from blue berry Method, makes full use of vaccinium oxycoccus pigment, expands the application of vaccinium oxycoccus pigment.
Summary of the invention
The technical problem that present invention mainly solves: extracting during anthocyanidin for current traditional method, water carry or Solvent extraction method can affect its biological activity and productivity due to temperature too high destruction anthocyanidin structure, and supercritical extraction Though extraction ratio can be improved, but apparatus expensive, cost is high, is difficult to the present situation of industrialized production, it is provided that one with blue berry is Raw material, crushing and beating, with mass fraction be 40% ethanol solution as extracting solution, and add cellulase, carry under ultrasonic wave added Taking, then be performing centrifugal separation on, precipitation repeats to extract once, after united extraction liquid concentrates, by high-pressure pulse electric, to two interpolars Material applies the high voltage of short pulse punching and processes, and makes polar substances move to electrode direction at a high speed under the effect of electric field, utilizes thin After birth electroporation principle, causes histiocytic irreversible breaking, thus promotes the dissolution of vaccinium oxycoccus pigment, increases extracting solution Vaccinium oxycoccus pigment stripping quantity, then through absorption with macroporous adsorbent resin, alcohol is washed, and concentrates, lyophilization, thus obtains vaccinium oxycoccus pigment and carry Access method.The method operation is controlled, and method is unique, decreases production cost, pollution-free so that the vaccinium oxycoccus pigment prepared extracts Rate up to more than 80%, high purity more than 75%, there is higher value medical health care and broader practical application area.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) weigh 200~300g blue berry and clean roguing, add crushing and beating 10 in refiner with 200~300mL deionized waters ~15min, it is in 40% ethanol solution by blue berry serosity addition 2~3L mass concentrations, under 50~52 DEG C of waters bath with thermostatic control, adds 30~45g cellulase, and with 200W ultrasonic echography 10~12min, be that 10% hydrochloric acid solution regulates pH extremely by mass concentration 2.0~2.5, extract 2~3h, lixiviating solution inserted in 4000~6000/min centrifuges centrifugal 10~15min, must precipitate and on Clear liquid, is extracted once by precipitation by aforesaid operations and is collected supernatant again, merges supernatant, by supernatant at 50~55 DEG C, It is evaporated to the 30~35% of original volume, obtains vaccinium oxycoccus pigment crude extract;
(2) quality added containing mass concentration is 0.1% hydrochloric acid by solid-liquid ratio 1:6~1:7 by above-mentioned vaccinium oxycoccus pigment crude extract is dense Degree is in 60% ethanol solution, and with 7~8mL/min by high-pressure pulse electric, controlling umber of pulse is 8~10, and electric field intensity is 18~19KV/cm, and mixed liquor is inserted in 4000~6000/min centrifuges centrifugal 10~15min, take supernatant, obtain blue berry Anthocyanidin two extract;
(3) above-mentioned vaccinium oxycoccus pigment two extract is filled with 2~4 times of column volumes/h flow velocity process the adsorption column of macroporous resin, Repetition aforesaid operations is to extracting liquid colourless, then is that 70% ethanol solution is washed with 0.1~0.5 times of column volume/h flow velocity by mass concentration De-by the vaccinium oxycoccus pigment of macroporous resin adsorption, collect eluent, eluent is reduced pressure dense in 50~55 DEG C of vacuum drying ovens Contracting, obtains vaccinium oxycoccus pigment by concentrated solution lyophilization.
The application process of the present invention is: by solid-to-liquid ratio 1: 50~1: 100, the vaccinium oxycoccus pigment present invention prepared pours temperature into In boiled water, stir, oral, it is proposed that morning and evening every day one after each meal, take rear fasting seafood, maror, adhere to even Continue and take 7~14 days, can substantially feel the fine and smooth gloss that skin becomes, enhance the immunity of skin, for easy autopath, Can be effective against various allergic conditions, effect is the most notable.
