CN105326055B - A kind of plum halogen essence functional food rich in aldehydes matter and organic acid and preparation method thereof - Google Patents

A kind of plum halogen essence functional food rich in aldehydes matter and organic acid and preparation method thereof Download PDF

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CN105326055B
CN105326055B CN201510821422.XA CN201510821422A CN105326055B CN 105326055 B CN105326055 B CN 105326055B CN 201510821422 A CN201510821422 A CN 201510821422A CN 105326055 B CN105326055 B CN 105326055B
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organic acid
aldehydes matter
acid
plum halogen
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CN105326055A (en
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刘学铭
程镜蓉
陈智毅
林耀盛
杨春英
张友胜
张业辉
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Puning Xiaomeiwu Food Co ltd
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Sericulture and Agri Food Research Institute GAAS
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Abstract

The invention discloses a kind of preparation method of the plum halogen essence functional food rich in aldehydes matter and organic acid, the plum halogen produced in process is pickled using green plum as raw material, separate and recover Phenolic components therein and organic acid composition, the invention also discloses a kind of plum halogen essence functional food rich in aldehydes matter and organic acid, including the extract made from the above method rich in aldehydes matter and the extract rich in organic acid, wherein the weight/mass percentage composition of the extract rich in aldehydes matter is 5%~30%, the weight/mass percentage composition of extract rich in organic acid is 70%~95%.The inventive method can effectively utilize plum halogen resource, and energy-conserving and environment-protective are high using added value of product produced by the present invention.

