CN111635444A - Method for extracting naringin from plants by counter-current hot water method - Google Patents
Method for extracting naringin from plants by counter-current hot water method Download PDFInfo
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- CN111635444A CN111635444A CN202010586176.5A CN202010586176A CN111635444A CN 111635444 A CN111635444 A CN 111635444A CN 202010586176 A CN202010586176 A CN 202010586176A CN 111635444 A CN111635444 A CN 111635444A
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- 239000001606 7-[(2S,3R,4S,5S,6R)-4,5-dihydroxy-6-(hydroxymethyl)-3-[(2S,3R,4R,5R,6S)-3,4,5-trihydroxy-6-methyloxan-2-yl]oxyoxan-2-yl]oxy-5-hydroxy-2-(4-hydroxyphenyl)chroman-4-one Substances 0.000 title claims abstract description 126
- 229930019673 naringin Natural products 0.000 title claims abstract description 126
- DFPMSGMNTNDNHN-ZPHOTFPESA-N naringin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1[C@H](OC=2C=C3O[C@@H](CC(=O)C3=C(O)C=2)C=2C=CC(O)=CC=2)O[C@H](CO)[C@@H](O)[C@@H]1O DFPMSGMNTNDNHN-ZPHOTFPESA-N 0.000 title claims abstract description 126
- 229940052490 naringin Drugs 0.000 title claims abstract description 126
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 103
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- 230000008025 crystallization Effects 0.000 claims description 18
- 240000000560 Citrus x paradisi Species 0.000 claims description 15
- 235000013399 edible fruits Nutrition 0.000 claims description 15
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- CWBZAESOUBENAP-QVNVHUMTSA-N Naringin dihydrochalcone Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1[C@H](OC=2C=C(O)C(C(=O)CCC=3C=CC(O)=CC=3)=C(O)C=2)O[C@H](CO)[C@@H](O)[C@@H]1O CWBZAESOUBENAP-QVNVHUMTSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Extraction Or Liquid Replacement (AREA)
- Medicines Containing Plant Substances (AREA)
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Abstract
The invention discloses a method for extracting naringin from plants by a countercurrent hot water method, which comprises the steps of countercurrent extraction: adding hot water into a countercurrent extractor, and then feeding the raw material to be extracted and dried into the countercurrent extractor according to the liquid-material ratio (20-30): 1; or feeding the fresh raw material to be extracted into a countercurrent extractor according to the liquid-material ratio not more than 10:1, wherein the flow directions of the raw material and hot water are opposite, the extraction is carried out for 1-3 hours, and the initial temperature of the hot water and the temperature in the extraction process are both kept at 90 ℃ or above. The method for extracting the naringin from the plants by the counter-current hot water method innovatively adopts the technology of combining hot water and counter-current extraction, the material flow and the extracting solution run in reverse directions, the raw material with high naringin content and the hot water with low naringin content are fully communicated in a head-on mode, and the naringin in the raw material is dissolved in the hot water to the maximum extent.
Description
Technical Field
The invention relates to the technical field of extraction of plant components, in particular to a method for extracting naringin from plants by a countercurrent hot water method.
Background
The orange is the first fruit in the world, is rich in flavonoid functional components such as naringin and the like, and is widely applied to the aspects of medicine, food science, chemistry and the like. Naringin is also called naringin, has various pharmacological activities, such as regulating blood fat, resisting diabetes, resisting allergy, maintaining nerves and the like, and a large number of researches show that the naringin also has the effects of resisting oxidation, inflammation and cancer, can influence the activity of digestive tract enzymes, can enhance the curative effect of other medicines as a supplement, and is a potential bioactive component. Naringin can be hydrogenated and reduced into naringin dihydrochalcone, is a novel non-caloric sweetener, and is mainly used as sugar substitute in chewing gum, preserved fruit of preserved fruit and pericarpium Citri Tangerinae, beer, fruit juice beverage and functional beverage. The naringin can also be used as a sweetening agent of daily chemical products such as toothpaste, is already included in the use standard of food additives in China (GB2760-2011), and is put into a list of natural food additives which are generally accepted as safe substances by the American food and drug administration, Japan and the like.