The invention has the beneficial effects as follows:
(1) present invention operates controlled, and method is unique, without specific apparatus during preparation, decreases production cost, without dirty Dye, belongs to environmental protection technique;
(2) present invention passes through high-pressure pulse electric, the material of two interpolars is applied the high voltage process that short pulse rushes so that polar material Matter is moved to electrode direction at a high speed under the effect of electric field, utilizes electroporation of cell membrane principle, causes histiocytic irreversible Destroy, thus promote the dissolution of vaccinium oxycoccus pigment, increase the vaccinium oxycoccus pigment stripping quantity of extracting solution, improve extraction ratio;
(3) present invention finally makes the vaccinium oxycoccus pigment extraction ratio up to more than 80% prepared, high purity more than 75%, has Higher value medical health care and broader practical application area.
Detailed description of the invention
First weigh 200~300g blue berry and clean roguing, add in refiner broken with 200~300mL deionized waters Blue berry serosity addition 2~3L mass concentrations are in 40% ethanol solution, 50~52 DEG C of waters bath with thermostatic control by making beating 10~15min Under, add 30~45g cellulase, and with 200W ultrasonic echography 10~12min, be that 10% hydrochloric acid solution is adjusted by mass concentration Joint pH to 2.0~2.5, extracts 2~3h, is inserted by lixiviating solution and is centrifuged 10~15min in 4000~6000/min centrifuges, and it is heavy to obtain Form sediment and supernatant, precipitation is extracted once and collected supernatant by aforesaid operations again, merge supernatant, by supernatant 50~55 At DEG C, it is evaporated to the 30~35% of original volume, obtains vaccinium oxycoccus pigment crude extract;Then by above-mentioned vaccinium oxycoccus pigment crude extract The mass concentration added containing mass concentration is 0.1% hydrochloric acid by solid-liquid ratio 1:6~1:7 is in 60% ethanol solution, with 7~8mL/ Min passes through high-pressure pulse electric, and controlling umber of pulse is 8~10, and electric field intensity is 18~19KV/cm, and is inserted by mixed liquor 4000~6000/min centrifuges are centrifuged 10~15min, take supernatant, obtain vaccinium oxycoccus pigment two extract;Finally by above-mentioned indigo plant Certain kind of berries anthocyanidin two extract through being filled with the adsorption column of macroporous resin, repeats aforesaid operations to carrying with 2~4 times of column volumes/h flow velocity Take liquid colourless, then with mass concentration be 70% ethanol solution with 0.1~0.5 times of column volume/h flow velocity eluting by macroporous resin adsorption Vaccinium oxycoccus pigment, collect eluent, by eluent concentrating under reduced pressure in 50~55 DEG C of vacuum drying ovens, concentrated solution freezing is done Dry vaccinium oxycoccus pigment.
Example 1
First weigh 200g blue berry and clean roguing, add crushing and beating 10min in refiner with 200mL deionized water, by indigo plant It is in 40% ethanol solution that certain kind of berries serosity adds 2L mass concentration, under 50 DEG C of waters bath with thermostatic control, adds 30g cellulase, and uses 200W ultrasonic echography 10min, is 10% hydrochloric acid solution regulation pH to 2.0 by mass concentration, extracts 2h, inserted by lixiviating solution In 4000/min centrifuge, centrifugal 10min, must precipitate and supernatant, precipitation extracted once by aforesaid operations again and collect supernatant Liquid, merges supernatant, by supernatant at 50 DEG C, is evaporated to the 30% of original volume, obtains vaccinium oxycoccus pigment crude extract;Then The mass concentration added containing mass concentration is 0.1% hydrochloric acid by solid-liquid ratio 1:6 by above-mentioned vaccinium oxycoccus pigment crude extract is 60% ethanol In solution, with 7mL/min by high-pressure pulse electric, controlling umber of pulse is 8, and electric field intensity is 18KV/cm, and by mixed liquor Insert centrifugal 10min in 4000/min centrifuge, take supernatant, obtain vaccinium oxycoccus pigment two extract;Finally by above-mentioned blue berry cyanine Element two extracts through being filled with the adsorption column of macroporous resin, repeat aforesaid operations to extracting liquid colourless with 2 times of column volumes/h flow velocity, It is 70% ethanol solution with 0.1 times of column volume/h flow velocity eluting by the vaccinium oxycoccus pigment of macroporous resin adsorption by mass concentration again, receives Collection eluent, by eluent concentrating under reduced pressure in 50 DEG C of vacuum drying ovens, obtains vaccinium oxycoccus pigment by concentrated solution lyophilization.
