CN115428948B - Shaddock seed extract extraction process and application thereof - Google Patents
Shaddock seed extract extraction process and application thereof Download PDFInfo
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- 238000000605 extraction Methods 0.000 title claims abstract description 45
- 244000276331 Citrus maxima Species 0.000 title claims description 8
- 235000001759 Citrus maxima Nutrition 0.000 title claims description 8
- 239000000284 extract Substances 0.000 title abstract description 13
- 240000000560 Citrus x paradisi Species 0.000 claims abstract description 95
- 229940107702 grapefruit seed extract Drugs 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims description 57
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 238000007127 saponification reaction Methods 0.000 claims description 31
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 21
- 239000012670 alkaline solution Substances 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000007781 pre-processing Methods 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims 2
- 241000220225 Malus Species 0.000 claims 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 abstract description 22
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 abstract description 22
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 abstract description 22
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 abstract description 22
- 239000005642 Oleic acid Substances 0.000 abstract description 22
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 abstract description 22
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 abstract description 19
- 239000002537 cosmetic Substances 0.000 abstract description 7
- 239000002699 waste material Substances 0.000 abstract description 7
- 235000013402 health food Nutrition 0.000 abstract description 5
- 235000021122 unsaturated fatty acids Nutrition 0.000 abstract description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002994 raw material Substances 0.000 description 8
- 241001528553 Malus asiatica Species 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 235000019500 Grapefruit seed oil Nutrition 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 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 description 1
- 208000007882 Gastritis Diseases 0.000 description 1
- 244000141359 Malus pumila Species 0.000 description 1
- 235000011430 Malus pumila Nutrition 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 235000011203 Origanum Nutrition 0.000 description 1
- 240000000783 Origanum majorana Species 0.000 description 1
- 208000007107 Stomach Ulcer Diseases 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 239000010692 aromatic oil Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 235000015203 fruit juice Nutrition 0.000 description 1
- 235000019990 fruit wine Nutrition 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 201000005917 gastric ulcer Diseases 0.000 description 1
- 230000035784 germination Effects 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 235000012907 honey Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 235000015094 jam Nutrition 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 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 description 1
- 229940052490 naringin Drugs 0.000 description 1
- 229930019673 naringin Natural products 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000006041 probiotic Substances 0.000 description 1
- 235000018291 probiotics Nutrition 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- 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]
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microbiology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Mycology (AREA)
- Botany (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Biotechnology (AREA)
- Epidemiology (AREA)
- Birds (AREA)
- Dermatology (AREA)
- General Chemical & Material Sciences (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to the field of A23L33/105, in particular to a grapefruit seed extract extraction process and application thereof. Based on the application requirements and application prospects of components such as rich unsaturated fatty acids in the grapefruit seeds in the fields of health foods and cosmetics, the extraction process of the grapefruit seed extract is provided aiming at effective components such as oleic acid and oleic glyceride in the grapefruit seeds, the extraction rate is high, and the extraction process is environment-friendly, so that the waste grapefruit seed resources are fully utilized in grapefruit processing, and the content of oleic acid and oleic glyceride in the extract is improved on the premise of not influencing the extraction rate, so that the high-value utilization of the grapefruit seed extract in the fields of health foods and cosmetics is realized, and the grapefruit seed extract has high practical application value.
Description
Technical Field
The invention relates to the field of A23L33/105, in particular to a grapefruit seed extract extraction process and application thereof.
Background
The pomelo contains natural medicinal components such as natural oil, volatile oil, alkaloid, glycoside and the like, can be used for treating gastric ulcer and eliminating gastric inflammation, has wide application in fruits, skins, flowers and leaves, can be used as a raw material for extracting aromatic oil, can extract pectin from pomelo peel, can be directly eaten or processed into fruit juice, fruit wine, jam and can, contains abundant effective components such as oleic acid, flavone, naringin and the like, is beneficial to health care of human body, can tighten skin and reduce wrinkles, and has a small number of extraction and utilization processes related to the pomelo seeds at present.
Chinese patent CN110257161A discloses a grapefruit seed oil rich in fat-soluble probiotics and a preparation method thereof, which takes grapefruit seeds as raw materials, and after shelling, peeling and water planting germination treatment of the grapefruit seeds, the grapefruit seed oil is prepared by leaching or microwave-ultrasonic auxiliary extraction through an organic solvent, and the operation steps are complex, the used reagent is complex, and the realization of large-scale industrial production is not facilitated. Therefore, based on the application requirements and application prospects of components such as rich unsaturated fatty acids in the grapefruit seeds in the fields of health foods and cosmetics, the extraction process of the grapefruit seed extract is provided aiming at the effective components such as oleic acid and oleic glyceride in the grapefruit seeds, the extraction rate is high, and the extraction process is environment-friendly, so that the waste grapefruit seed resources in grapefruit processing are fully utilized, and the content of oleic acid and oleic glyceride in the extract is improved on the premise of not influencing the extraction rate, so that the high-value utilization of the grapefruit seed extract in the fields of health foods and cosmetics is realized, and the grapefruit seed extract has high practical application value.
