CN115500443A - Naringin-rich extract and preparation method thereof - Google Patents
Naringin-rich extract and preparation method thereof Download PDFInfo
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- 239000000284 extract Substances 0.000 title claims abstract description 49
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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 45
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses an extract rich in naringin and a preparation method thereof, wherein the extract is obtained by carrying out micro-pressure water leaching extraction on shaddock peel, and the content of the naringin is more than 80%. The preparation method of the extract rich in naringin comprises the following steps: selecting shaddock peel: peeling fresh, non-rotten and non-deteriorated pomelo peel, and cutting into blocks of about 1 cm; drying: drying the shaddock peel at the temperature lower than 60 ℃ until the water content is less than or equal to 5 percent; crushing and sieving: crushing and sieving the shaddock peel by using a high-speed universal crusher for later use; extraction: adding water into the shaddock peel powder according to a certain volume ratio, heating and pressurizing for extraction, and carrying out suction filtration while the shaddock peel powder is hot to obtain an extracting solution. The extraction process disclosed by the invention uses water as an extraction reagent, the obtained extracting solution has high naringin content, and the preparation process is low in price, economic and environment-friendly, high in safety, simple in process and easy to realize industrialization.
Description
Technical Field
The invention relates to the technical field of extraction of active substances of shaddock ped, and particularly relates to an extract rich in naringin and a preparation method thereof.
Background
The pomelo is one of the main economic fruit and vegetable varieties in China, the planting area and the yield are at the top of the world, and the pomelo accounts for more than half of the total yield of the pomelo in the world. The pomelo is a citrus fruit with the largest volume, the pomelo peel is thick, the pomelo peel accounts for 40-50% of the weight of the whole pomelo, and the pomelo peel is thrown away as waste under most conditions due to the limitations of the traditional processing technology, the processing technology and the like, so that the resource is greatly wasted.
Naringin is a dihydroflavonoids compound, widely exists in shaddock peel and shaddock peel, has a series of physiological activities of resisting cancer, resisting oxidation, reducing cholesterol and the like, and has important economic value and social benefit.
At present, the following methods are mainly used for extracting naringin: (1) aqueous solution extraction method: the aqueous solution extraction method is an original method for extracting functional substance components, has simple extraction process and low cost, but has long extraction time and low extraction rate in the traditional aqueous solution extraction method. (2) organic solvent method: the organic solvent extraction method is the most common method for extracting naringin, but the organic solvent method has relatively complex process, large organic solvent consumption and low safety factor, and is not suitable for being applied in industrial production. (3) supercritical fluid extraction: supercritical fluid extraction can retain the original properties of the extract to the maximum extent, but the equipment is expensive and is not suitable for industrial production. (4) enzyme extraction method: the enzyme has high selectivity, and the extraction efficiency can be greatly improved by selecting proper enzyme aiming at different extraction materials, but the enzyme is sensitive to the extraction environment, the temperature and pH of the enzyme reaction need to be strictly controlled in the extraction process, and the requirement on equipment in industrial production is high.
In conclusion, the preparation method which is efficient in extraction, simple and convenient to operate, economical, safe and suitable for industrial production is found, and the extraction of naringin from shaddock peel is of great significance.
Disclosure of Invention
The invention aims to provide an extract rich in naringin and a preparation method of the extract to make up for the defects of the prior art.
In order to achieve the purpose, the invention adopts the following specific technical scheme:
an extract rich in naringin is prepared by extracting pericarpium Citri Grandis with water under slight pressure, wherein the naringin content is above 80%.
The preparation method of the extract rich in naringin comprises the following steps:
(1) Selecting shaddock peel: peeling fresh, rotten and deteriorated pomelo peel, and cutting into blocks of about 1 cm;
(2) Drying: drying the shaddock peel at the temperature lower than 60 ℃ until the water content is less than or equal to 5 percent;
(3) Crushing and sieving: crushing and sieving the shaddock peel by using a high-speed universal crusher for later use;
(4) Extraction: adding water into the pomelo peel powder according to a certain volume ratio, heating and pressurizing for extraction, and carrying out suction filtration while the pomelo peel powder is hot to obtain the extract.
Further, the grapefruit in the step (1) can be Chongqing Liangping grapefruit.
Further, the temperature in the step (2) is 55 ℃.
Further, in the step (3), a 40-mesh sieve is sieved.
Further, the mass volume ratio in the step (4) is as follows: liquid (distilled water) = 1; the extraction temperature is 80-120 ℃; the extraction pressure is 0.11-0.14 MPa; the extraction time is 10-120 min.
The invention has the advantages and beneficial effects that:
the extraction process disclosed by the invention uses water as an extraction reagent, the obtained extracting solution has high naringin content, the preparation process is low in price, economic and environment-friendly, high in safety, simple in process and easy to realize industrialization, and the flavone compounds in the pomelo peel can be quickly, stably and massively extracted, so that the method is suitable for industrially producing the flavone compounds in the pomelo peel.
