CN112472651A - Ginger extract, preparation method and application thereof - Google Patents

Ginger extract, preparation method and application thereof Download PDF

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CN112472651A
CN112472651A CN201910960769.0A CN201910960769A CN112472651A CN 112472651 A CN112472651 A CN 112472651A CN 201910960769 A CN201910960769 A CN 201910960769A CN 112472651 A CN112472651 A CN 112472651A
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ginger
extract
hot water
drying
purified water
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代文豪
孙云起
孙怀庆
聂艳峰
郭朝万
胡露
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Guangdong Marubi Biological Technology Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9794Liliopsida [monocotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/70Biological properties of the composition as a whole
    • A61K2800/72Hypo-allergenic
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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Abstract

The invention discloses a ginger extract, which is an active substance extracted from the following raw materials in parts by weight by adopting a pressurized hot water method: 5-10 parts of ginger root and 0-1 part of ginger leaf, wherein the extraction temperature is 110-200 ℃, and the pressurizing pressure is 1.5-8.5 MPa. The invention adopts a pressurized hot water extraction method to extract the active substances of the ginger, the pressurized hot water reduces the polarity in a subcritical state, and the ginger phenolic substances with smaller polarity can be extracted efficiently, so that no organic solvent is used in the extraction process, the production process is environment-friendly, and the production cost is lower. The obtained rhizoma Zingiberis recens extract has good antioxidant, free radical scavenging, and antiinflammatory effects.

Description

Ginger extract, preparation method and application thereof
Technical Field
The invention relates to a ginger extract, a preparation method and application thereof.
Background
The skin is the largest organ of the human body, and one of the important functions is to provide a protective barrier to the body, which is critical to maintain homeostasis. Oxidative damage is a major cause of skin aging, and reducing the production of free radicals, scavenging aging metabolites, increasing the activity of antioxidant enzymes, and the like are effective means for delaying skin aging. Reactive oxygen species can initiate inflammatory responses through a variety of pathways and form a vicious cycle of oxidative stress-inflammation-oxidative stress-inflammation. Thus, anti-oxidation is an important approach for anti-inflammation. The different functions of the antioxidant are reasonably utilized, and the long-term use can effectively slow down the skin aging speed and achieve the effects of anti-allergy, anti-inflammation and the like. The cosmetic antioxidants are mainly divided into the following 2 types: artificially synthesized antioxidants and natural antioxidants. With the further development of the cosmetic industry and the improvement of the environmental concern of people, the artificially synthesized antioxidants with the defects of environmental pollution, safety problems and the like are gradually eliminated.
Ginger (ginger of fiscinale Roscoe) belongs to Zingiberaceae plants, is native to tropical areas such as China and southeast Asia, and has a long history of cultivation of ginger in China. The effective components of the ginger are researched and reported at home and abroad, and the ginger can be used as medicine and food, and has multiple effects of anticoagulation, antioxidation, antitumor, pressure boosting and heart strengthening, blood fat reducing, atherosclerosis resisting, gastric mucosa protecting, liver and gallbladder protecting, inflammation diminishing, cough relieving, dizziness preventing and vomiting stopping, central nerve inhibiting and the like. The research data show that the bioactivity is mainly determined by gingerol substances which are pungent components in the ginger, is an important compound group with similar functions, is applied to the field of cosmetics, has good antioxidant, free radical scavenging and anti-inflammatory effects, and is a powerful substitute for artificially synthesized antioxidants.
Although more methods for extracting gingerol have been disclosed, there are some drawbacks, resulting in limited applications. For example, patent CN105218333A discloses a method for extracting ginger, which uses a mixture of 95% ethanol and ethylene glycol dimethyl ether for ultrasonic extraction. The disadvantage of organic solvent residue exists; CN104000752A discloses the use of supercritical carbon dioxide extraction, which eliminates solvent residues, but at a higher production cost.
Disclosure of Invention
The invention aims to provide a preparation method of a ginger extract, which is rapid, easy to operate, low in cost and free of organic residues.
In order to solve the technical problems, the invention discloses a ginger extract which is an active substance extracted from the following raw materials in parts by weight by adopting a pressurized hot water method: 5-10 parts of ginger root and 0-1 part of ginger leaf, wherein the extraction temperature is 110-200 ℃, and the pressurizing pressure is 1.5-8.5 MPa.