Disclosure of Invention
In order to solve the above problems, in one aspect, the present invention provides an extraction process of a grapefruit seed extract, at least comprising the following steps:
s1, preprocessing grapefruit seeds;
s2, placing the cleaned and dried grapefruit seeds into a pulverizer for pulverizing;
s3, placing the crushed grapefruit seeds into a glass container, and adding an alkaline solution with a certain mass for saponification reaction;
S4, carrying out suction filtration on the liquid after the saponification reaction, separating and collecting filtrate, and dripping acid solution with certain mass into the filtrate for stirring reaction;
and S5, standing the liquid after the stirring reaction for 8-12h, reserving upper-layer liquid, and washing the upper-layer liquid with clear water for 3-5 times to obtain the grapefruit seed extract.
As a preferable technical scheme, the grapefruit seed in the step S1 is one selected from a grapefruit seed of a marjoram, a grapefruit seed of a Shatian, a grapefruit seed of a honey grapefruit, and a grapefruit seed of a grapefruit; preferably, the grapefruit seed in the step S1 is a marjoe grapefruit seed. The shaddock has a plurality of varieties, but the shaddock has full pulp and high edibility like the four season shaddock, the white shaddock and the like, but has smaller fruit pits, is not beneficial to oil extraction, and cannot ensure to obtain the high-quality shaddock seed extract with high extraction rate of active ingredients. The grapefruit is pear-shaped or oblate, the peel is yellowish green, the sponge tissue in the peel is light red, the mass of Ma Gu grapefruit is 1600-2100 g, the navel is small, the pulp is light red, the juice is thick and sweet, the pulp is tender, the seeds are numerous and full, the number of grapefruit seeds of each grapefruit is 80-120, the inventor finds that the quality of the grapefruit seed extract finally obtained by taking different grapefruit seeds as raw materials is different in actual production application, and the application provides a foundation for obtaining the grapefruit seed extract with high extraction rate and high effective component content by taking the grapefruit seeds as raw materials.
As a preferable technical solution, the preprocessing in step S1 specifically includes: the method comprises the steps of rolling and cleaning the waste grapefruit seeds with clear water for 2-3 times, naturally drying in the sun, drying in an oven at 50-60 ℃ for 20-40min, cleaning and drying the grapefruit seeds, and avoiding the influence of impurities carried in raw materials on the subsequent extraction efficiency and the quality of the extract.
As a preferable technical scheme, the fineness of the crushed grapefruit seeds in the step S2 is 300-400 meshes; the inventor finds that the crushing fineness of the grapefruit seeds influences the saponification reaction efficiency of oleic acid and oleic glyceride in the grapefruit seeds in the subsequent saponification process, and further influences the extraction rate and the extraction efficiency of the grapefruit seed extract, and the inventor ensures higher extraction rate and extraction efficiency by crushing the grapefruit seeds to 300-400 meshes, improves the content of oleic acid and oleic glyceride in the grapefruit seed extract, and the inventor speculates that the reason is probably that the grapefruit seeds have high surface area under the fineness, the active ingredients in the grapefruit seed extract fully contact and react with alkaline solution, so that the subsequent saponification reaction efficiency is improved, the release of oleic acid and oleic glyceride in the grapefruit seeds is promoted, and the extraction efficiency, the extraction rate and the extraction effect of the plant extract are ensured.