This example operation is easy, and during use, by solid-to-liquid ratio 1: 50, the vaccinium oxycoccus pigment present invention prepared pours warm water into In, stir, oral, it is proposed that morning and evening every day one after each meal, take rear fasting seafood, maror, adhere to taking continuously With 7 days, can substantially feel the fine and smooth gloss that skin becomes, enhance the immunity of skin, for easy autopath, can be effective Resisting various allergic conditions, effect is the most notable.
Example 2
First weigh 250g blue berry and clean roguing, add crushing and beating 13min in refiner with 250mL deionized water, by indigo plant It is in 40% ethanol solution that certain kind of berries serosity adds 2.5L mass concentration, under 51 DEG C of waters bath with thermostatic control, adds 40g cellulase, and uses 200W ultrasonic echography 11min, is 10% hydrochloric acid solution regulation pH to 2.3 by mass concentration, extracts 2.5h, inserted by lixiviating solution In 5000/min centrifuge, centrifugal 13min, must precipitate and supernatant, precipitation extracted once by aforesaid operations again and collect supernatant Liquid, merges supernatant, by supernatant at 53 DEG C, is evaporated to the 33% of original volume, obtains vaccinium oxycoccus pigment crude extract;Then The mass concentration added containing mass concentration is 0.1% hydrochloric acid by solid-liquid ratio 1:65 by above-mentioned vaccinium oxycoccus pigment crude extract is 60% ethanol In solution, with 7.5mL/min by high-pressure pulse electric, controlling umber of pulse is 9, electric field intensity 18.5KV/cm, and will mixing Liquid inserts centrifugal 13min in 5000/min centrifuge, takes supernatant, obtains vaccinium oxycoccus pigment two extract;Finally by above-mentioned blue berry flower Blue or green plain two extracts with 3 times of column volumes/h flow velocity through being filled with the adsorption column of macroporous resin, repeat aforesaid operations to extracting solution without Color, then with mass concentration be 70% ethanol solution with 0.4 times of column volume/h flow velocity eluting by the blue berry cyanine of macroporous resin adsorption Element, collects eluent, by eluent concentrating under reduced pressure in 53 DEG C of vacuum drying ovens, concentrated solution lyophilization is obtained blue berry cyanine Element.
This example operation is easy, and during use, by solid-to-liquid ratio 1: 80, the vaccinium oxycoccus pigment present invention prepared pours warm water into In, stir, oral, it is proposed that morning and evening every day one after each meal, take rear fasting seafood, maror, adhere to taking continuously With 12 days, can substantially feel the fine and smooth gloss that skin becomes, enhance the immunity of skin, for easy autopath, Ke Yiyou Effect resists various allergic conditions, and effect is the most notable.