Naringin is mainly present in the pericarp and is present in lower amounts in the pulp and seeds. The young fruit has large proportion of peel and high content. The citrus processing peel and residue utilization rate in China is low, and the fruit dropping and the thinned small fruit are not utilized basically before picking, so that the resource waste is caused, and the environment is polluted. In the past, the extraction of naringin mainly adopts an organic solvent or low-concentration alkali liquor, so that the cost is high, impurities are more, the pollution is serious, and the naringin is easily degraded by the alkali liquor extraction.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for extracting naringin from plants by a counter-current hot water method, which creatively combines hot water and counter-current extraction technology and realizes the aims of high naringin extraction rate and high naringin purity.
The purpose of the invention is realized by adopting the following technical scheme:
a method for extracting naringin from plants by countercurrent hot water method comprises countercurrent extraction steps: adding hot water into a countercurrent extractor, and then feeding the raw material to be extracted and dried into the countercurrent extractor according to the liquid-material ratio (20-30): 1; or feeding the fresh raw material to be extracted into a countercurrent extractor according to the liquid-material ratio not more than 10:1, wherein the flow directions of the raw material and hot water are opposite, the extraction is carried out for 1-3 hours, and the initial temperature of the hot water and the temperature in the extraction process are both kept at 90 ℃ or above.
Further, the extraction time is 1-3 hours, and the initial temperature of hot water and the temperature in the extraction process are both more than or equal to 90 ℃.
Further, the raw material is fruit or pericarp of pomelo, grapefruit, tangelo, sour orange, satsuma orange, bitter orange, trifoliate orange or trifoliate orange.
Further, when the raw material to be extracted is dry raw material and the liquid-material ratio is (20-30):1, the method comprises the following steps:
a cutting step: cutting the raw material to be extracted to obtain a cut product;
drying the raw materials: drying the cut product to obtain a dried product; the dried raw materials are bagged and stored, and the drying aims to facilitate the storage of the raw materials and is beneficial to the annual production of the naringin;
a crushing step: crushing the dried product to obtain a crushed product;
a countercurrent extraction step: adding hot water into a countercurrent extractor, then feeding the crushed product into the countercurrent extractor according to a liquid-material ratio (20-30):1, wherein the flow directions of the crushed product and the hot water are opposite, extracting for 1-3 hours, and keeping the initial temperature of the hot water and the temperature during the extraction at 90 ℃ or above to obtain an extracting solution;
a concentration step: concentrating the extracting solution to obtain a concentrated solution;
a crystallization step: putting the concentrated solution into a crystallizing tank, and separating out naringin crystals;
a dehydration step: collecting naringin crystal, dehydrating to obtain dehydrated crystal;
and (3) drying a product: and drying the dehydrated crystal to obtain a finished product.
Further, in the cutting step, the raw material to be extracted is cut into cubes or into pieces; when dicing, dicing the raw material to be extracted into pieces of less than 0.8cm by a machine; when the cut pieces are cut into slices, the slices are cut into the thickness of less than 0.5cm to obtain cut products;
in the raw material drying step, drying the cut product by using a hot air dryer at the drying temperature of less than or equal to 110 ℃ until the moisture content is less than or equal to 12 percent to obtain a dried product;
in the crushing step, crushing the dried product by a crusher to obtain a crushed product, wherein the particle size diameter of the crushed product is less than or equal to 0.5 cm;
in the countercurrent extraction step: adding hot water into a countercurrent extractor, then feeding the crushed product into the countercurrent extractor according to the liquid-material ratio (20-30):1, wherein the flow directions of the crushed product and the hot water are opposite, extracting for 1-3 hours, and the initial temperature of the hot water and the temperature in the extraction process are both more than or equal to 90 ℃, thus obtaining an extracting solution;
in the concentration step, the extracting solution is concentrated to obtain a concentrated solution, and the content of soluble solids in the concentrated solution is more than or equal to 10 DEG Brix; generally, the extract is concentrated about 15 times.