As a preferable technical scheme, in the step S3, the mass ratio of the alkaline solution to the grapefruit seed is (6-8): (0.8-1.2);
As a preferable technical scheme, the alkaline solution in the step S3 is sodium hydroxide aqueous solution, and the mass concentration of the sodium hydroxide aqueous solution is 1.5-4%;
As a preferable technical scheme, the saponification reaction in the step S3 is performed under the following conditions: controlling the temperature to be 70-80 ℃, stirring the materials at the stirring speed of 100-150 rpm, wherein the stirring mode is paddle stirring or spiral stirring, and the stirring time is 100-150min;
In the actual extraction and exploration process, the inventor simultaneously meets the requirements of economy, environmental protection and high product quality for realizing large-scale industrial production by controlling the mass ratio of alkaline solution to grapefruit seeds in the saponification process to be (6-8): (0.8-1.2), on the premise of ensuring the extraction effect, the raw material cost and the post-treatment cost caused by excessive use of the alkaline solution are reduced, and the economy is improved; in addition, the inventor finds that in the process of carrying out saponification reaction by adopting a sodium hydroxide aqueous solution with the mass concentration of 1.5-4%, the uniformity degree of the saponification reaction influences the content of oleic acid and oleic glyceride in the grapefruit seed extract, and the inventor has proved that the inventor can ensure that the saponification reaction is complete when the temperature of the saponification reaction is controlled to be 70-80 ℃ and the rotating speed is 100-150 rpm and the stirring is continuously carried out for 100-150min, so that the grapefruit seed extract contains more oleic acid and oleic glyceride on the premise of not influencing the extraction rate of the grapefruit seed extract, and the inventor speculates that the reason is probably that: the temperature of the saponification reaction is increased to accelerate the saponification reaction of oleic acid and oleic acid glyceride and sodium hydroxide, but the temperature is too high to reduce the uniformity of the saponification reaction, the release of oleic acid and oleic acid glyceride in grapefruit seeds is a continuous release process, and the released oleic acid can be fully contacted with sodium hydroxide solution in a system and is subjected to stable and full saponification reaction by controlling the lower rotating speed and stirring for a certain time.
As a preferable technical scheme, the acid solution in the step S4 is an aqueous hydrochloric acid solution, and the mass concentration of the aqueous hydrochloric acid solution is 3-5%;
as a preferable technical scheme, the specific operation conditions of the stirring reaction in the step S4 are as follows: stirring at 20-30deg.C at 30-50 rpm for 50-70min;
As a preferable technical scheme, the environmental temperature of the standing in the step S5 is 60-80 ℃.
The inventor finds that in the actual extraction process, the rotating speed is controlled to be 30-50 revolutions per minute, the hydrochloric acid aqueous solution with the mass concentration of 3-5% is dripped, and after 50-70 minutes of stirring, the complete conversion of oleic acid and oleic glyceride in the system is ensured, and further, the oil-water separation of the system is promoted by controlling the temperature in the subsequent standing separation process to be 60-80 ℃, so that the water content in the grapefruit seed extract is reduced, the content of oleic acid and oleic glyceride in the grapefruit seed extract is improved, and the grapefruit seed extract is better applied to the fields of health foods and cosmetics.
The invention further provides an application of the extraction process of the pomelo leaf extract, which is applied to preparing the pomelo seed extract by treating waste pomelo seeds in the process, and the pomelo seed extract obtained by the process is suitable for the fields of health-care foods and cosmetics.
The beneficial effects are that:
1. The invention provides an extraction process of a grapefruit seed extract, which has the advantages of simple process, high extraction rate and environment friendliness, fully utilizes the waste grapefruit seed resources in grapefruit processing, improves the content of oleic acid and oleic glyceride in the extract on the premise of not influencing the extraction rate, realizes high-value utilization in the fields of health-care foods and cosmetics, and has high practical application value.
2. The invention takes the grapefruit seeds of Malus domestica as raw materials, cleans, dries and pulverizes the grapefruit seeds to 300-400 meshes, ensures higher extraction rate and extraction efficiency, and improves the content of oleic acid and oleic glyceride in the grapefruit seed extract.
3. The mass ratio of the alkaline solution to the grapefruit seeds in the saponification process is controlled to be (6-8): (0.8-1.2), on the premise of ensuring the extraction effect, the raw material cost and the post-treatment cost caused by the excessive use of the alkaline solution are reduced, and the economy is improved, so that the requirements of economy, environmental protection and high product quality for realizing large-scale industrial production are simultaneously met.
4. The invention can ensure the complete saponification reaction by controlling the temperature of the saponification reaction to be 70-80 ℃ and the rotating speed to be 100-150 r/min and continuously stirring for 100-150min, thereby ensuring that the grapefruit seed extract contains more oleic acid and oleic glyceride on the premise of not influencing the extraction rate of the grapefruit seed extract.
5. The extraction process of the grapefruit seed extract provides a high-value utilization method for the waste grapefruit seed resources in grapefruit processing, and avoids the waste of the grapefruit seed resources.