Description

It is a kind of to be rich in aldehydes matter and the plum halogen essence functional food of organic acid and its preparation Method
Technical field
The invention belongs to technical field of functional food, and in particular to a kind of plum halogen elite rich in aldehydes matter and organic acid Plain functional food and preparation method thereof.
Background technology
Green plum (Prunus mume Sieb.et Zucc.) is also known as smoked plum, fruit plum, is the fruit that rose family apricot belongs to arbor It is real, the Yangtze river basin and south China, the band of southwest one are distributed mainly on, is saved with Guangdong, Guangxi, Yunnan, Fujian, Zhejiang, Jiangsu etc. Yield it is more.Recent study shows that green plum has anti-oxidant, anti-inflammatory, antibacterial, hypoglycemic, reducing blood lipid, anti-trioxypurine, fat-reducing With regulation gastrointestinal function isoreactivity, with wide exploitation prospect.Green plum as a kind of fruit of medicine-food two-purpose, due to Acidity is too high and should not eat raw, is a kind of typical processing type fruit.For a long time, in addition to being fabricated to Chinese medicine dark plum except part, Green plum is mainly used in the processing of preserved fruit, is first pickled after fruit picking with salt, and plum base is made, and following process is then carried out again.
During green plum pickles production plum base, 250~300kg salt is added per 1000kg green plums fresh fruit, is produced 400kg or so salt marsh liquid, this salt marsh liquid is plum halogen.Because current green plum is all mainly that the production such as preserved fruit is reprocessed into after pickling Product, by the 400000 tons of calculating of China's green plum yield, about produce 160,000 tons of plum halogen.In China's green plum secondary industry, plum halogen does not originally have It is utilized, the overwhelming majority is directly discharged into environment, both wastes resource, environment is polluted again.
According to analysis, 120,000mg/ are up to containing 15%~20% or so salt, its COD (COD) in plum halogen (the yellow moral people report the COD of plum halogen to L (Kubo etc., 2001)CrFor 10,000mg/L), pH is less than 2.5, if directly into environment Discharge, is typical high salt, peracid, high-COD waste water.Because plum halogen contains substantial amounts of salt and organic acid, to environmental ecology system The destructive power of system is larger, makes local environment salinization and acidifying, breaks the local ecological balance.Protection can be played by developing plum halogen The effect of environment.
The mixture of plum halogen actually fruit plum juice and salt, than water, mainly contain leached from fruit plum organic acid, The nutrition such as carbohydrate, phenols and bioactive substance, are valuable resources generally without noxious material.Develop plum Halogen can play the purpose economized on resources.
There is presently no the report that essence functional food is processed using plum halogen.Patent 200710033012.4 discloses one The preparation method of plum halogen beverage is planted, plum halogen obtains a kind of plum halogen health beverage through techniques such as filtering, concentrating and desalinating, clarification, refined filtration, allotments Material;Patent 201010227224.8 discloses a kind of method of producing plum juice via plum halogen desalination, and plum halogen is used after normal pressure distillation and concentration Edible alcohol extracts desalination, then recovered alcohol, and the liquid obtained when concentrate is with distillation is mixed, so as to obtain desalination plum juice. This two patents are required for carrying out concentration, and the bioactive substance not only contained in high energy consumption, and obtained product contains Amount is low, therefore, develops in a kind of low energy consumption, product the high plum halogen essence functional food production technology of bioactivity content very It is necessary.
The content of the invention
First technical problem to be solved by this invention is to provide a kind of rich plum halogen essence containing aldehydes matter and organic acid The preparation method of magnificent element functional food, the preparation method energy consumption and cost are low, environment-friendly, and the plum halogen essence function of obtaining Aldehydes matter and organic acid content are high in food.
Second technical problem to be solved by this invention is to provide a kind of plum halogen essence rich in aldehydes matter and organic acid Magnificent element functional food, the functional food, which is used, includes the obtained extract for being rich in aldehydes matter of above-mentioned preparation method and rich in having The extract of machine acid is as active component, and the functional food is rich in aldehydes matter and organic acid, and added value of product is high.
First technical problem to be solved by this invention is achieved through the following technical solutions:One kind is rich in phenols The preparation method of the plum halogen essence functional food of material and organic acid, comprises the following steps:
(1) take filtrate to centrifuge after taking plum halogen, filtering, obtain clarifying plum halogen, clarification plum halogen is added to macroporous absorbent resin In post, collection omission timber 1 is standby, aldehydes matter in detection omission timber 1, and being positive, it is full to show that large pore resin absorption column has been adsorbed With stopping addition plum halogen;