The extract obtained by the invention has good DPPH removing capability and good antioxidant activity, and can be applied to the deep processing fields of beverages, cosmetics and the like.
Drawings
FIG. 1 is an HPLC chromatogram of the extract prepared in example 1.
FIG. 2 is an HPLC chromatogram of the extract prepared in example 2.
FIG. 3 is an HPLC chromatogram of the extract prepared in example 3.
FIG. 4 is the naringin content in the extract under different heating temperature conditions in the process of the invention.
FIG. 5 shows the naringin extraction rate of the extract under different heating temperature conditions in the preparation process of the present invention.
FIG. 6 shows DPPH clearance of extracts at different heating temperatures in the preparation process of the present invention.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
The numerical values set forth in the examples of the present invention are approximations, not necessarily values. All values within the error range may be included without limiting to the specific values disclosed in the embodiments of the present invention, where the error or experimental conditions allow.
Example 1:
a preparation method of an extract rich in naringin comprises the following steps:
(1) Selecting shaddock peel: selecting Chongqing Liangping pomelo, peeling fresh pomelo peel without rottenness and deterioration, and cutting into 1cm blocks;
(2) Drying: drying the shaddock peel at 55 ℃ until the water content is less than or equal to 5 percent;
(3) Crushing and sieving: crushing the shaddock peel by using a high-speed universal crusher, and sieving by using a 40-mesh sieve for later use;
(4) Heating at normal pressure for water extraction: taking the following materials (pomelo peel powder) according to volume ratio: liquid (distilled water) = 1, and water is added into the pomelo peel powder for extraction, wherein the extraction temperature is 80 ℃, and the extraction time is 120 min. And after extraction, carrying out suction filtration while the extract is hot to obtain the extract.
Example 2:
a preparation method of an extract rich in naringin comprises the following steps:
(1) Selecting shaddock peel: selecting Chongqing Liangping pomelo, peeling fresh, rotten and deteriorated pomelo peel, and cutting into 1cm blocks;
(2) Drying: drying the shaddock peel at 55 ℃ until the water content is less than or equal to 5 percent;
(3) Crushing and sieving: crushing the shaddock peel by using a high-speed universal crusher, and sieving by using a 40-mesh sieve for later use;
(4) Micro-pressure heating water extraction: taking the materials (pomelo peel powder) according to the volume ratio: liquid (distilled water) = 1, and water is added into the pomelo peel powder for extraction, wherein the extraction temperature is 110 ℃, the extraction time is 120 min, and the pressure is 0.11 Mpa. And after extraction, carrying out suction filtration while the extract is hot to obtain the extract.
Example 3:
a preparation method of an extract rich in naringin comprises the following steps:
(1) Selecting shaddock peel: selecting Chongqing Liangping pomelo, peeling fresh, rotten and deteriorated pomelo peel, and cutting into 1cm blocks;
(2) Drying: drying the shaddock peel at 55 ℃ until the water content is less than or equal to 5 percent;
(3) Crushing and sieving: crushing the shaddock peel by using a high-speed universal crusher, and sieving by using a 40-mesh sieve for later use;
(4) Micro-pressure heating water extraction: taking the materials (pomelo peel powder) according to the volume ratio: liquid (distilled water) = 1, and water is added into the pomelo peel powder for extraction, wherein the extraction temperature is 120 ℃, the extraction time is 120 min, and the pressure is 0.14 Mpa. And after extraction, carrying out suction filtration while the extract is hot to obtain the extract.
Examples 4 and 5
The invention adopts a liquid chromatography (HPLC) method to measure the naringin content in the extracting solution.
HPLC chromatographic conditions: a chromatographic column: agilent ZORBAX Eclipse Plus C18 (100X 4.6mm, 3.5 μm) mobile phase: acetonitrile (A) and water (B), and gradient elution is adopted, wherein the elution procedure is as follows: (1) 0-8 min,23% A; (2) 8-13 min,65% A; (3) The time for the reaction is 14-16 min,70% of A; (4) 17-18 min,73% A; (5) 19-20 min,23% A; column temperature: at 40 ℃; flow rate: 1.0 mL min -1 The sample size is 10.0 muL; detection wavelength: 280 nm;
respectively extracting 5 ml of the extract rich in naringin obtained in examples 1-3 with 5 ml of ethyl acetate, retaining the upper layer of extract, adding 5 ml of ethyl acetate again into the lower layer of extract for extraction, repeating the extraction for 2-3 times, combining the extracts, performing rotary evaporation concentration at 55 ℃, and taking down nitrogen to blow white to pale yellow particles when about 1 ml of liquid is left in a rotary evaporation bottle. And adding 5 ml of chromatographic grade methanol into the rotary evaporation bottle for redissolution, filtering the mixture through a filter membrane of 0.45 mu m to obtain a naringenin extract, and carrying out liquid chromatography analysis.