Thermodynamically, liquid water below the critical values of 374 ℃ and 22MPa is called subcritical water, wherein pressurized hot water specifically means subcritical water above the boiling point of 100 ℃. Compared with the traditional extraction method, the pressurized hot water extraction technology has unique characteristics, and the polarity of water can be effectively changed by changing the extraction temperature and the extraction pressure so as to extract non-polar compounds. At the same time, increasing the pressure also increases the diffusivity of the substance and the penetration of the solvent, thus increasing the yield of the desired extract. The invention adopts a pressurized hot water extraction method to extract the active substances of the ginger, the pressurized hot water reduces the polarity in a subcritical state, and the ginger phenolic substances with smaller polarity can be extracted efficiently, so that no organic solvent is used in the extraction process, the production process is environment-friendly, and the production cost is lower. The obtained rhizoma Zingiberis recens extract has good antioxidant, free radical scavenging, and antiinflammatory effects.
The ginger root and ginger leaf is fresh rhizome and leaf of ginger, and the preferred weight ratio is 9: 1. The ginger root and the ginger leaf are preferably selected in proportion, so that the effect is better.
The ginger extract disclosed by the invention can be prepared by the following steps: a, preparing ginger powder: drying, crushing and sieving fresh raw materials to obtain ginger powder; b, enzymolysis: mixing ginger powder and purified water according to a ratio of 1: 20-80, adjusting the pH value to 3.5-5.5, and mixing alpha-amylase, cellulase, protease and pectinase with the ginger powder according to a ratio of 1: 0.8-1.2: 15-20 by weight, and hydrolyzing at constant temperature of 30-40 ℃ for 30-60 min; c, pressurized hot water extraction: after enzymolysis, supplementing purified water according to the ratio of 1: 40-100 of ginger powder to purified water, and adjusting the pH value to be neutral. Extracting by a pressurized hot water method for 10-40 min, and filtering to obtain a crude extract after extraction is finished; d, ultrafiltration: filtering the crude extractive solution in a roll-type ultrafiltration device capable of intercepting substances with molecular weight of above 900 daltons by cross-flow filtration method under pressure of 0.01MPa to obtain ultrafiltration extractive solution; e, concentration: concentrating the ultrafiltration extractive solution obtained in step d under reduced pressure to obtain concentrated extractive solution; f, nanofiltration and desalination: and e, performing nanofiltration on the concentrated extracting solution in the step e in a nanofiltration device capable of filtering substances with the molecular weight of below 250 daltons under the pressure of 0.01MPa, retaining the retentate, and drying the retentate to obtain the ginger extract.
Preferably, the drying method in the step a is drying in a drying oven at 45 ℃; step b, enzymolysis: mixing ginger powder and purified water according to a ratio of 1:45, adjusting the pH value to 4.5, and mixing alpha-amylase, cellulase, protease and pectinase with the ginger powder 1: adding the raw materials in a weight ratio of 1:1:18, and hydrolyzing for 45min at constant temperature of 35 ℃; step c pressurized hot water extraction: adding purified water at a ratio of 1:60 of ginger powder to purified water, extracting at 165 deg.C under 3.5MP for 20 min; the drying of the retentate from step f is carried out by spray drying.
Before extraction, the cell wall structure of ginger is destroyed by an enzymolysis method, so that active substances can be dissolved out more easily, the extraction time is shortened, and the extraction rate is improved. The preparation process comprises the steps of pressurized hot water extraction and ultrafiltration nanofiltration separation, can effectively remove microorganisms, does not need to additionally add a sterilization process in the final extraction, and reduces the processing steps.
The ginger extract disclosed by the invention can be used as an antioxidant of cosmetics, replaces an artificial antioxidant in the cosmetics, realizes the antioxidant effect, reduces the irritation of products, improves the safety of the products, and has the advantages of being natural, non-toxic, non-irritant, non-allergic to skin and the like.
Detailed Description
The above-mentioned aspects of the present invention will be further described in detail with reference to the following specific examples. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples. Various substitutions and alterations according to the general knowledge and conventional practice in the art are intended to be included within the scope of the present invention without departing from the technical spirit of the present invention as described above.
Example 1
The preparation method of the ginger root extract comprises the following steps:
a. preparing ginger powder: 1kg of fresh rhizome of ginger, cutting into small pieces, drying in a drying oven at 45 ℃ to constant weight, crushing and sieving to obtain ginger powder;
b. pressurized hot water extraction: adding purified water according to the proportion of 1:60 of ginger powder and purified water, and adjusting the pH value to be neutral. Extracting with pressurized hot water at 165 deg.C under 3.5MP for 20min, and filtering to obtain crude extractive solution;
c. and (3) ultrafiltration: filtering the crude extractive solution in a roll-type ultrafiltration device capable of intercepting substances with molecular weight of above 900 daltons by cross-flow filtration method under pressure of 0.01MPa to obtain ultrafiltration extractive solution;
d. concentration: concentrating the ultrafiltration extractive solution obtained in step d under reduced pressure to obtain concentrated extractive solution;
e. nanofiltration and desalination: and e, performing nanofiltration on the concentrated extracting solution in the step e in a nanofiltration device capable of filtering substances with the molecular weight of below 250 daltons under the pressure of 0.01MPa, retaining the retentate, and drying the retentate to obtain the ginger extract.