In the crystallization step, the concentrated solution is put into a crystallization tank, and after naringin is crystallized and separated out;
in the dehydration step, collecting naringin crystals, and filtering and dehydrating the naringin crystals by using a centrifugal machine or a vibrating screen to obtain dehydrated crystals;
and in the product drying step, drying the dehydrated crystallized product by using a hot air dryer until the water content of the naringin is less than or equal to 5 percent, and obtaining a finished product.
Further, when the raw material to be extracted is fresh raw material and the liquid-material ratio is not more than 10:1, the method comprises the following steps:
a cutting step: cutting the raw material to be extracted to obtain a cut product;
a countercurrent extraction step: adding hot water into a countercurrent extractor, then feeding the cut product into the countercurrent extractor according to the liquid-material ratio not more than 10:1, wherein the flow directions of the cut product and the hot water are opposite, extracting for 1-3 hours, and keeping the initial temperature of the hot water and the temperature in the extraction process at 90 ℃ or above to obtain an extracting solution;
a concentration step: concentrating the extracting solution to obtain a concentrated solution;
a crystallization step: putting the concentrated solution into a crystallizing tank, and separating out naringin crystals;
a dehydration step: collecting naringin crystal, dehydrating to obtain dehydrated crystal;
and (3) drying a product: and drying the dehydrated crystal to obtain a finished product.
Further, in the cutting step, cutting the raw materials into dices with the granularity of 0.1-3cm to obtain cut products;
in the countercurrent extraction step: adding hot water into a countercurrent extractor, then feeding the cut product into the countercurrent extractor according to a liquid-material ratio not more than 10:1, wherein the flow directions of the cut product and the hot water are opposite, extracting for 1-3 hours, and the initial temperature of the hot water and the temperature in the extraction process are both more than or equal to 90 ℃, so as to obtain an extracting solution;
in the concentration step, the extracting solution is concentrated to obtain a concentrated solution, and the content of soluble solids in the concentrated solution is more than or equal to 10 DEG Brix; generally, the extract is concentrated about 15 times.
In the crystallization step, the concentrated solution is put into a crystallization tank, and after naringin is crystallized and separated out;
in the dehydration step, collecting naringin crystals, and filtering and dehydrating the naringin crystals by using a centrifugal machine or a vibrating screen to obtain dehydrated crystals;
and in the product drying step, drying the dehydrated crystallized product by using a hot air dryer until the water content of the naringin is less than or equal to 5 percent, and obtaining a finished product.
Further, the method also comprises a packaging step, wherein the finished product is put into a lining bag for food and is put into a packaging barrel, and the barrel is sealed and labeled according to a preset weight.
Compared with the prior art, the invention has the beneficial effects that:
the method for extracting naringin from plants by the counter-current hot water method innovatively adopts the technology of combining hot water and counter-current extraction, the material flow and the extracting solution run in reverse directions, the raw material with high content of naringin is fully communicated with the hot water with low content of naringin, the material and the water run in reverse directions, the raw material with gradually reduced content and the hot water with gradually increased concentration of naringin continue to communicate to a certain degree along with the extraction of the naringin, after more than 80 percent of the naringin is extracted, the raw material is extruded to remove residues, and in the extraction process, the extraction temperature, the extraction time and the liquid-material ratio are all set to be the optimal process parameters according to the characteristics of the raw material. Compared with other extraction methods, the method has the advantages of high naringin extraction rate, high extraction automation degree, energy and water conservation, labor and time conservation, high naringin purity, good quality, low extraction cost and environmental friendliness.
Drawings
Fig. 1 is a diagram of naringin in real form obtained in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and the detailed description, and it should be noted that any combination of the embodiments or technical features described below can be used to form a new embodiment without conflict. The raw materials, equipments and the like used in the following examples are commercially available unless otherwise specified.
The raw materials of the method for extracting the naringin from the plant by the counter-current hot water method can be fruits, peels or skin residues of pomelos, Shatian pomelos, honey pomelos, grapefruits, tangerines, limes, miscellaneous oranges, bitter oranges, poncirus trifoliata or poncirus trifoliata. The pomelo is not of the same species as grapefruit, tangelo, lime, satsuma orange, bitter orange, trifoliate orange and trifoliate orange, and the pomelo is related to these species.