(2) large pore resin absorption column is rinsed to eluate water white transparency with pure water, eluted using acid alcohol solvent big Macroporous adsorbent resin post, collects eluent and is concentrated to give the extract rich in aldehydes matter;
(3) omission timber 1 in step (1) is taken, is added in anion-exchange resin column, omission timber 2 is collected, detection is spilt Organic acid in liquid 2, is presented the positive and shows anion-exchange resin column adsorption saturation, stops adding omission timber 1;
(4) anion-exchange resin column is rinsed to eluate water white transparency with pure water, eluted using alcohols solvent, collect Eluent is concentrated to give the extract rich in organic acid.
In the preparation method of the above-mentioned plum halogen essence functional food rich in aldehydes matter and organic acid:
The aperture of filter cloth is preferably 80~300 mesh when being filtered in step (1), and the rotating speed of centrifuge is preferably 4000 during centrifugation ~10000 revs/min.
Large pore resin absorption column described in step (1) is preferably X-5 macroporous absorbent resins or AB-8 macroporous absorbent resins.
It is preferred to use aldehydes matter in forint- phenol law detection omission timber 1 in step (1).
Acid alcohol solvent described in step (2) is the alcohol solution containing acid, wherein described acid be hydrochloric acid or Formic acid, described alcohol solution is methanol aqueous solution or ethanol water, and the volumn concentration of wherein methanol or ethanol is 30~95%, the volumn concentration of hydrochloric acid or formic acid is 0.08~0.12%.
Total phenol content is not less than 20.0%, weight ratio, not have in the extract rich in aldehydes matter described in step (2) Gallate-based meter.
Through high performance liquid chromatography detection, the extract of the present invention rich in aldehydes matter is mainly containing neochlorogenic acid, green The phenolic acids such as ortho acid, Cryptochlorogenic acid and p-Coumaric Acid.
Anion-exchange resin column described in step (3) be preferably 717 type anion exchange resin or D301G types it is cloudy from Sub-exchange resin.
The organic acid being preferred to use in step (3) in pH meter or acid-base titration detection omission timber 2 is positive.
Alcohols solvent described in step (4) is methanol aqueous solution or ethanol water, its volumn concentration 30~ 80%;Total acid content is not less than 30%, weight ratio, with citrometer in the extract rich in organic acid described in step (4).
Through high performance liquid chromatography detection, the extract of the present invention rich in organic acid mainly contains citric acid and apple Acid.
Second technical problem to be solved by this invention is achieved through the following technical solutions:One kind is rich in phenols The plum halogen essence functional food of material and organic acid, including using the extract made from the above method rich in aldehydes matter and Extract rich in organic acid, wherein the weight/mass percentage composition of the extract rich in aldehydes matter is 5%~30%, rich in organic The weight/mass percentage composition of the extract of acid is 70%~95%.
I.e. the present invention pickles the plum halogen produced in process using green plum as raw material, separates and recovers phenolic material therein Matter component and organic acid composition, (the auxiliary of this area routine can be also added as needed on after two kinds of components are mixed by a certain percentage Material), formulation described in energy bromatology is successfully prepared according to a conventional method, is produced of the present invention rich in aldehydes matter and organic The plum halogen essence functional food of acid.
Compared with prior art, the invention has the advantages that:
(1) cost is low:The accessory substance plum halogen that current green plum pickles processing is abandoned as discarded object, is not used also, this Invention greatly reduces production cost using plum halogen as raw material, improves the utilization rate of resource, in addition, prepared by product of the present invention During the solvent that uses it is recovered, reusable edible;
(2) it is environment-friendly:The accessory substance plum halogen that the present invention pickles processing to green plum has carried out deep processing, turns waste into wealth, subtracts Lack the discharge to environmentally hazardous substance, it is environment-friendly, eluting solvent is recycled in whole production process, is not brought to environment New pollution;
(3) added value of product is high:The food of the plum halogen essence function rich in aldehydes matter and organic acid developed using plum halogen Product have the function such as anti-oxidant, antibacterial, reducing blood lipid, anti-trioxypurine, aid digestion, have than broader market prospects, and that brings is additional Value is higher.
Brief description of the drawings
Fig. 1 is the system of the plum halogen essence functional food rich in aldehydes matter and organic acid in 1-4 of the embodiment of the present invention The flow chart of Preparation Method.
Embodiment
Following examples are used merely to explain the present invention, are not intended to limit protection scope of the present invention.The art it is common The purpose of the present invention can be achieved according to scope disclosed above in technical staff.