Detailed Description
Example 1
The embodiment 1 of the invention provides an extraction process of a grapefruit seed extract, which comprises the following steps:
s1, preprocessing grapefruit seeds;
s2, placing the cleaned and dried grapefruit seeds into a pulverizer for pulverizing;
s3, placing the crushed grapefruit seeds into a glass container, and adding an alkaline solution with a certain mass for saponification reaction;
S4, carrying out suction filtration on the liquid after the saponification reaction, separating and collecting filtrate, and dripping acid solution with certain mass into the filtrate for stirring reaction;
And S5, standing the liquid after the stirring reaction for 10 hours, retaining upper-layer liquid, and washing the upper-layer liquid with clear water for 5 times to obtain the grapefruit seed extract.
The grapefruit seeds in the step S1 are grapefruit seeds of Malus asiatica.
The preprocessing in the step S1 specifically comprises the following steps: and (3) rolling and cleaning the discarded grapefruit seeds after grapefruit processing with clear water for 3 times, naturally drying in the sun, and then drying in an oven at 50 ℃ for 30min.
The fineness of the crushed grapefruit seeds in the step S2 is 400 meshes.
In the step S3, the mass ratio of the alkaline solution to the grapefruit seeds is 7:1, a step of;
The alkaline solution in the step S3 is sodium hydroxide aqueous solution, and the mass concentration of the sodium hydroxide aqueous solution is 1.8%;
the saponification reaction in the step S3 is performed under the following conditions: the temperature is controlled to be 75 ℃, the stirring rotating speed is 120 revolutions per minute, the stirring mode is spiral stirring, and the stirring time is 120 minutes.
The acid solution in the step S4 is hydrochloric acid aqueous solution, and the mass concentration of the hydrochloric acid aqueous solution is 3.5%;
The specific operation conditions of the stirring reaction in the step S4 are as follows: the stirring temperature is 25 ℃, the stirring rotating speed is 50 revolutions per minute, and the stirring time is 60 minutes.
The ambient temperature at rest in step S5 is 70 ℃.
Example 2
Embodiment 2 of the present invention provides a process for extracting a grapefruit seed extract, comprising the steps of:
s1, preprocessing grapefruit seeds;
s2, placing the cleaned and dried grapefruit seeds into a pulverizer for pulverizing;
s3, placing the crushed grapefruit seeds into a glass container, and adding an alkaline solution with a certain mass for saponification reaction;
S4, carrying out suction filtration on the liquid after the saponification reaction, separating and collecting filtrate, and dripping acid solution with certain mass into the filtrate for stirring reaction;
And S5, standing the liquid after the stirring reaction for 12 hours, retaining upper-layer liquid, and washing the upper-layer liquid with clear water for 5 times to obtain the grapefruit seed extract.
The grapefruit seeds in the step S1 are grapefruit seeds of Malus asiatica.
The preprocessing in the step S1 specifically comprises the following steps: and (3) rolling and cleaning the discarded grapefruit seeds after grapefruit processing with clear water for 3 times, naturally drying in the sun, and then drying in a baking oven at 55 ℃ for 25min.
The fineness of the crushed grapefruit seeds in the step S2 is 400 meshes.
In the step S3, the mass ratio of the alkaline solution to the grapefruit seeds is 6:1, a step of;
The alkaline solution in the step S3 is sodium hydroxide aqueous solution, and the mass concentration of the sodium hydroxide aqueous solution is 2%;
The saponification reaction in the step S3 is performed under the following conditions: the temperature is controlled to be 80 ℃, the stirring rotating speed is 150 revolutions per minute, the stirring mode is paddle stirring, and the stirring time is 100 minutes.
The acid solution in the step S4 is hydrochloric acid aqueous solution, and the mass concentration of the hydrochloric acid aqueous solution is 3.5%;
The specific operation conditions of the stirring reaction in the step S4 are as follows: the stirring temperature is 25 ℃, the stirring rotating speed is 50 revolutions per minute, and the stirring time is 60 minutes.
The ambient temperature at rest in step S5 is 80 ℃.
Example 3
Embodiment 3 of the present invention provides a process for extracting a grapefruit seed extract, comprising the following steps:
s1, preprocessing grapefruit seeds;
s2, placing the cleaned and dried grapefruit seeds into a pulverizer for pulverizing;
s3, placing the crushed grapefruit seeds into a glass container, and adding an alkaline solution with a certain mass for saponification reaction;
S4, carrying out suction filtration on the liquid after the saponification reaction, separating and collecting filtrate, and dripping acid solution with certain mass into the filtrate for stirring reaction;
And S5, standing the liquid after the stirring reaction for 12 hours, retaining upper-layer liquid, and washing the upper-layer liquid with clear water for 5 times to obtain the grapefruit seed extract.