When the extraction is carried out, the invention innovatively adopts a hot water countercurrent extraction technology to extract high-value naringin from picked fruit drops, thinned fruits, and other fruits and peel residues with high efficiency and low cost, thereby not only realizing the resource utilization of the wastes, but also meeting the increasing requirements of consumers on natural health care products and simultaneously having good environmental protection.
The conventional extraction method of naringin is to extract naringin by alcohol medium or alkali liquor, and the conventional methods have high cost, low extraction rate, low purity and heavy pollution. The invention changes the conventional alcohol extraction or alkali extraction method, adopts hot water as a solvent, has much lower hot water cost than ethanol, is pollution-free and safer, skillfully selects hot water as an extraction solvent, and carries out one-time countercurrent extraction without circulating repeated countercurrent extraction. This is the greatest difference between the hot water + countercurrent extraction core technology of the present invention and conventional extraction technology.
The embodiment of the invention is based on the production test of pilot plant test, the extraction rate of the naringin can reach more than 80 percent under the condition of the same equipment and experiment process, and the purity of the naringin is more than 90 percent; the traditional hot water extraction rate is generally less than 60%, the purity is less than 80%, the time is more than one time, and the processing cost (manpower, solvent, energy consumption and the like) is more than one time higher.
Example 1:
a method for extracting naringin from plants by countercurrent hot water method comprises the following steps:
dicing: dicing the fresh Shatian pomelo young fruit raw material by using a dicing machine, and cutting into pieces with the size of 0.6 cm;
drying the raw materials: drying the diced meat with a hot air dryer at 110 deg.C until the water content is lower than 12%, bagging, and ventilating at normal temperature for storage;
a crushing step: crushing the dried raw materials by a crusher, wherein the particle size diameter is 0.3 cm;
a countercurrent extraction step: the crushed material was fed into a counter current extractor with hot water added at a liquid to material ratio of 20:1 (weight ratio) and maintained at 95 ℃. The raw material and hot water flow oppositely, and the extraction time is 2 hours;
a concentration step: concentrating the extractive solution to 15 ° Brix;
a crystallization step: placing the concentrated solution in a crystallizing tank until a large amount of naringin is crystallized and precipitated,
a dehydration step: collecting naringin crystal, dewatering with centrifuge,
and (3) drying a finished product: drying naringin with hot air drier to water content of 5%;
packaging: weighing dried naringin according to a certain weight, placing into a lining bag for food in a packaging barrel, and binding tape to seal the barrel and label.
As shown in FIG. 1, it is a real diagram of the obtained naringin product. Example 1 the extraction rate of naringin is 88% and the purity of naringin is 95%.
Example 2:
a method for extracting naringin from plants by countercurrent hot water method comprises the following steps:
slicing: slicing the fresh Shatian pomelo young fruit raw material by using a slicing machine, and cutting into slices with the thickness of 0.3 cm;
drying the raw materials: the cut pieces were dried with a hot air dryer. The drying temperature is 110 deg.C, and the raw material is dried to water content of less than 12%. Bagging the dried raw materials, and ventilating and storing at normal temperature;
a crushing step: crushing the dried raw materials by a crusher, wherein the particle size diameter is 0.25 cm;
a countercurrent extraction step: the crushed material was fed into a counter current extractor with hot water added at a liquid to material ratio of 25:1 (weight ratio) and maintained at 95 ℃. The raw material and hot water flow oppositely, and the extraction time is 1.5 hours;
a concentration step: concentrating the extractive solution to 16 ° Brix;
a crystallization step: putting the concentrated solution into a crystallizing tank until a large amount of naringin is crystallized and separated out;
a dehydration step: collecting naringin crystal, and dehydrating with centrifuge;
and (3) drying a finished product: drying naringin with hot air drier to water content of 3%;
packaging: weighing dried naringin according to a certain weight, placing into a lining bag for food in a packaging barrel, and binding tape to seal the barrel and label.
