CN108403487B - Preparation process of pine pollen extract - Google Patents
Preparation process of pine pollen extract Download PDFInfo
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- CN108403487B CN108403487B CN201810399729.9A CN201810399729A CN108403487B CN 108403487 B CN108403487 B CN 108403487B CN 201810399729 A CN201810399729 A CN 201810399729A CN 108403487 B CN108403487 B CN 108403487B
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- 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
- A61K8/9755—Gymnosperms [Coniferophyta]
- A61K8/9767—Pinaceae [Pine family], e.g. pine or cedar
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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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
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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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
- 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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Abstract
The invention belongs to the technical field of biology, and particularly relates to a preparation process of a pine pollen extract. The invention provides a pollen pini extraction process which takes caprylic capric triglyceride (GTCC) and polyalcohol or polyalcohol water solution as an extractant, and omits the processes of concentration, drying or blending and the like, so that the extract is a finished product. The extraction process is simple and easy to implement, the cost is low, the loss of the pine pollen raw material is less, the maximum utilization of the raw material is achieved, and the method is suitable for industrial production. The invention adopts caprylic capric triglyceride (GTCC) or polyalcohol with minimum skin irritation, has small irritation to human skin, low sensitization and good compatibility with cosmetic matrix; the pine pollen extract is rich in flavone and oil components, has the effects of whitening, resisting aging, resisting inflammation and resisting bacteria, and is very suitable for being used as an active raw material of cosmetics.
Description
Technical Field
The invention belongs to the technical field of biology, and particularly relates to a preparation process of a pine pollen extract.
Background
The pine pollen is a pollen used as both medicine and food, is a traditional medicinal material which has been used for thousands of years, is rich in more than 200 nutrient components, and is a total nutrient. The pollen flavone and other active components have whitening, anti-aging, antibacterial and anti-inflammatory effects, and are often used in cosmetics.
At present, most of pollen pini extraction methods are pure water extraction, ethanol extraction, enzymolysis extraction and the like, and a final product is obtained by complicated processes such as concentration, drying or blending, and the like, so that the process is complex, the cost is high, the yield is not high, and the method is not suitable for industrial production; in addition, other organic agents which are irritant to the skin may need to be introduced in the process, so that the sensitization risk is greatly increased, and the method is not suitable for being added into cosmetics.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation process of a pine pollen extract, which has the advantages of simple operation, low cost and high yield.
The invention provides a preparation process of a pine pollen extract, which comprises the following steps:
(1) performing wall breaking treatment on pollen Pini to obtain wall-broken pollen Pini;
(2) extracting the wall-broken pine pollen in the step (1) by using an extracting agent to obtain an extracting solution; wherein the extractant is caprylic capric triglyceride, polyhydric alcohol or polyhydric alcohol aqueous solution;
(3) and (3) filtering the extracting solution in the step (2), and passing the obtained filtrate through an organic microporous membrane to obtain the pine pollen extract.
Wherein the pine pollen in the step (1) is one or more of masson pine, Chinese pine, yellow pine, white pine, red pine, black pine or Chinese pine.
In the step (1), the wall breaking treatment is a low-temperature high-speed airflow dry grinding method.
The polyhydric alcohol in the step (2) is 1, 3-butanediol, glycerol or 1, 3-propanediol.
The concentration of the polyhydric alcohol aqueous solution in the step (2) is 1.0 to 99.9 weight percent.
The extraction method in the step (2) is dipping extraction, water bath hot reflux extraction, ultrasonic-assisted water bath hot reflux extraction or microwave-assisted water bath hot reflux extraction.
In the ultrasonic-assisted water bath hot reflux extraction, the ultrasonic frequency is 10-70KHz, and the ultrasonic power is 30-1000W.
In the microwave-assisted water-bath hot reflux extraction, the microwave power is 100-1000W.
In the step (2), the weight ratio of the extracting agent to the wall-broken pine pollen is (1-100): 1; the extraction times are 1-3 times, the extraction temperature is 20-180 deg.C, and the single extraction time is 0.5-10 hr.
In the step (3), the filter paper used for filtration is qualitative filter paper or quantitative filter paper.
In the step (3), the aperture of the organic microporous membrane is 0.22-10 μm.