Embodiment 1
As shown in fig. 1, the plum halogen essence functional food rich in aldehydes matter and organic acid that the present embodiment is provided Preparation method, comprises the following steps:
(1) plum halogen 100L is taken, 100 mesh nylon filtering cloths filtering, 10000 revs/min of centrifugations obtain clarification plum halogen and (wherein filtered Liquid dilution discharge reclaims sodium chloride);Will clarification plum halogen be pumped into by pretreatment (preprocess method is carried by production of resins company For mainly high concentration ethanol immersion, sodium hydroxide solution and watery hydrochloric acid is rinsed etc.) X-5 macroporous absorbent resins, collection spills Liquid 1 is standby, and detects the aldehydes matter in omission timber 1, and aldehydes matter in omission timber 1 is detected using forint- phenol law, is presented positive Stop adding plum halogen during reaction;
(2) rinse resin column to flushing liquor with pure water to clarify, with 80% containing 0.1% hydrochloric acid (volumn concentration) (volumn concentration) ethanol water is eluted, and collects eluent, and concentration and recovery ethanol obtains the extraction rich in aldehydes matter Thing, the total phenol content of the obtained extract rich in aldehydes matter is not less than 20.0%, weight ratio, in terms of gallic acid;
Through high performance liquid chromatography detection, the extract of the present invention rich in aldehydes matter is mainly containing neochlorogenic acid, green The phenolic acids such as ortho acid, Cryptochlorogenic acid and p-Coumaric Acid.
(3) omission timber 1 by X-5 macroporous absorbent resin absorbing phenolic materials is pumped into and (given birth to by pretreatment by resin Production company is provided, and mainly high concentration ethanol immersion, sodium hydroxide solution and watery hydrochloric acid is rinsed etc.) 717 anion exchange trees Fat, collects the organic acid in omission timber 2, detection omission timber 2, stops being pumped into when positive reaction is presented;
(4) rinse 717 anion-exchange resin columns to flushing liquor with pure water to clarify, be 30% with volumn concentration Ethanol water is eluted, and collects eluent, concentration and recovery ethanol is obtained rich in extracts such as organic acids, obtained rich in organic Total acid content is not less than 30%, weight ratio, with citrometer in the extract of acid;
Through high performance liquid chromatography detection, the extract of the present invention rich in organic acid mainly contains citric acid and apple Acid.
Active component system is used as using the extract obtained above rich in aldehydes matter and the extract rich in organic acid Into the plum halogen essence functional food rich in aldehydes matter and organic acid, wherein the quality hundred of the extract rich in aldehydes matter It is 5% to divide content, and the weight/mass percentage composition of the extract rich in organic acid is 95%.
Preparation process is:Two kinds of extracts are freeze-dried, respective powder is obtained, by the extraction rich in aldehydes matter The weight/mass percentage composition of thing is 5%, and the weight/mass percentage composition of the extract rich in organic acid is 95% mixing, loads capsule, i.e., The plum halogen essence functional food of aldehydes matter and organic acid must be rich in.
Embodiment 2
As shown in fig. 1, the plum halogen essence functional food rich in aldehydes matter and organic acid that the present embodiment is provided Preparation method, comprises the following steps:
(1) plum halogen 100L is taken, 300 mesh nylon filtering cloths filtering, 8000 revs/min of centrifugations obtain clarifying plum halogen;Plum halogen will be clarified The AB-8 macroporous absorbent resins by pretreatment are pumped into, collection omission timber 1 is standby, and detects the aldehydes matter in omission timber 1, is in Stop adding plum halogen during existing positive reaction;
(2) rinse resin column to flushing liquor with pure water to clarify, with 50% containing 0.1% hydrochloric acid (volumn concentration) (volumn concentration) ethanol water is eluted, and collects eluent, and concentration and recovery ethanol obtains the extraction rich in aldehydes matter Thing, the total phenol content of the obtained extract rich in aldehydes matter is not less than 20.0%, weight ratio, in terms of gallic acid;
(3) by the omission timber 1 by AB-8 macroporous absorbent resin absorbing phenolic materials be pumped into by pretreatment 717 it is cloudy from Sub-exchange resin, collects the organic acid in omission timber 2, detection omission timber 2, stops being pumped into when positive reaction is presented;
(4) rinse D301G anion exchange resin to flushing liquor with pure water to clarify, be 50% with volumn concentration Ethanol water is eluted, and collects eluent, concentration and recovery ethanol is obtained rich in extracts such as organic acids, obtained rich in organic Total acid content is not less than 30%, weight ratio, with citrometer in the extract of acid;
Active component system is used as using the extract obtained above rich in aldehydes matter and the extract rich in organic acid Into the plum halogen essence functional food rich in aldehydes matter and organic acid, wherein the quality hundred of the extract rich in aldehydes matter It is 10% to divide content, and the weight/mass percentage composition of the extract rich in organic acid is 90%.