Example 2 the extraction rate of naringin is more than 85%, and the purity of naringin is 93%.
Example 3:
a method for extracting naringin from plants by countercurrent hot water method comprises the following steps:
dicing: dicing the raw material of the fresh grapefruit young fruit by using a dicing machine, and cutting into the size of 0.5 cm;
drying the raw materials: drying the diced meat with hot air dryer. The drying temperature is 110 ℃, and the raw material is dried to the moisture content of 10%. Bagging the dried raw materials, and ventilating and storing at normal temperature;
a crushing step: crushing the dried raw materials by a crusher, wherein the particle size diameter is 0.3 cm;
a countercurrent extraction step: feeding the crushed raw materials into a countercurrent extractor which is added with hot water according to the liquid-material ratio of 30:1 (weight ratio), and keeping the temperature at 96 ℃; the raw material and hot water flow oppositely, and the extraction time is 2.5 hours;
a concentration step: concentrating the extractive solution to 18 ° Brix;
a crystallization step: putting the concentrated solution into a crystallizing tank until a large amount of naringin is crystallized and separated out;
a dehydration step: collecting naringin crystal, and dehydrating with centrifuge;
and (3) drying a finished product: drying naringin with hot air drier to water content of 4%;
packaging: weighing dried naringin according to a certain weight, placing into a lining bag for food in a packaging barrel, and binding tape to seal the barrel and label.
Example 3 naringin extraction rate is 90%, naringin purity 93%.
Example 4:
a method for extracting naringin from plants by countercurrent hot water method comprises the following steps:
a cutting step: cutting the young fruits of GUAN xi GUAN into pieces with particle size of 0.2 cm;
a countercurrent extraction step: the chopped material was fed into a countercurrent extractor with hot water added at a liquid to feed ratio of 10:1 (by weight) and maintained at 95 ℃. The raw material and hot water flow oppositely, and the extraction time is 2 hours;
a concentration step: concentrating the extractive solution to 20 ° Brix;
a crystallization step: putting the concentrated solution into a crystallizing tank until a large amount of naringin is crystallized out.
A dehydration step: collecting naringin crystal, and dewatering with centrifuge.
And (3) drying: drying naringin with hot air drier to water content of 5%;
packaging: weighing dried naringin according to a certain weight, placing into a lining bag for food in a packaging barrel, and binding tape to seal the barrel and label.
Example 4 naringin extraction rate was 90% and naringin purity was 91%.
Example 5:
a method for extracting naringin from plants by countercurrent hot water method comprises the following steps:
a cutting step: cutting the fresh peel residue of sour pomelo into particles with a particle size of 0.5 cm;
a countercurrent extraction step: the chopped material was fed into a countercurrent extractor with hot water added at a liquid to feed ratio of 5:1 (by weight) and maintained at 90 ℃. The raw material and hot water flow oppositely, and the extraction time is 3 hours;
a concentration step: concentrating the extractive solution to 18 ° Brix;
a crystallization step: putting the concentrated solution into a crystallizing tank until a large amount of naringin is crystallized out.
A dehydration step: collecting naringin crystal, and dewatering with centrifuge.
And (3) drying: drying naringin with hot air drier to water content of 4.5%;
packaging: weighing dried naringin according to a certain weight, placing into a lining bag for food in a packaging barrel, and binding tape to seal the barrel and label.
Example 5 naringin extraction rate was 86% and naringin purity was 90%.
Comparative example 1
Comparative example 1 differs from example 1 in that: during the counter-current extraction step, the hot water temperature was maintained at 85 ℃. The rest is the same as in example 1.
Comparative example 1 the naringin extraction rate is 80% and the naringin purity is 81%. It can be seen that, in the process of countercurrent extraction, the hot water temperature is a very critical parameter, the hot water temperature is lower than 90 ℃, the extraction rate and the naringin purity can be reduced, and in the process of countercurrent extraction, the hot water temperature, the liquid-material ratio and the extraction time are three very important parameters, and the three must be accurately controlled at the same time to obtain the best benefit.