Example 3
First weigh 300g blue berry and clean roguing, add crushing and beating 15min in refiner with 300mL deionized water, by indigo plant It is in 40% ethanol solution that certain kind of berries serosity adds 3L mass concentration, under 52 DEG C of waters bath with thermostatic control, adds 45g cellulase, and uses 200W ultrasonic echography 12min, is 10% hydrochloric acid solution regulation pH to 2.5 by mass concentration, extracts 3h, inserted by lixiviating solution In 6000/min centrifuge, centrifugal 15min, must precipitate and supernatant, precipitation extracted once by aforesaid operations again and collect supernatant Liquid, merges supernatant, by supernatant at 55 DEG C, is evaporated to the 35% of original volume, obtains vaccinium oxycoccus pigment crude extract;Then The mass concentration added containing mass concentration is 0.1% hydrochloric acid by solid-liquid ratio 1:7 by above-mentioned vaccinium oxycoccus pigment crude extract is 60% ethanol In solution, with 8mL/min by high-pressure pulse electric, controlling umber of pulse is 10, and electric field intensity is 19KV/cm, and will mixing Liquid inserts centrifugal 15min in 6000/min centrifuge, takes supernatant, obtains vaccinium oxycoccus pigment two extract;Finally by above-mentioned blue berry flower Blue or green plain two extracts with 4 times of column volumes/h flow velocity through being filled with the adsorption column of macroporous resin, repeat aforesaid operations to extracting solution without Color, then with mass concentration be 70% ethanol solution with 0.5 times of column volume/h flow velocity eluting by the blue berry cyanine of macroporous resin adsorption Element, collects eluent, by eluent concentrating under reduced pressure in 55 DEG C of vacuum drying ovens, concentrated solution lyophilization is obtained blue berry cyanine Element.
This example operation is easy, and during use, by solid-to-liquid ratio 1: 100, the vaccinium oxycoccus pigment present invention prepared is poured temperature into and opened In water, stir, oral, it is proposed that morning and evening every day one after each meal, take rear fasting seafood, maror, adhere to continuously Take 14 days, can substantially feel the fine and smooth gloss that skin becomes, enhance the immunity of skin, for easy autopath, permissible Being effective against various allergic conditions, effect is the most notable.

Claims (1)

1. the extracting method of a vaccinium oxycoccus pigment, it is characterised in that concrete preparation process is:
(1) weigh 200~300g blue berry and clean roguing, add crushing and beating 10 in refiner with 200~300mL deionized waters ~15min, it is in 40% ethanol solution by blue berry serosity addition 2~3L mass concentrations, under 50~52 DEG C of waters bath with thermostatic control, adds 30~45g cellulase, and with 200W ultrasonic echography 10~12min, be that 10% hydrochloric acid solution regulates pH extremely by mass concentration 2.0~2.5, extract 2~3h, lixiviating solution inserted in 4000~6000/min centrifuges centrifugal 10~15min, must precipitate and on Clear liquid, is extracted once by precipitation by aforesaid operations and is collected supernatant again, merges supernatant, by supernatant at 50~55 DEG C, It is evaporated to the 30~35% of original volume, obtains vaccinium oxycoccus pigment crude extract;
(2) quality added containing mass concentration is 0.1% hydrochloric acid by solid-liquid ratio 1:6~1:7 by above-mentioned vaccinium oxycoccus pigment crude extract is dense Degree is in 60% ethanol solution, and with 7~8mL/min by high-pressure pulse electric, controlling umber of pulse is 8~10, and electric field intensity is 18~19KV/cm, and mixed liquor is inserted in 4000~6000/min centrifuges centrifugal 10~15min, take supernatant, obtain blue berry Anthocyanidin two extract;
(3) above-mentioned vaccinium oxycoccus pigment two extract is filled with 2~4 times of column volumes/h flow velocity process the adsorption column of macroporous resin, Repetition aforesaid operations is to extracting liquid colourless, then is that 70% ethanol solution is washed with 0.1~0.5 times of column volume/h flow velocity by mass concentration De-by the vaccinium oxycoccus pigment of macroporous resin adsorption, collect eluent, eluent is reduced pressure dense in 50~55 DEG C of vacuum drying ovens Contracting, obtains vaccinium oxycoccus pigment by concentrated solution lyophilization.
