CN105707658A - Preparation method of radix glycyrrhizae sweetening agent for removing bitter taste - Google Patents
Preparation method of radix glycyrrhizae sweetening agent for removing bitter taste Download PDFInfo
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- CN105707658A CN105707658A CN201610100583.4A CN201610100583A CN105707658A CN 105707658 A CN105707658 A CN 105707658A CN 201610100583 A CN201610100583 A CN 201610100583A CN 105707658 A CN105707658 A CN 105707658A
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- radix glycyrrhizae
- preparation
- adsorbent resin
- sweeting agent
- macroporous adsorbent
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- 235000019658 bitter taste Nutrition 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 235000003599 food sweetener Nutrition 0.000 title abstract 4
- 239000003765 sweetening agent Substances 0.000 title abstract 4
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 claims abstract description 38
- 239000011347 resin Substances 0.000 claims abstract description 36
- 229920005989 resin Polymers 0.000 claims abstract description 36
- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229960004949 glycyrrhizic acid Drugs 0.000 claims abstract description 35
- UYRUBYNTXSDKQT-UHFFFAOYSA-N glycyrrhizic acid Natural products CC1(C)C(CCC2(C)C1CCC3(C)C2C(=O)C=C4C5CC(C)(CCC5(C)CCC34C)C(=O)O)OC6OC(C(O)C(O)C6OC7OC(O)C(O)C(O)C7C(=O)O)C(=O)O UYRUBYNTXSDKQT-UHFFFAOYSA-N 0.000 claims abstract description 35
- 235000019410 glycyrrhizin Nutrition 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- VTAJIXDZFCRWBR-UHFFFAOYSA-N Licoricesaponin B2 Natural products C1C(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2)C(O)=O)C)(C)CC2)(C)C2C(C)(C)CC1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O VTAJIXDZFCRWBR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001685 glycyrrhizic acid Substances 0.000 claims abstract description 18
- 239000012153 distilled water Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000003672 processing method Methods 0.000 claims abstract description 5
- 238000001694 spray drying Methods 0.000 claims abstract description 4
- 239000003463 adsorbent Substances 0.000 claims description 24
- 239000003795 chemical substances by application Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000004378 Glycyrrhizin Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 15
- 238000011010 flushing procedure Methods 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- -1 flavonoids compounds Chemical class 0.000 abstract description 6
- 229930003935 flavonoid Natural products 0.000 abstract description 4
- 235000017173 flavonoids Nutrition 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 4
- 239000003814 drug Substances 0.000 abstract description 3
- 229940079593 drug Drugs 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract description 2
- 229940074774 glycyrrhizinate Drugs 0.000 abstract 3
- 239000008213 purified water Substances 0.000 abstract 2
- 238000001179 sorption measurement Methods 0.000 abstract 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 4
- 239000000796 flavoring agent Substances 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 235000019605 sweet taste sensations Nutrition 0.000 description 4
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 description 3
- 244000303040 Glycyrrhiza glabra Species 0.000 description 3
- 230000001476 alcoholic effect Effects 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 235000011477 liquorice Nutrition 0.000 description 3
- 235000013555 soy sauce Nutrition 0.000 description 3
- 239000002156 adsorbate Substances 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 235000013373 food additive Nutrition 0.000 description 2
- 239000002778 food additive Substances 0.000 description 2
- 238000009418 renovation Methods 0.000 description 2
- 101100313763 Arabidopsis thaliana TIM22-2 gene Proteins 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 208000008589 Obesity Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 235000015218 chewing gum Nutrition 0.000 description 1
- 229940112822 chewing gum Drugs 0.000 description 1
- 235000019219 chocolate Nutrition 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 235000020824 obesity Nutrition 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 235000021110 pickles Nutrition 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Seasonings (AREA)
- Medicinal Preparation (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention provides a preparation method of a radix glycyrrhizae sweetening agent for removing bitter taste. According to the method, glycyrrhizinate R-21 serves as the raw material and is dissolved with purified water or distilled water, a dissolved solution slowly passes through macroreticular resin, then the adsorption resin is eluted with purified water or distilled water, then flowing out liquid is combined, concentration and spray drying are conducted, and the radix glycyrrhizae sweetening agent for removing bitter taste is obtained. By means of the method that adsorption is conducted through the macroreticular resin, part of analogue of glycyrrhizic acid in the glycyrrhizinate R-21, part of radix glycyrrhizae flavonoids compounds and other irrelevant ingredients are removed, meanwhile the content of glycyrrhizic acid in a glycyrrhizinate product is raised, and other items meet the national drug standard WS-10001-(HD-0504)-2002. The radix glycyrrhizae sweetening agent is free of bitter taste, high in sweetness and pure in mouthfeel, and the preparation method is an environmentally friendly processing method.