Comparative example 2
Comparative example 2 differs from example 2 in that: in the countercurrent extraction step, the extraction time was 45 minutes. The rest is the same as in example 2.
Comparative example 2 the extraction rate of naringin is 70%, and the purity of naringin is 82%. It can be seen that, in the process of countercurrent extraction, the extraction time is a very critical parameter, the extraction rate and the naringin purity can be reduced if the extraction time is less than 1 hour, and in the process of countercurrent extraction, the hot water temperature, the liquid-material ratio and the extraction time are three very important parameters, and the three must be accurately controlled at the same time to obtain the best benefit.
Comparative example 3
Comparative example 3 differs from example 3 in that: in the countercurrent extraction step, hot water is added according to the liquid-material ratio of 15:1 (weight ratio). The rest is the same as in example 3.
Comparative example 3 the extraction rate of naringin is 75%, and the purity of naringin is 80%. It can be seen that the liquid-material ratio is a very critical parameter in the countercurrent extraction process, when the raw material is a dry product, the liquid-material ratio exceeds the range of (20-30):1 (weight ratio), the extraction rate and the naringin purity can be reduced, and in the countercurrent extraction process, the hot water temperature, the liquid-material ratio and the extraction time are three very important parameters, and the three must be accurately controlled at the same time to obtain the best benefit.
Comparative example 4
Comparative example 4 differs from example 4 in that: does not comprise a countercurrent extraction step, and the specific operation of the extraction step is as follows: placing the chopped raw materials into an extraction tank, adding hot water according to the liquid-material ratio of 10:1 (weight ratio), maintaining the temperature at 95 deg.C, soaking for 5 hr, and stirring for 3 times. The rest is the same as in example 4.
Comparative example 4 the naringin extraction rate is 60% and the naringin purity is 75%. Therefore, only hot water is adopted for extracting naringin, and countercurrent extraction operation is not combined, so that the extraction rate and the purity of the naringin can be greatly reduced.
Comparative example 5
Comparative example 5 differs from example 5 in that: in the countercurrent extraction step, the chopped material was fed into a countercurrent extractor and hot water was added at a liquid to material ratio of 15:1 (by weight) and the temperature was maintained at 88 ℃. The raw material and hot water flow oppositely, and the extraction time is 50 minutes; the rest is the same as in example 5.
Comparative example 5 the naringin extraction rate is 72% and the naringin purity is 80%. Therefore, under the condition of using fresh raw materials, the extraction rate and the naringin purity are also reduced by overhigh liquid-material ratio, lower extraction temperature and shorter extraction time.
Comparative example 6
Example 6 differs from example 1 in that conventional 70% ethanol extraction is used, the liquid-material ratio is 5:1, the extraction temperature is 60 ℃, the extraction method is to soak in an extraction tank for 3 hours under the condition of heat preservation, after filtering residue, ethanol is volatilized, naringin in residual liquid is crystallized, and the dehydration and drying methods are the same as example 1.
Comparative example 6 the naringin extraction rate is 65% and the naringin purity is 82%.
Comparative example 7
Example 7 differs from example 1 in that the extraction is carried out with a conventional lye (pH13) at a liquor-to-feed ratio of 20:1 at an extraction temperature of 95 ℃ for 1 hour in an extraction tank, the extraction is carried out by filtering off the residue, neutralizing the residue with hydrochloric acid to a pH of 6, concentrating the solution 5 times, placing the solution in a crystallization tank, crystallizing, dehydrating and drying the solution in the same manner as in example 1.
Comparative example 7 naringin extraction rate was 45%, naringin purity was 73%.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (8)
1. A method for extracting naringin from plants by a countercurrent hot water method is characterized by comprising the steps of countercurrent extraction: adding hot water into a countercurrent extractor, and then feeding the raw material to be extracted and dried into the countercurrent extractor according to the liquid-material ratio (20-30): 1; or feeding the fresh raw material to be extracted into a countercurrent extractor according to the liquid-material ratio not more than 10:1, wherein the flow directions of the raw material and hot water are opposite, the extraction is carried out for 1-3 hours, and the initial temperature of the hot water and the temperature in the extraction process are both kept at 90 ℃ or above.