Preparation process is:Two kinds of extracts are freeze-dried, respective powder is obtained, by the extraction rich in aldehydes matter The weight/mass percentage composition of thing is 10%, and the weight/mass percentage composition of the extract rich in organic acid is 90% mixing, loads capsule, i.e., The plum halogen essence functional food of aldehydes matter and organic acid must be rich in.
Embodiment 3
As shown in fig. 1, the plum halogen essence functional food rich in aldehydes matter and organic acid that the present embodiment is provided Preparation method, comprises the following steps:
(1) plum halogen 100L is taken, 80 mesh nylon filtering cloths filtering, 6000 revs/min of centrifugations obtain clarifying plum halogen;Plum halogen will be clarified The X-5 macroporous absorbent resins by pretreatment are pumped into, collection omission timber 1 is standby, and detects the aldehydes matter in omission timber 1, is in Stop adding plum halogen during existing positive reaction;
(2) rinse resin column to flushing liquor with pure water to clarify, with 30% containing 0.12% hydrochloric acid (volumn concentration) (volumn concentration) methanol aqueous solution is eluted, and collects eluent, and concentration and recovery methanol obtains the extraction rich in aldehydes matter Thing, the total phenol content of the obtained extract rich in aldehydes matter is not less than 20.0%, weight ratio, in terms of gallic acid;
(3) by the omission timber 1 by X-5 macroporous absorbent resin absorbing phenolic materials be pumped into by pretreatment 717 it is cloudy from Sub-exchange resin, collects the organic acid in omission timber 2, detection omission timber 2, stops being pumped into when positive reaction is presented;
(4) rinse D301G anion exchange resin to flushing liquor with pure water to clarify, be 30% with volumn concentration Methanol aqueous solution is eluted, and collects eluent, concentration and recovery methanol is obtained rich in extracts such as organic acids, obtained rich in organic Total acid content is not less than 30%, weight ratio, with citrometer in the extract of acid;
Active component system is used as using the extract obtained above rich in aldehydes matter and the extract rich in organic acid Into the plum halogen essence functional food rich in aldehydes matter and organic acid, wherein the quality hundred of the extract rich in aldehydes matter It is 30% to divide content, and the weight/mass percentage composition of the extract rich in organic acid is 70%.
Preparation process is:Two kinds of extracts are freeze-dried, respective powder is obtained, by the extraction rich in aldehydes matter The weight/mass percentage composition of thing is 30%, and the weight/mass percentage composition of the extract rich in organic acid is 70% mixing, and addition tablet is normal With auxiliary material, tablet is pressed into, the plum halogen essence functional food rich in aldehydes matter and organic acid is produced.
Embodiment 4
As shown in fig. 1, the plum halogen essence functional food rich in aldehydes matter and organic acid that the present embodiment is provided Preparation method, comprises the following steps:
(1) plum halogen 100L is taken, 200 mesh nylon filtering cloths filtering, 4000 revs/min of centrifugations obtain clarifying plum halogen;Plum halogen will be clarified The X-5 macroporous absorbent resins by pretreatment are pumped into, collection omission timber 1 is standby, and detects the aldehydes matter in omission timber 1, is in Stop adding plum halogen during existing positive reaction;
(2) rinse resin column to flushing liquor with pure water to clarify, with 92% containing 0.08% hydrochloric acid (volumn concentration) (volumn concentration) ethanol water is eluted, and collects eluent, and concentration and recovery ethanol obtains the extraction rich in aldehydes matter Thing, the total phenol content of the obtained extract rich in aldehydes matter is not less than 20.0%, weight ratio, in terms of gallic acid;
(3) by the omission timber 1 by X-5 macroporous absorbent resin absorbing phenolic materials be pumped into by pretreatment 717 it is cloudy from Sub-exchange resin, collects the organic acid in omission timber 2, detection omission timber 2, stops being pumped into when positive reaction is presented;
(4) rinse D301G anion exchange resin to flushing liquor with pure water to clarify, be 80% with volumn concentration Ethanol water is eluted, and collects eluent, concentration and recovery ethanol is obtained rich in extracts such as organic acids, obtained rich in organic Total acid content is not less than 30%, weight ratio, with citrometer in the extract of acid;
Active component system is used as using the extract obtained above rich in aldehydes matter and the extract rich in organic acid Into the plum halogen essence functional food rich in aldehydes matter and organic acid, wherein the quality hundred of the extract rich in aldehydes matter It is 20% to divide content, and the weight/mass percentage composition of the extract rich in organic acid is 80%.
Preparation process is:By two kinds of extracts with pure water constant volume into equal volume, by the extract rich in aldehydes matter Weight/mass percentage composition be 20%, the weight/mass percentage composition of the extract rich in organic acid is 80% mixing, oral liquid is made, i.e., The plum halogen essence functional food of aldehydes matter and organic acid must be rich in.