Example 2
The preparation method of the ginger extract comprises the following steps:
a. preparing ginger powder: 0.83kg of fresh rhizome of ginger, cutting into small pieces, and 0.17kg of fresh leaf of ginger, drying in a drying oven at 45 ℃ to constant weight, crushing, and sieving to obtain ginger powder;
b. enzymolysis: mixing ginger powder and purified water at a ratio of 1:35, adjusting pH to 3.5, adding alpha-amylase, cellulase, protease and pectinase at a weight ratio of 1:0.8:1.2:20 respectively, and hydrolyzing at constant temperature of 35 deg.C for 30 min;
c. pressurized hot water extraction: adding purified water according to the proportion of 1:40 of ginger powder and purified water, and adjusting the pH value to be neutral. Extracting with pressurized hot water at 110 deg.C under 8.5MP for 15min, and filtering to obtain crude extractive solution;
d. and (3) ultrafiltration: filtering the crude extractive solution in a roll-type ultrafiltration device capable of intercepting substances with molecular weight of above 900 daltons by cross-flow filtration method under pressure of 0.01MPa to obtain ultrafiltration extractive solution;
e. concentration: concentrating the ultrafiltration extractive solution obtained in step d under reduced pressure to obtain concentrated extractive solution;
f. nanofiltration and desalination: and e, performing nanofiltration on the concentrated extracting solution in the step e in a nanofiltration device capable of filtering substances with the molecular weight of below 250 daltons under the pressure of 0.01MPa, retaining the retentate, and drying the retentate to obtain the ginger extract.
Example 3
The preparation method of the ginger root extract comprises the following steps:
a. preparing ginger powder: 1.0kg of fresh rhizome of ginger, drying in a drying oven at 45 ℃ to constant weight, crushing and sieving to obtain ginger powder;
b. enzymolysis: mixing ginger powder and purified water at a ratio of 1:45, adjusting pH to 4.5, adding alpha-amylase, cellulase, protease and pectinase at a weight ratio of 1:1:1:18 to the ginger powder, and hydrolyzing at constant temperature of 35 deg.C for 45 min;
c. pressurized hot water extraction: adding purified water according to the proportion of 1:60 of ginger powder and purified water, and adjusting the pH value to be neutral. Extracting with pressurized hot water at 165 deg.C under 3.5MP for 20min, and filtering to obtain crude extractive solution;
d. and (3) ultrafiltration: filtering the crude extractive solution in a roll-type ultrafiltration device capable of intercepting substances with molecular weight of above 900 daltons by cross-flow filtration method under pressure of 0.01MPa to obtain ultrafiltration extractive solution;
e. concentration: concentrating the ultrafiltration extractive solution obtained in step d under reduced pressure to obtain concentrated extractive solution;
f. nanofiltration and desalination: and e, performing nanofiltration on the concentrated extracting solution in the step e in a nanofiltration device capable of filtering substances with the molecular weight of below 250 daltons under the pressure of 0.01MPa, retaining the retentate, and drying the retentate to obtain the ginger extract.
Example 4
The preparation method of the ginger extract comprises the following steps:
a. preparing ginger powder: 0.9kg of fresh rhizome of ginger, cutting into small pieces, and 0.1kg of fresh leaf of ginger, drying in a drying oven at 45 ℃ to constant weight, crushing, and sieving to obtain ginger powder;
b. enzymolysis: mixing ginger powder and purified water at a ratio of 1:45, adjusting pH to 4.5, adding alpha-amylase, cellulase, protease and pectinase at a weight ratio of 1:1:1:18 to the ginger powder, and hydrolyzing at constant temperature of 35 deg.C for 45 min;
c. pressurized hot water extraction: adding purified water according to the proportion of 1:60 of ginger powder and purified water, and adjusting the pH value to be neutral. Extracting with pressurized hot water at 165 deg.C under 3.5MP for 20min, and filtering to obtain crude extractive solution;
d. and (3) ultrafiltration: filtering the crude extractive solution in a roll-type ultrafiltration device capable of intercepting substances with molecular weight of above 900 daltons by cross-flow filtration method under pressure of 0.01MPa to obtain ultrafiltration extractive solution;
e. concentration: concentrating the ultrafiltration extractive solution obtained in step d under reduced pressure to obtain concentrated extractive solution;
f. nanofiltration and desalination: and e, performing nanofiltration on the concentrated extracting solution in the step e in a nanofiltration device capable of filtering substances with the molecular weight of below 250 daltons under the pressure of 0.01MPa, retaining the retentate, and drying the retentate to obtain the ginger extract.