2. The counter-current hot water process for the extraction of naringin from plants as claimed in claim 1, wherein the extraction time is 1-3 hours, and the initial temperature of the hot water and the temperature during the extraction are both maintained at 90 ℃ and above.
3. The counter-current hot water method for extracting naringin from plants as claimed in claim 1, wherein the raw material is fruit or pericarp of pomelo, grapefruit, tangelo, lime, satsuma orange, bitter orange, trifsuma orange or trifsuma orange.
4. The method for extracting naringin from plants by the counter-current hot water method as claimed in claim 1, which comprises the following steps when the raw material to be extracted is dry raw material and the liquid-to-material ratio is (20-30): 1:
a cutting step: cutting the raw material to be extracted to obtain a cut product;
drying the raw materials: drying the cut product to obtain a dried product;
a crushing step: crushing the dried product to obtain a crushed product;
a countercurrent extraction step: adding hot water into a countercurrent extractor, then feeding the crushed product into the countercurrent extractor according to a liquid-material ratio (20-30):1, wherein the flow directions of the crushed product and the hot water are opposite, extracting for 1-3 hours, and keeping the initial temperature of the hot water and the temperature during the extraction at 90 ℃ or above to obtain an extracting solution;
a concentration step: concentrating the extracting solution to obtain a concentrated solution;
a crystallization step: putting the concentrated solution into a crystallizing tank, and separating out naringin crystals;
a dehydration step: collecting naringin crystal, dehydrating to obtain dehydrated crystal;
and (3) drying a product: and drying the dehydrated crystal to obtain a finished product.
5. The counter-current hot water method for extracting naringin from plants as claimed in claim 4, wherein in the cutting step, the raw material to be extracted is cut into cubes or into pieces; when dicing, dicing the raw material to be extracted into pieces of less than 0.8cm by a machine; when the cut pieces are cut into slices, the slices are cut into the thickness of less than 0.5cm to obtain cut products;
in the raw material drying step, drying the cut product by using a hot air dryer at the drying temperature of less than or equal to 110 ℃ until the moisture content is less than or equal to 12 percent to obtain a dried product;
in the crushing step, crushing the dried product by a crusher to obtain a crushed product, wherein the particle size diameter of the crushed product is less than or equal to 0.5 cm;
in the countercurrent extraction step: adding hot water into a countercurrent extractor, then feeding the crushed product into the countercurrent extractor according to the liquid-material ratio (20-30):1, wherein the flow directions of the crushed product and the hot water are opposite, extracting for 1-3 hours, and the initial temperature of the hot water and the temperature in the extraction process are both more than or equal to 90 ℃, thus obtaining an extracting solution;
in the concentration step, the extracting solution is concentrated to obtain a concentrated solution, and the content of soluble solids in the concentrated solution is more than or equal to 10 DEG Brix;
in the crystallization step, the concentrated solution is put into a crystallization tank, and after naringin is crystallized and separated out;
in the dehydration step, collecting naringin crystals, and filtering and dehydrating the naringin crystals by using a centrifugal machine or a vibrating screen to obtain dehydrated crystals;
and in the product drying step, drying the dehydrated crystallized product by using a hot air dryer until the water content of the naringin is less than or equal to 5 percent, and obtaining a finished product.
6. The method for extracting naringin from plants by the counter-current hot water method as claimed in claim 1, which comprises the following steps when the raw material to be extracted is fresh raw material and the liquid-material ratio is not more than 10: 1:
a cutting step: cutting the raw material to be extracted to obtain a cut product;
a countercurrent extraction step: adding hot water into a countercurrent extractor, then feeding the cut product into the countercurrent extractor according to the liquid-material ratio not more than 10:1, wherein the flow directions of the cut product and the hot water are opposite, extracting for 1-3 hours, and keeping the initial temperature of the hot water and the temperature in the extraction process at 90 ℃ or above to obtain an extracting solution;
a concentration step: concentrating the extracting solution to obtain a concentrated solution;
a crystallization step: putting the concentrated solution into a crystallizing tank, and separating out naringin crystals;
a dehydration step: collecting naringin crystal, dehydrating to obtain dehydrated crystal;
and (3) drying a product: and drying the dehydrated crystal to obtain a finished product.