The invention has the beneficial effects that:
1. the invention provides a pollen pini extraction process which takes caprylic capric triglyceride (GTCC) and polyalcohol or polyalcohol water solution as an extractant, and omits the processes of concentration, drying or blending and the like, so that the extract is a finished product. The extraction process is simple and easy to implement, the cost is low, the loss of the pine pollen raw material is less, the maximum utilization of the raw material is achieved, and the method is suitable for industrial production.
2. The invention adopts caprylic capric triglyceride (GTCC) or polyalcohol with minimum skin irritation, has small irritation to human skin, low sensitization and good compatibility with cosmetic matrix; the pine pollen extract is rich in flavone and oil components, has the effects of whitening, resisting aging, resisting inflammation and resisting bacteria, and is very suitable for being used as an active raw material of cosmetics.
Drawings
FIG. 1 is a diagram illustrating the DPPH free radical scavenging rate of the pollen pini extract prepared in embodiments 1-3 of the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
A preparation process of a pine pollen extract comprises the following steps:
(1) performing wall breaking treatment on pollen Pini to obtain wall-broken pollen Pini;
(2) extracting 5g of the wall-broken pine pollen in the step (1) by using 1, 3-propylene glycol as an extracting agent at a weight ratio of 10:1 in a water bath at 95 ℃ for 3 hours for 2 times to obtain an extracting solution;
(3) filtering the 2 times of extractive solutions in step (2) with slow qualitative filter paper, and passing the obtained filtrate through 5 μm organic microporous membrane to obtain 97.9g pollen Pini extract with flavone content of 0.23mg/m L.
Example 2
A preparation process of a pine pollen extract comprises the following steps:
(1) performing wall breaking treatment on pollen Pini to obtain wall-broken pollen Pini;
(2) taking 5g of the wall-broken pine pollen in the step (1) as an extractant by using a 60 wt% aqueous solution of 1, 3-butanediol as an extractant, extracting for the first time according to the weight ratio of the extractant to the wall-broken pine pollen of 10:1, extracting for the second time according to the weight ratio of the extractant to the wall-broken pine pollen of 8:1, and performing ultrasonic-assisted water bath hot reflux extraction for 2 hours each time at an ultrasonic power of 120W to obtain an extract;
(3) filtering the 2 times of extractive solutions in step (2) with slow qualitative filter paper, passing the obtained filtrate through 0.45 μm organic microporous membrane, adding 0.2 wt% MTI into the obtained filtrate to obtain 87.3g pollen Pini extract with flavone content of 0.43mg/m L.
Example 3
A preparation process of a pine pollen extract comprises the following steps:
(1) performing wall breaking treatment on pollen Pini to obtain wall-broken pollen Pini;
(2) adopting 60 wt% glycerol aqueous solution as an extracting agent, extracting 5g of the wall-broken pine pollen in the step (1) according to the weight ratio of the extracting agent to the wall-broken pine pollen of 10:1, carrying out ultrasonic-assisted water bath hot reflux extraction for 2 times, 2 hours each time and 120W of ultrasonic power to obtain an extracting solution;
(3) filtering the 2 times of extractive solutions in step (2) with slow qualitative filter paper, passing the obtained filtrate through 5 μm organic microporous membrane, adding 0.2 wt% MTI into the obtained filtrate to obtain 96.4g pollen Pini extract with flavone content of 0.26mg/m L.
Stability survey
The pollen pini extracts of the embodiments 1-3 are respectively taken 40g, evenly distributed in four transparent sample bottles, placed in different environments, and observed regularly. The four samples are respectively placed in an indoor sunshine irradiation place for 35 days, a 45 ℃ constant temperature box for 30 days, a-20 ℃ refrigerator freezing chamber for 7 days, a 45 ℃ constant temperature box and a-20 ℃ refrigerator freezing chamber for circulation and placement for 10 days. The state of the pine pollen extract is observed every day, the appearance change is extremely small, and the flavone content is almost unchanged, which indicates that the pine pollen extract has good stability.
Evaluation of anti-aging efficacy
Respectively carrying out DPPH free radical clearance test and human fibroblast survival rate test on the pine pollen extract obtained in the examples 1-3 and the pine pollen extract diluted by 10 times, wherein the DPPH free radical clearance rate is shown in figure 1, and the DPPH free radical clearance rate of the pine pollen extract obtained in the examples 1-3 is shown in the figure 1 sequentially from left to right; the relative survival rate of human fibroblasts is used as an evaluation index, and specific data are shown in table 1.