CN201610441777.0A 2016-06-20 2016-06-20 A kind of extracting method of vaccinium oxycoccus pigment Pending CN106083796A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107411088A (en) * 2017-06-20 2017-12-01 哈尔滨工业大学 Special blueberry anthocyanin complex tablet of a kind of the elderly and preparation method thereof
CN108576142A (en) * 2018-05-21 2018-09-28 遵义盛林农业发展有限公司 A kind of production method of blueberry biscuit
CN108719395A (en) * 2018-05-21 2018-11-02 遵义盛林农业发展有限公司 A kind of production method for blueberry biscuit
CN108991197A (en) * 2018-07-27 2018-12-14 贵州省普定县黔龙茶业有限公司 A kind of processing method rich in anthocyanidin instant tea
CN109293618A (en) * 2018-11-30 2019-02-01 黑龙江绿知都生物科技开发有限公司 A kind of blueberry anthocyanin isolation and purification method
CN109553599A (en) * 2019-01-17 2019-04-02 江苏省农业科学院 A kind of blueberry anthocyanin and its preparation method and application
CN109793236A (en) * 2019-04-03 2019-05-24 海南松吉云商科技有限公司 A kind of preparation method of Noni extract
CN111418742A (en) * 2020-05-28 2020-07-17 山西纳安生物科技股份有限公司 Preparation method of wild cherry juice
CN112042846A (en) * 2020-09-16 2020-12-08 深圳鼎盛和兴科技有限公司 Sea-buckthorn solid beverage for enhancing immunity and inhibiting tumors and preparation method thereof
CN115381012A (en) * 2022-09-07 2022-11-25 黑龙江敬众堂生物科技有限公司 Preparation method of beverage rich in purple corn anthocyanin

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CN103435588A (en) * 2013-09-12 2013-12-11 南京泽朗农业发展有限公司 Novel method for preparing blueberry anthocyanidin
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CN103435588A (en) * 2013-09-12 2013-12-11 南京泽朗农业发展有限公司 Novel method for preparing blueberry anthocyanidin
CN105175380A (en) * 2015-08-14 2015-12-23 北京中农弘科生物技术有限公司 Method for preparing Yunnan pine bark procyanidine

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107411088A (en) * 2017-06-20 2017-12-01 哈尔滨工业大学 Special blueberry anthocyanin complex tablet of a kind of the elderly and preparation method thereof
CN108576142A (en) * 2018-05-21 2018-09-28 遵义盛林农业发展有限公司 A kind of production method of blueberry biscuit
CN108719395A (en) * 2018-05-21 2018-11-02 遵义盛林农业发展有限公司 A kind of production method for blueberry biscuit
CN108991197A (en) * 2018-07-27 2018-12-14 贵州省普定县黔龙茶业有限公司 A kind of processing method rich in anthocyanidin instant tea
CN109293618B (en) * 2018-11-30 2022-06-17 黑龙江绿知都生物科技开发有限公司 Blueberry anthocyanin separation and purification method
CN109293618A (en) * 2018-11-30 2019-02-01 黑龙江绿知都生物科技开发有限公司 A kind of blueberry anthocyanin isolation and purification method
CN109553599A (en) * 2019-01-17 2019-04-02 江苏省农业科学院 A kind of blueberry anthocyanin and its preparation method and application
CN109793236A (en) * 2019-04-03 2019-05-24 海南松吉云商科技有限公司 A kind of preparation method of Noni extract
CN109793236B (en) * 2019-04-03 2022-04-08 海南松吉云商科技有限公司 Preparation method of noni extract
CN111418742A (en) * 2020-05-28 2020-07-17 山西纳安生物科技股份有限公司 Preparation method of wild cherry juice
CN112042846A (en) * 2020-09-16 2020-12-08 深圳鼎盛和兴科技有限公司 Sea-buckthorn solid beverage for enhancing immunity and inhibiting tumors and preparation method thereof
CN115381012A (en) * 2022-09-07 2022-11-25 黑龙江敬众堂生物科技有限公司 Preparation method of beverage rich in purple corn anthocyanin
CN115381012B (en) * 2022-09-07 2024-02-09 黑龙江敬众堂生物科技有限公司 Preparation method of beverage rich in purple corn anthocyanin

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