7. The counter-current hot water method for extracting naringin from plants as claimed in claim 6, wherein in the cutting step, the raw material is cut into dices with a particle size of 0.1-3cm to obtain a cut product;
in the countercurrent extraction step: adding hot water into a countercurrent extractor, then feeding the cut product into the countercurrent extractor according to a liquid-material ratio not more than 10:1, wherein the flow directions of the cut product and the hot water are opposite, extracting for 1-3 hours, and the initial temperature of the hot water and the temperature in the extraction process are both more than or equal to 90 ℃, so as to obtain an extracting solution;
in the concentration step, the extracting solution is concentrated to obtain a concentrated solution, and the content of soluble solids in the concentrated solution is more than or equal to 10 DEG Brix;
in the crystallization step, the concentrated solution is put into a crystallization tank, and after naringin is crystallized and separated out;
in the dehydration step, collecting naringin crystals, and filtering and dehydrating the naringin crystals by using a centrifugal machine or a vibrating screen to obtain dehydrated crystals;
and in the product drying step, drying the dehydrated crystallized product by using a hot air dryer until the water content of the naringin is less than or equal to 5 percent, and obtaining a finished product.
8. The counter-current hot-water method for extracting naringin from plants as claimed in claim 4 or 6, further comprising a packaging step of putting the finished product into a lining bag for food and into a packaging barrel, and tying the barrel with a label according to a predetermined weight.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112830946A (en) * | 2021-01-31 | 2021-05-25 | 中山大学 | Method for extracting naringin at low temperature under boiling point |
| CN112940060A (en) * | 2021-02-20 | 2021-06-11 | 嘉应学院 | Method for extracting naringin from shaddock peel by counter-current hot water method |
| CN115500443A (en) * | 2022-09-25 | 2022-12-23 | 中国海洋大学 | Naringin-rich extract and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964408A (en) * | 2012-12-19 | 2013-03-13 | 广东中大天翼生物科技发展有限公司 | Method for extracting naringin from red tangerine peel |
| CN109369753A (en) * | 2018-12-19 | 2019-02-22 | 湖北康乐源生物科技有限公司 | A method of extracting aurantiin from shaddock okra fruit |
| CN110684063A (en) * | 2019-10-28 | 2020-01-14 | 成都蜀西制药有限公司 | Method for preparing naringin |
-
2020
- 2020-06-24 CN CN202010586176.5A patent/CN111635444A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964408A (en) * | 2012-12-19 | 2013-03-13 | 广东中大天翼生物科技发展有限公司 | Method for extracting naringin from red tangerine peel |
| CN109369753A (en) * | 2018-12-19 | 2019-02-22 | 湖北康乐源生物科技有限公司 | A method of extracting aurantiin from shaddock okra fruit |
| CN110684063A (en) * | 2019-10-28 | 2020-01-14 | 成都蜀西制药有限公司 | Method for preparing naringin |
Non-Patent Citations (1)
| Title |
|---|
| 乔延江 主编: "《中华医学百科全书﹒中药制剂学》", 30 April 2017 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112830946A (en) * | 2021-01-31 | 2021-05-25 | 中山大学 | Method for extracting naringin at low temperature under boiling point |
| CN112940060A (en) * | 2021-02-20 | 2021-06-11 | 嘉应学院 | Method for extracting naringin from shaddock peel by counter-current hot water method |
| CN112940060B (en) * | 2021-02-20 | 2023-08-11 | 嘉应学院 | Method for extracting naringin from shaddock peel by countercurrent hot water method |
| CN115500443A (en) * | 2022-09-25 | 2022-12-23 | 中国海洋大学 | Naringin-rich extract and preparation method thereof |
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