Description
Technical field
The invention belongs to technical field of food additives, be specifically related to the preparation method of a kind of Radix Glycyrrhizae sweeting agent removing bitterness in food additive.
Background technology
Radix Glycyrrhizae is the conventional Chinese medicine of integration of edible and medicinal herbs, and main effective ingredient is glycyrrhizic acid.Chinese patent ZL201010179453.7 discloses production glycyrrhizin sodium salt or the method for potassium salt, wherein glycyrrhizin sodium salt i.e. glycyrrhizin gourmet powder R-21.Glycyrrhizin gourmet powder R-21 is a kind of pure natural sweeting agent and flavor potentiator;There is strong Radix Glycyrrhizae peat-reek;Have that sugariness is high, heat energy is low, safety non-toxic and stronger medicinal health care function;It is hypertension, obesity, the most preferable sweeting agent of diabetics use;It is widely used in the field such as food, feedstuff.Glycyrrhizin gourmet powder is widely used at food service industry such as pickles, preserved fruit, soy sauce, oils and fats etc..It is frequently as tame and docile salt, correctives, such as: 1. in beer and beverages, can overcome that multiplex sugar causes turn sour, the sweet feature such as greasy;2. confection, chocolate and chewing gum have sterilization, cleans the teeth, antiinflammatory, wet one's whistle;3., in soy sauce, the local flavor of soy sauce can be increased, play sweetened, go, optimize effect of product;4. pair flavoring agent also have potentiation, anti-corruption to go mouldy, the effect such as colouring;5. pair oil and fat product has antioxidative effect;6. for curing food, there is the sweetened and effect of taste, for preserved fruit, there is acid adjustment effect etc..
In the ordinary course of things, R-21 such glycyrrhizin gourmet powder disclosure satisfy that the needs of food service industry substantially, but because of the relatively low (< 15.0% of glycyrrhizic acid content, HPLC), containing a large amount of glycyrrhizic acid analog and liquorice flavonoids compound, slightly bitterness, the few fashion of usage amount can simultaneously;When but addition increases, just there is sugariness relatively low, there is bitterness, the deficiencies such as mouthfeel difference, in order to remove bitterness, adapt to mouthfeel requirement, expand its purposes, adapt to people to sweet taste and the requirements at the higher level of local flavor, it is necessary the process that general glycyrrhizin gourmet powder series products is carried out removes bitterness, improves mouthfeel, meet market demand.
Summary of the invention
The present invention provides the preparation method of a kind of Radix Glycyrrhizae sweeting agent removing bitterness, and the product that the method obtains is a kind of without bitterness, and sugariness is high, and the Radix Glycyrrhizae sweeting agent of pure in mouth feel improves the glycyrrhizic acid content in this Radix Glycyrrhizae sweeting agent simultaneously.
For achieving the above object, the technical scheme that the present invention takes is:
A kind of preparation method removing bitterness Radix Glycyrrhizae sweeting agent, with glycyrrhizin gourmet powder R-21 as raw material, dissolved with pure water or distilled water, the solution dissolved is slow transitted through macroporous adsorbent resin, then with pure water or distilled water eluting adsorbent resin, it is then combined with effluent, concentrates, be spray-dried, i.e. obtain bitterness Radix Glycyrrhizae sweeting agent.It specifically comprises the following steps that
The glycyrrhizin gourmet powder R-21 of glycyrrhizic acid content 13%~16% is dissolved in pure water or the distilled water of raw material 4~15 times of weight so that it is be slowly added in the chromatographic column of processed good macroporous adsorbent resin, coutroi velocity 100 ~ 180ml/ minute;Continue with the pure water of raw material 15~20 times of weight or distilled water eluting, coutroi velocity 180~300ml/ minute, to effluent colourless, collect effluent;By effluent concentrating under reduced pressure, being spray-dried, obtain glycyrrhizic acid content >=30% removes bitterness Radix Glycyrrhizae sweeting agent.
Further:
The method of described spray drying is: spray tower temperature is 85~90 DEG C, inlet temperature: 145~158 DEG C, leaving air temp: 80~85 DEG C, charging rate: 300~400ml/ minute.
Processing method after described macroporous adsorbent resin uses is: with 75%~95% alcohol flushing chromatographic column of the 2~5 of this macroporous adsorbent resin times of volumes, the material of parsing absorption with macroporous adsorbent resin, to flushing liquor colourless;Then re-using 1~10% alkaline ethanol solution of 2~5 times of volumes of described macroporous adsorbent resin, wherein the concentration of ethanol is 75%~95%, rinse chromatographic column to flushing liquor colourless;Again with pure water or the distilled water flushing resin column of 2~3 times of volumes of described macroporous adsorbent resin, until recycling during effluent pH value 6~7.