Claims (9)

1. a kind of plum halogen essence functional food rich in aldehydes matter and organic acid, it is characterized in that:The activity of the functional food Composition includes the extract rich in aldehydes matter and the extract rich in organic acid, wherein the matter of the extract rich in aldehydes matter It is 5%~30% to measure percentage composition, and the weight/mass percentage composition of the extract rich in organic acid is 70%~95%, rich in aldehydes matter Acquisition is made by the steps in extract and extract rich in organic acid:
(1)Take filtrate to centrifuge after taking plum halogen, filtering, obtain clarifying plum halogen, clarification plum halogen is added in large pore resin absorption column, Collect omission timber 1 standby, aldehydes matter in detection omission timber 1 is positive and shows large pore resin absorption column adsorption saturation, stops Only add plum halogen;
(2)Large pore resin absorption column is rinsed to eluate water white transparency with pure water, is inhaled using acid alcohol solvent elution macropore Attached resin column, collects eluent and is concentrated to give the extract rich in aldehydes matter;
(3)Take step(1)In omission timber 1, be added in anion-exchange resin column, collect omission timber 2, detect omission timber 2 In organic acid, the positive is presented and shows anion-exchange resin column adsorption saturation, stops adding omission timber 1;
(4)Anion-exchange resin column is rinsed to eluate water white transparency with pure water, is eluted using alcohols solvent, is collected elution Liquid is concentrated to give the extract rich in organic acid.
2. the plum halogen essence functional food according to claim 1 rich in aldehydes matter and organic acid, it is characterized in that:Step Suddenly(1)The aperture of filter cloth is 80 ~ 300 mesh during middle filtering, and the rotating speed of centrifuge is 4000 ~ 10000 revs/min during centrifugation.
3. the plum halogen essence functional food according to claim 1 rich in aldehydes matter and organic acid, it is characterized in that:Step Suddenly(1)Described in large pore resin absorption column be X-5 macroporous absorbent resins or AB-8 macroporous absorbent resins.
4. the plum halogen essence functional food according to claim 1 rich in aldehydes matter and organic acid, it is characterized in that:Step Suddenly(1)Aldehydes matter in middle use forint- phenol law detection omission timber 1.
5. the plum halogen essence functional food according to claim 1 rich in aldehydes matter and organic acid, it is characterized in that:Step Suddenly(2)Described in acid alcohol solvent be containing acid alcohol solution, wherein described acid be hydrochloric acid or formic acid, it is described Alcohol solution is methanol aqueous solution or ethanol water, and the wherein volumn concentration of methanol or ethanol is 30~95%, hydrochloric acid Or the volumn concentration of formic acid is 0.08 ~ 0.12%.
6. the plum halogen essence functional food according to claim 1 rich in aldehydes matter and organic acid, it is characterized in that:Step Suddenly(2)Described in the extract rich in aldehydes matter in total phenol content be not less than 20.0%, weight ratio, in terms of gallic acid.
7. the plum halogen essence functional food according to claim 1 rich in aldehydes matter and organic acid, it is characterized in that:Step Suddenly(3)Described in anion-exchange resin column be 717 type anion exchange resin or D301G type anion exchange resin.
8. the plum halogen essence functional food according to claim 1 rich in aldehydes matter and organic acid, it is characterized in that:Step Suddenly(3)Organic acid in middle use pH meter or acid-base titration detection omission timber 2.
9. the plum halogen essence functional food according to claim 1 rich in aldehydes matter and organic acid, it is characterized in that:Step Suddenly(4)Described in alcohols solvent be methanol aqueous solution or ethanol water, described methanol or the volumn concentration of ethanol 30~80%;Step(4)Described in the extract rich in organic acid in total acid content be not less than 30%, weight ratio, with citric acid Meter.
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CN109953312A (en) * 2019-03-06 2019-07-02 广东省农业科学院蚕业与农产品加工研究所 A kind of plum halogen red acid soup and preparation method thereof
CN111978422B (en) * 2020-08-25 2022-06-21 湖南华诚生物资源股份有限公司 Method for separating multiple active ingredients from waste liquid after pigment extraction from roselle
CN112544764A (en) * 2020-11-19 2021-03-26 溜溜果园集团股份有限公司 Acid locking process in green plum product processing process

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CN101904528A (en) * 2010-07-15 2010-12-08 大理学院 Method for producing plum juice via plum halogen desalination
CN104642701B (en) * 2015-03-11 2018-03-13 广东殿羽田食品有限公司 A kind of preparation method of organic acid rich green plum sweetmeat

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PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: A plum bittern essence functional food rich in phenols and organic acids and its preparation method

Granted publication date: 20170822

Pledgee: Bank of Communications Co.,Ltd. Jieyang Branch

Pledgor: Puning xiaomeiwu Food Co.,Ltd.

Registration number: Y2024980006836