TABLE 1
Evaluation of whitening efficacy
Table 2 shows the effect of the samples on the amount of melanin in B16 cells, and Table 3 shows the effect of the samples on the amount of tyrosinase activity in B16 cells.
TABLE 2
TABLE 3
As shown in tables 2 and 3, the pine pollen extract has the effects of inhibiting tyrosinase activity and reducing melanin content, and has certain whitening effect.
TABLE 4 relative survival rates of human keratinocytes
As can be seen from the data in table 4, the pine pollen extract has an effect of inhibiting the proliferation of human keratinocytes, and the pine pollen extract has an effect of inhibiting keratinocytes, and may have an effect of softening keratinocytes in the product.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (2)
1. A preparation process of a pine pollen extract is characterized by comprising the following steps:
(1) performing wall breaking treatment on pollen Pini to obtain wall-broken pollen Pini;
(2) taking 5g of the wall-broken pine pollen in the step (1) as an extractant by using a 60 wt% aqueous solution of 1, 3-butanediol as an extractant, extracting for the first time according to the weight ratio of the extractant to the wall-broken pine pollen of 10:1, extracting for the second time according to the weight ratio of the extractant to the wall-broken pine pollen of 8:1, and performing ultrasonic-assisted water bath hot reflux extraction for 2 hours each time at an ultrasonic power of 120W to obtain an extract;
(3) and (3) filtering the 2 times of extracting solutions in the step (2) by slow qualitative filter paper respectively, passing the obtained filtrate through a 0.45 mu m organic microporous membrane, and adding 0.2 wt% of MTI into the obtained filtrate to obtain the pine pollen extract.
2. A preparation process of a pine pollen extract is characterized by comprising the following steps:
(1) performing wall breaking treatment on pollen Pini to obtain wall-broken pollen Pini;
(2) adopting 60 wt% glycerol aqueous solution as an extracting agent, extracting 5g of the wall-broken pine pollen in the step (1) according to the weight ratio of the extracting agent to the wall-broken pine pollen of 10:1, carrying out ultrasonic-assisted water bath hot reflux extraction for 2 times, 2 hours each time and 120W of ultrasonic power to obtain an extracting solution;
(3) and (3) filtering the 2 times of extracting solutions in the step (2) through slow qualitative filter paper respectively, passing the obtained filtrate through a 5-micron organic microporous membrane, and adding 0.2 wt% of MTI into the obtained filtrate to obtain the pine pollen extract.
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| CN111084795A (en) * | 2019-09-12 | 2020-05-01 | 天津芸熙生物技术有限公司 | Preparation process of compound preparation extracted from sandalwood leaves at low temperature |
| CN110787070A (en) * | 2019-10-23 | 2020-02-14 | 云南百叶集生物科技有限公司 | Preparation method of hemp flower and leaf extract, preparation method of hemp flower and leaf extract and microcapsule, microcapsule and cosmetic |
| CN114668784A (en) * | 2022-04-07 | 2022-06-28 | 烟台新时代健康产业有限公司 | Preparation process of pollen pini alcohol extract with ovary protection function |
| CN115414312B (en) * | 2022-09-13 | 2023-06-23 | 延安大学咸阳医院有限公司 | Fermented composition containing pollen Pini extract and its application in skin care product |
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| JP2000109410A (en) * | 1998-10-05 | 2000-04-18 | Yoshio Nakamura | Composition for hair growing agent |
| KR100438855B1 (en) * | 2002-02-28 | 2004-07-05 | 주식회사 바이오리 | Oral anti-acnepreparation containing pine pollen extract |
| CN1215848C (en) * | 2003-04-04 | 2005-08-24 | 靳玉群 | Freeze-dried powder injection made from total flavone of may tree leaf |
| CN100515387C (en) * | 2006-11-20 | 2009-07-22 | 吴桂谦 | Whitening skin-caring composition containing snow lotus |
| US8435541B2 (en) * | 2010-09-02 | 2013-05-07 | Bath & Body Works Brand Management, Inc. | Topical compositions for inhibiting matrix metalloproteases and providing antioxidative activities |
| CN104189024A (en) * | 2014-07-18 | 2014-12-10 | 昆明尔玉商贸有限公司 | Extraction method for pine pollen active substances |
| CN105434482B (en) * | 2015-12-30 | 2019-05-24 | 甘肃省医学科学研究院 | A kind of enrichment method of cedar needles general flavone and its application in antitumor |
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