The grapefruit seeds in the step S1 are grapefruit seeds of Malus asiatica.
The preprocessing in the step S1 specifically comprises the following steps: and (3) rolling and cleaning the discarded grapefruit seeds after grapefruit processing with clear water for 3 times, naturally drying in the sun, and then drying in a baking oven at 50 ℃ for 40min.
The fineness of the crushed grapefruit seeds in the step S2 is 300 meshes.
In the step S3, the mass ratio of the alkaline solution to the grapefruit seeds is 8:1.2;
The alkaline solution in the step S3 is sodium hydroxide aqueous solution, and the mass concentration of the sodium hydroxide aqueous solution is 2%;
the saponification reaction in the step S3 is performed under the following conditions: the temperature is controlled to be 70 ℃, the stirring speed is 100 revolutions per minute, the stirring mode is spiral stirring, and the stirring time is 150 minutes.
The acid solution in the step S4 is hydrochloric acid aqueous solution, and the mass concentration of the hydrochloric acid aqueous solution is 4%;
The specific operation conditions of the stirring reaction in the step S4 are as follows: the stirring temperature is 30 ℃, the stirring rotating speed is 40 revolutions per minute, and the stirring time is 50 minutes.
The ambient temperature at rest in step S5 is 70 ℃.
Comparative example 1
Comparative example 1 of the present invention provides a process for extracting grapefruit seed extract, which is different from example 1 in that the fineness of the grapefruit seed after being crushed in step S2 is 100 mesh.
Comparative example 2
Comparative example 2 of the present invention provides a process for extracting grapefruit seed extract, which is different from example 1 in that the saponification reaction in step S3 is performed under the following conditions: the temperature is controlled to be 40 ℃, the stirring rotating speed is 300 revolutions per minute, the stirring mode is paddle stirring, and the stirring time is 60 minutes.
Comparative example 3
Comparative example 3 of the present invention provides an extraction process of grapefruit seed extract, which is different from example 1 in that the ambient temperature of rest in step S5 is 25 ℃.
Performance test method
1. The extraction rate of the grapefruit seed extract obtained by the grapefruit seed extraction process provided in examples and comparative examples was calculated by the formula (extraction rate=extract weight/grapefruit seed weight×100%), with reference to table 1.
2. The content of oleic acid and oleic acid glyceride in the grapefruit seed extracts obtained in examples 1-3 and comparative examples 1-3 was measured by a liquid chromatograph-nuclear magnetic resonance spectrometer, and the results of the performance test are shown in table 1.
Referring to Table 1, table 1 shows the performance test data of grapefruit seeds prepared by specific processes of examples 1 to 3 and comparative examples 1 to 3.
Claims (1)
1. An extraction process of a grapefruit seed extract comprises the following steps:
s1, preprocessing grapefruit seeds;
s2, placing the cleaned and dried grapefruit seeds into a pulverizer for pulverizing;
s3, placing the crushed grapefruit seeds into a glass container, and adding an alkaline solution with a certain mass for saponification reaction;
S4, carrying out suction filtration on the liquid after the saponification reaction, separating and collecting filtrate, and dripping acid solution with certain mass into the filtrate for stirring reaction;
S5, standing the liquid after the stirring reaction for 10 hours, retaining upper-layer liquid, and washing the upper-layer liquid with clear water for 5 times to obtain a grapefruit seed extract;
The grapefruit seeds in the step S1 are grapefruit seeds of Malus pummelo;
the preprocessing in the step S1 specifically comprises the following steps: rolling and cleaning the discarded grapefruit seeds after grapefruit processing with clear water for 3 times, naturally drying in the sun, and drying in a baking oven at 50 ℃ for 30min;
The fineness of the crushed grapefruit seeds in the step S2 is 400 meshes;
In the step S3, the mass ratio of the alkaline solution to the grapefruit seeds is 7:1, a step of;
The alkaline solution in the step S3 is sodium hydroxide aqueous solution, and the mass concentration of the sodium hydroxide aqueous solution is 1.8%;
The saponification reaction in the step S3 is performed under the following conditions: controlling the temperature to be 75 ℃, stirring the mixture at the speed of 120 r/min, and stirring the mixture in a spiral stirring mode for 120min;
the acid solution in the step S4 is hydrochloric acid aqueous solution, and the mass concentration of the hydrochloric acid aqueous solution is 3.5%;
The specific operation conditions of the stirring reaction in the step S4 are as follows: stirring temperature is 25 ℃, stirring rotating speed is 50 revolutions per minute, and stirring time is 60 minutes;
The ambient temperature at rest in step S5 is 70 ℃.
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