The HPLC chromatograms obtained in example 4 are shown in fig. 1-3, respectively, and according to the peak areas of the HPLC chromatograms, the ratio of naringin in the naringin extract is 80.63% -89.84%. The test results of naringin content and extraction rate in the extract are shown in Table 1, and the naringin content in the extract of the pomelo in the examples 1 to 3 is 0.335 to 0.721 mg/ml, and the extraction rate is 1.72 to 3.74 percent. Test results show that the naringin content in the extract under the condition of micro-pressure is obviously higher than that of the extract under the condition of normal pressure, and the extraction of the naringin is more facilitated under the condition of micro-pressure heating. As shown in figures 4 and 5, under the condition of micro-pressure extraction, the extraction rate of the extract rich in naringin prepared by the invention can reach 3.74 percent, and the extraction rate is high. The problem of low naringin extraction rate in an aqueous solution extraction method in the prior art is effectively solved, water is used as an extraction reagent, the cost is low, the method is economical and environment-friendly, the safety is high, the process is simple, the industrialization is easy to realize, and the naringin in the naringin can be quickly, stably and massively extracted.
TABLE 1 naringin concentration and naringin content in the extract
The method adopts a spectrophotometry method to measure the DPPH clearance rate in the shaddock peel extracting solution.
The extracts rich in naringin obtained in examples 1-3 are diluted by 10 times and tested for DPPH scavenging capability, the testing result shows that the DPPH scavenging capability of the extracts is 59.29% -82.14%, the DPPH scavenging rate of examples 1-3 is shown in figure 6, and the extracts rich in naringin prepared by the invention have the efficacy of scavenging DPPH free radical activity, which shows that the extracts rich in naringin have the capability of resisting oxidative damage on a biochemical level and have the potential of product development.
The invention relates to a preparation method of an extract rich in naringin, which is characterized in that on the basis of the original water extraction process, heating and pressurizing extraction are carried out, the heating and pressurizing are optimized and improved, and the fact that the concentration of extracted non-medium naringin is higher under the condition of micro-pressure is found. The invention optimizes the water extraction conditions and improves the extraction rate of naringin in the shaddock peel. The obtained extract has naringin content of 0.335-0.721 mg/ml, and DPPH scavenging capacity of 59.29% -82.14%.
The above description is only a preferred embodiment of the present invention, and should not be construed as limiting the scope of the claims, and other substantially equivalent alternatives can be conceived by those skilled in the art and are within the scope of the present invention.
Claims (6)
1. An extract rich in naringin, which is characterized in that the extract is obtained by carrying out micro-pressure water leaching extraction on shaddock peel, and the content of the naringin is more than 80 percent.
2. A method for preparing an extract enriched in naringin, as claimed in claim 1, comprising the steps of:
(1) Selecting shaddock peel: peeling fresh, non-rotten and non-deteriorated pomelo peel, and cutting into blocks;
(2) Drying: drying the shaddock peel at the temperature lower than 60 ℃ until the water content is less than or equal to 5 percent;
(3) Crushing and sieving: crushing and sieving the shaddock peel by using a high-speed universal crusher for later use;
(4) Extraction: adding water into the shaddock peel powder according to a certain volume ratio, heating and pressurizing for extraction, and carrying out suction filtration while the shaddock peel powder is hot to obtain an extracting solution.
3. The preparation method according to claim 2, wherein the grapefruit in the step (1) is Chongqing Liangping grapefruit.
4. The method according to claim 2, wherein the temperature in the step (2) is 55 ℃.
5. The method of claim 2, wherein step (3) is carried out by passing through a 40 mesh sieve.
6. The preparation method according to claim 2, wherein the mass-to-volume ratio in the step (4) is material: liquid = 1; the extraction temperature is 80-120 ℃; the extraction pressure is 0.11-0.14 MPa; the extraction time is 10-120 min.
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| CN111635444A (en) * | 2020-06-24 | 2020-09-08 | 广东李金柚农业科技有限公司 | Method for extracting naringin from plants by counter-current hot water method |
| CN112336667A (en) * | 2020-12-17 | 2021-02-09 | 太和康美(北京)中医研究院有限公司 | Microcos paniculata leaf extract and preparation method and application thereof |
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| CN111635444A (en) * | 2020-06-24 | 2020-09-08 | 广东李金柚农业科技有限公司 | Method for extracting naringin from plants by counter-current hot water method |
| CN112336667A (en) * | 2020-12-17 | 2021-02-09 | 太和康美(北京)中医研究院有限公司 | Microcos paniculata leaf extract and preparation method and application thereof |
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