Example 5
The application of the ginger root extract prepared in example 3 in BB cream comprises the following raw materials in parts by mass, and is specifically shown in Table 1.
TABLE 1 BB cream formulation
Figure BDA0002228831820000041
Figure BDA0002228831820000051
Example 6
The ginger extract prepared in example 4 was used in BB cream having the same composition as in example 5, except that the ginger extract prepared in example 4 was used instead of the ginger root extract prepared in example 3.
Example 7
The application of the ginger root extract prepared in example 3 in the emulsion comprises the following raw materials in parts by mass, and is specifically shown in table 2.
TABLE 2 emulsion formulation
Figure BDA0002228831820000052
Figure BDA0002228831820000061
Example 8
The use of the ginger extract prepared in example 4 in an emulsion having the same raw material composition as in example 7, except that the ginger extract prepared in example 4 is used instead of the ginger root extract prepared in example 3.
Comparative example
Comparative example 1 preparation method of ginger root extract: except that the step c is normal pressure hot water extraction: adding purified water according to the proportion of 1:60 of ginger powder and purified water, and adjusting the pH value to be neutral. Extracting with hot water at 165 deg.C for 20min under normal pressure, and filtering to obtain crude extractive solution. The rest of the procedure was the same as in example 3.
Comparative example 2 ginger extract preparation method: except that the step c is normal pressure hot water extraction: adding purified water according to the proportion of 1:60 of ginger powder and purified water, and adjusting the pH value to be neutral. Extracting with hot water at 165 deg.C for 20min under normal pressure, and filtering to obtain crude extractive solution. The rest of the procedure was the same as in example 4.
Comparative example 3 preparation method of ginger root extract: and (c) removing step c by water vapor extraction: adding purified water according to the proportion of 1:60 of ginger powder and purified water, and adjusting the pH value to be neutral. Extracting with vapor for 20min, and filtering to obtain crude extractive solution. The rest of the procedure was the same as in example 3.
Comparative example 4 ginger extract preparation method: and (c) removing step c by water vapor extraction: adding purified water according to the proportion of 1:60 of ginger powder and purified water, and adjusting the pH value to be neutral. Extracting with vapor for 20min, and filtering to obtain crude extractive solution. The rest of the procedure was the same as in example 4.
The test results of the samples prepared in the above examples of the present invention are as follows:
1) DPPH radical neutralization experiments: free radicals are a class of active chemical species with very strong oxidizing power. A large amount of free radicals generated in the body also cause damage to the skin and accelerate aging. DPPH (diphenylbitter acyl radical) is a stable long-life radical, and the ethanol solution of DPPH is dark purple and has strong absorption near 517 nm. In the presence of a free radical scavenger, the degree of decolorization of the DPPH ethanol solution is quantitatively related to the number of electrons it receives due to the decrease in DPPH light absorption by pairing with its single electron, thereby allowing an assessment of the ability of the substance to scavenge free radicals. The experimental method comprises the following steps: 2.0mL of a sample solution of the corresponding extract (prepared with distilled water, pH6.8, ginger extract concentration 1mg/mL) was added to each of the sample tube and the sample control tube, and distilled water was used instead of the negative control tube and the blank control tube. 0.5mL (20mg/100mL) of ethanol DPPH solution was added to the sample tube and the negative control tube. Distilled water was added until the final volume of each tube was 4mL, mixed well, and after standing for 30 minutes, absorbance (Abs) was measured at 517 nm. Calculation of the rate of removal of DPPH radicals:
Figure BDA0002228831820000071
in the formula: t-sample tube Abs; t is0-sample control Abs; c-negative control Abs; c0Blank controls Abs.