Alkali in described 1 ~ 10% alkaline ethanol solution is sodium hydroxide or potassium hydroxide.
Described macroporous adsorbent resin is low pole resin, including HP-20, AB-8, D101, X-5, HPD-100, DM130 or CAD-40.
Because bitter principle is probably part analog and the part liquorice flavonoids compound of glycyrrhizic acid in general glycyrrhizin gourmet powder.The present invention is the way using absorption with macroporous adsorbent resin, remove the analog of part glycyrrhizic acid in glycyrrhizin gourmet powder R-21 and part liquorice flavonoids compound and some other unrelated composition, improve the glycyrrhizic acid content in glycyrrhizin gourmet powder goods simultaneously, reach to prepare one without bitterness, sugariness is high, the Radix Glycyrrhizae sweeting agent of pure in mouth feel, is a kind of green processing method.
Products obtained therefrom of the present invention goes bitterness Radix Glycyrrhizae sweeting agent in addition to glycyrrhizic acid content is higher than standard, and sundry item all meets national drug standards WS-10001-(HD-0504)-2002.
Detailed description of the invention:
Embodiment 1
1. by glycyrrhizin gourmet powder R-21(glycyrrhizic acid content 13% HPLC of 3.00Kg) it is dissolved in 30Kg pure water, make it be slowly added into locate (post height 100cm in the chromatographic column of measured HP20 macroporous adsorbent resin, diameter 25cm), coutroi velocity 100 ~ 180ml/ minute or 150 ~ 160ml/ minute so that it is adsorb completely;Continue with 53Kg pure water eluting, coutroi velocity 180 ~ 300ml/ minute or 200 ~ 220ml/ minute, collect effluent to without sweet taste, and by this collection liquid concentrating under reduced pressure, it is spray-dried, obtains 1.25Kg and remove the Radix Glycyrrhizae sweeting agent of bitterness, glycyrrhizic acid content >=30% (HPLC).
2. the ethanol of macroporous resin this macroporous resin 2,3,4 or 5 times the 75% of volume, 80%, 85%, 90% or 95% after using rinses chromatographic column with the speed of 200ml/ minute, the material of parsing resin absorption to flushing liquor is colourless.Then re-use macroporous resin 2,3,4 or 5 times the 1% of volume, 2% or 10% alkali alcoholic solution with the speed of 300ml/ minute rinse chromatographic column to flushing liquor colourless, 1%, the alkali in 2% or 10% alkali alcoholic solution is sodium hydroxide or potassium hydroxide, 1%, the alcohol in 2% or 10% alkali alcoholic solution is ethanol, and its concentration is 75%, 80%, 85%, 90% or 95%;Rinsing chromatographic column with macroporous resin 2 or the pure water of 3 times of volumes or distilled water with the speed of 500ml/ minute again, until can recycle during effluent pH value 6~7, this processing method makes the reusable frequency of resin be up to 50 ~ 80 times.
Embodiment 2
1. by glycyrrhizin gourmet powder R-21(glycyrrhizic acid content 13% HPLC of 3.00Kg) it is dissolved in 45Kg pure water, make it be slowly added into locate (post height 100cm in the chromatographic column of measured AB-8 macroporous adsorbent resin, diameter 25cm), coutroi velocity 100 ~ 180ml/ minute or 160 ~ 170ml/ minute so that it is adsorb completely;Continuing to use 58Kg pure water eluting adsorbate, coutroi velocity 180 ~ 300ml/ minute or 210 ~ 220ml/ minute, collection effluent, to without sweet taste, will be collected liquid concentrating under reduced pressure, be spray-dried.1.22Kg can be obtained and remove the Radix Glycyrrhizae sweeting agent of bitterness, glycyrrhizic acid content >=30% (HPLC).
Macroporous adsorbent resin renovation process after above-mentioned use is with embodiment 1.
Embodiment 3
1. by glycyrrhizin gourmet powder R-21(glycyrrhizic acid content 13% HPLC of 3.00Kg) it is dissolved in 12Kg distilled water, make it be slowly added into locate (post height 100cm in the chromatographic column of measured D101 macroporous adsorbent resin, diameter 25cm), coutroi velocity 100 ~ 180ml/ minute or 170 ~ 180ml/ minute so that it is adsorb completely;Continuing to use 60Kg distilled water eluting adsorbate, coutroi velocity 180 ~ 300ml/ minute or 220 ~ 230ml/ minute, collection effluent is to without sweet taste, and will collect liquid concentrating under reduced pressure, is spray-dried.1.16Kg can be obtained and remove the Radix Glycyrrhizae sweeting agent of bitterness, glycyrrhizic acid content >=30% (HPLC).
Macroporous adsorbent resin renovation process after above-mentioned use is with embodiment 1.