The results show that under the test concentration, the scavenging rate of DPPH free radicals of the samples prepared in the examples is more than 50%, which is much higher than that of the samples prepared in the comparative examples, and the anti-oxidation effect is good. Specific results are shown in table 3 below:
TABLE 3 DPPH neutralization of different gingerol extracts
Figure BDA0002228831820000072
Figure BDA0002228831820000081
2) Human skin patch test skin closed patch test: the potential possibility of causing the adverse reaction of human skin by the test substances is detected, 160 social volunteers meeting the requirements are divided into 6 groups with the age of 20-45 years and half of men and women, 20 social volunteers are used for each group, the extracts prepared in the embodiments 1-4 and the cosmetics prepared in the embodiments 5-8 are respectively used according to the groups, and the test samples are respectively taken. 0.020-0.025 g (solid or semisolid) or 0.020-0.025 mL (liquid) is put into a chamber of a spot tester, and the control hole is not treated. The spot test device with the test substance is applied to the back or forearm of the subject with hypoallergenic tape, and is applied to the skin with palm pressure for 24 h. Skin reactions were observed at 30min (after disappearance of the indentation), 24h and 48h after removal of the plaque from the test article, respectively, according to the criteria of table 4.
TABLE 4 skin reaction grading Standard for skin Enclosed Patch test
Figure BDA0002228831820000082
The result proves that the cosmetic provided by the invention has guaranteed safety and does not generate adverse reactions such as skin irritation, sensitization (except people who are easy to be allergic or people who are allergic to the cosmetic) and the like. The specific results are shown in table 5 below:
TABLE 5 skin seal patch test skin reaction results
Figure BDA0002228831820000083
Figure BDA0002228831820000091

Claims (8)

1. The ginger extract is characterized in that the ginger extract is an active substance extracted from the following raw materials in parts by weight by adopting a pressurized hot water method: 5-10 parts of ginger root and 0-1 part of ginger leaf, wherein the extraction temperature is 110-200 ℃, and the pressurizing pressure is 1.5-8.5 MPa.
2. A ginger extract as claimed in claim 1, wherein: the ginger root and the ginger leaf are fresh rhizomes and leaves of the ginger, and the weight ratio is 9: 1.
3. A method of preparing a ginger extract according to claim 1, comprising the steps of:
a, preparing ginger powder: drying, crushing and sieving fresh raw materials to obtain ginger powder;
b, enzymolysis: mixing ginger powder and purified water according to a ratio of 1: 20-80, adjusting the pH value to 3.5-5.5, adding alpha-amylase, cellulase, protease and pectinase according to a weight ratio of 1: 0.8-1.2: 15-20 with the ginger powder respectively, and hydrolyzing at a constant temperature of 30-40 ℃ for 30-60 min;
c, pressurized hot water extraction: after enzymolysis, supplementing purified water according to the ratio of 1: 40-100 of ginger powder to purified water, and adjusting the pH value to be neutral. Extracting by a pressurized hot water method for 10-40 min, and filtering to obtain a crude extract after extraction is finished;
d, ultrafiltration: filtering the crude extractive solution in a roll-type ultrafiltration device capable of intercepting substances with molecular weight of above 900 daltons by cross-flow filtration method under pressure of 0.01MPa to obtain ultrafiltration extractive solution;
e, concentration: concentrating the ultrafiltration extractive solution obtained in step d under reduced pressure to obtain concentrated extractive solution;
f, nanofiltration and desalination: and e, performing nanofiltration on the concentrated extracting solution in the step e in a nanofiltration device capable of filtering substances with the molecular weight of below 250 daltons under the pressure of 0.01MPa, retaining the retentate, and drying the retentate to obtain the ginger extract.
4. The method of preparing a ginger extract according to claim 3, wherein the drying method in the step a is drying in a 45 ℃ drying oven.
5. A method of preparing a ginger extract according to claim 3, wherein the step b of enzymatic hydrolysis: mixing ginger powder and purified water at a ratio of 1:45, adjusting pH to 4.5, adding alpha-amylase, cellulase, protease and pectinase at a weight ratio of 1:1:1:18, and hydrolyzing at constant temperature of 35 deg.C for 45 min.
6. A method of preparing a ginger extract as claimed in claim 3, wherein said step c of pressurized hot water extraction: adding purified water at a ratio of 1:60 of ginger powder to purified water, and extracting at 165 deg.C under 3.5MPa for 20 min.
7. The method of preparing a ginger extract according to claim 3, wherein the step f retentate drying is spray drying.
8. Use of a ginger extract according to claim 1, for an antioxidant in cosmetics.
CN201910960769.0A 2019-10-11 2019-10-11 Ginger extract, preparation method and application thereof Pending CN112472651A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114377101A (en) * 2021-12-20 2022-04-22 冯大洲 Ginger pill and preparation method thereof

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Application publication date: 20210312