The method of the spray drying in embodiment 1,2,3 is: spray tower temperature is 85 ~ 90 DEG C, inlet temperature: 145 ~ 158 DEG C, leaving air temp: 80 ~ 85 DEG C, charging rate: 300 ~ 400ml/ minute.
Claims (6)
1. the preparation method removing bitterness Radix Glycyrrhizae sweeting agent, it is characterized in that: with glycyrrhizin gourmet powder R-21 as raw material, dissolved with pure water or distilled water, the solution dissolved is slow transitted through macroporous adsorbent resin, then with pure water or distilled water eluting adsorbent resin, it is then combined with effluent, concentrates, be spray-dried, i.e. obtain bitterness Radix Glycyrrhizae sweeting agent.
A kind of preparation method removing bitterness Radix Glycyrrhizae sweeting agent the most according to claim 1, it is characterised in that: this preparation method particularly as follows:
The glycyrrhizin gourmet powder R-21 of glycyrrhizic acid content 13%~16% is dissolved in pure water or the distilled water of raw material 4~15 times of weight so that it is be slowly added in the chromatographic column of processed good macroporous adsorbent resin, coutroi velocity 100 ~ 180ml/ minute;Continue with the pure water of raw material 15~20 times of weight or distilled water eluting, coutroi velocity 180~300ml/ minute, to effluent colourless, collect effluent;By effluent concentrating under reduced pressure, being spray-dried, obtain glycyrrhizic acid content >=30% removes bitterness Radix Glycyrrhizae sweeting agent.
A kind of preparation method removing bitterness Radix Glycyrrhizae sweeting agent the most according to claim 1 and 2, it is characterized in that: the method for described spray drying is: spray tower temperature is 85 ~ 90 DEG C, inlet temperature: 145 ~ 158 DEG C, leaving air temp: 80 ~ 85 DEG C, charging rate: 300 ~ 400ml/ minute.
A kind of preparation method removing bitterness Radix Glycyrrhizae sweeting agent the most according to claim 1, it is characterized in that: the processing method after described macroporous adsorbent resin uses is: with 75% ~ 95% alcohol flushing chromatographic column of the 2 ~ 5 of this macroporous adsorbent resin times of volumes, resolve absorption with macroporous adsorbent resin material, to flushing liquor colourless;Then re-using 1 ~ 10% alkaline ethanol solution of 2 ~ 5 times of volumes of described macroporous adsorbent resin, wherein the concentration of ethanol is 75 ~ 95%, flushing chromatographic column to flushing liquor is colourless;Again with pure water or the distilled water flushing chromatographic column of 2 ~ 3 times of volumes of described macroporous adsorbent resin, until recycling during effluent pH value 6 ~ 7.
A kind of preparation method removing bitterness Radix Glycyrrhizae sweeting agent the most according to claim 4, it is characterised in that: the alkali in described 1 ~ 10% alkaline ethanol solution is sodium hydroxide or potassium hydroxide.
6. according to a kind of preparation method removing bitterness Radix Glycyrrhizae sweeting agent according to any one of claim 1,2 or 4, it is characterised in that: described macroporous adsorbent resin is low pole resin, including HP-20, AB-8, D101, X-5, HPD-100, DM130 or CAD-40.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107751947A (en) * | 2017-08-24 | 2018-03-06 | 兰溪市捷喜食品加工技术有限公司 | Sweetener for candy and preparation method thereof |
CN107950845A (en) * | 2017-11-16 | 2018-04-24 | 湖北瀚思生物科技有限公司 | Honeysuckle functional beverage and its production method |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1036960A (en) * | 1988-04-14 | 1989-11-08 | 中国人民解放军空军总医院 | The separation and refining method of Potenlini |
CN1210865A (en) * | 1997-09-11 | 1999-03-17 | 中国科学院新疆化学研究所 | Refining method of glycyrrhizin |
CN103833805A (en) * | 2012-11-27 | 2014-06-04 | 杨超 | Process for refining glycyrrhizinic acid in liquorice |
-
2016
- 2016-02-24 CN CN201610100583.4A patent/CN105707658A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1036960A (en) * | 1988-04-14 | 1989-11-08 | 中国人民解放军空军总医院 | The separation and refining method of Potenlini |
CN1210865A (en) * | 1997-09-11 | 1999-03-17 | 中国科学院新疆化学研究所 | Refining method of glycyrrhizin |
CN103833805A (en) * | 2012-11-27 | 2014-06-04 | 杨超 | Process for refining glycyrrhizinic acid in liquorice |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107751947A (en) * | 2017-08-24 | 2018-03-06 | 兰溪市捷喜食品加工技术有限公司 | Sweetener for candy and preparation method thereof |
CN107950845A (en) * | 2017-11-16 | 2018-04-24 | 湖北瀚思生物科技有限公司 | Honeysuckle functional beverage and its production method |
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