CN113559025A - Extraction method of cherry blossom cell water and application of obtained cherry blossom cell water - Google Patents
Extraction method of cherry blossom cell water and application of obtained cherry blossom cell water Download PDFInfo
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- A—HUMAN NECESSITIES
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- 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
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- 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
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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- 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
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- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
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Abstract
The invention discloses a method for extracting cherry blossom cell water, which comprises the steps of primarily extracting cherry blossom by a low-temperature-vacuum (reduced pressure) technology without adding any solvent to obtain a part of cherry blossom cell water and primary extraction cherry blossom residues, adding a certain amount of cellulase and pectinase into the primary extraction cherry blossom cell water, then pouring the mixture back into the primary extraction cherry blossom residues, extracting again by the low-temperature-vacuum (reduced pressure) technology, and collecting the obtained cherry blossom cell water. The method has simple process and high extraction rate. The cherry blossom cell water obtained by the method is colorless, clear and transparent, is rich in more than 40 volatile active ingredients, has strong fragrance and high safety, and has certain antibacterial activity; has high utilization value, and can be applied in the fields of food, health products, medicines, cosmetics and the like.
Description
Technical Field
The invention relates to the technical field of agricultural product treatment, in particular to an extraction method of cherry blossom cell water and application of the obtained cherry blossom cell water.
Background
Cherry blossom (scientific name: Cerasus sp.) is a general name for several plants in the genus of cherry of the family Rosaceae. The native oriental cherry has grown in the region of the northern hemisphere temperate zone of Himalayas mountain, all over the world. Flowers usually bloom together with leaves or after leaves in 3 months, and are fragrant and gorgeous. The cherry blossom has a certain medicinal value, contains benzaldehyde, has the effects of inhibiting the generation of cancer cells and preventing the synthesis of cancer cell proteins, and has a certain inhibiting effect on both mould and bacteria; the oriental cherry also contains coumarin, and has various medicinal functions of resisting tumor, resisting blood coagulation, resisting oxidation, etc. The cherry blossom is one of important raw materials of skin care products, is rich in natural vitamin A, B, E and cherry leaf flavone, has the effects of maintaining beauty, keeping young, brightening skin color, and has the effects of shrinking pores, balancing grease, strengthening mucous membrane and promoting sugar metabolism; the cherry blossom enzyme component contained in the acne cream is usually used for removing acne.
The oriental cherry is rich in volatile active ingredients with high application value, but the essential oil product can not be obtained according to the traditional steam distillation method, and although oriental cherry is refined into oriental cherry tender oil by using the three-high fresh extraction technology in the prior art, the operation process is complex, the extraction condition requirement is higher, and the yield is lower. Therefore, the development of a new process suitable for industrial production to extract the oriental cherry extract which can be applied to the field of skin care products has important significance.
Chinese patent application CN106562908A discloses a method for extracting rose cell water, which comprises subjecting rose to rotary dry distillation at 58-62 deg.C and 0.08-0.10 Mpa in a rotary evaporator, condensing and collecting a part of cell liquid permeated from rose, and collecting a part of cell liquid in a rotary evaporation bottle to be filtered; repeating the above steps for 3 times, and collecting all cell water to obtain dried flower. However, the extraction rate of the method is not high, the aromatic substances in the flowers cannot be fully extracted by simply repeating rotary steaming (the obtained dried rose flower has a small fragrance difference with the fresh rose flower, which indicates that most of the aromatic ingredients are still remained in the flowers and cannot be fully extracted), and the content of volatile active ingredients in the obtained rose cell water is not high, and the aroma is insufficient.
The Chinese patent application CN109730948A discloses a method for preparing peony flower cell water by combining an ultrasonic low-temperature rotary steaming method and an enzyme method, which comprises the following steps: firstly, squeezing to obtain juice and residue 1, then carrying out rotary evaporation on the residue 1 to obtain cell water 1 and residue 2, and finally carrying out enzymatic hydrolysis on the residue 2 and then carrying out rotary evaporation to obtain cell water 2. And mixing the juice, the cell water 1 and the cell water 2 to obtain the peony cell water. The method has high extraction efficiency, but has the following defects: (1) the squeezing method is adopted and then mixed with the liquid obtained by the vacuum extraction method, so that polysaccharide, pigment and pungent smell are brought in, and the problems of corrosion prevention and decoloration are caused; (2) the method solves the problem of corrosion resistance by being matched with other plants for distillation at the later stage of the process, but easily changes the original water content and smell of the peony cells, and the quality cannot be controlled in the later-stage production.
Disclosure of Invention
The invention aims to provide a method for extracting cherry blossom cell water, which has simple process and high extraction rate; can extract and obtain cherry blossom cell water which is rich in volatile active ingredients and has high utilization value.
The invention is realized by the following technical scheme:
a method for extracting oriental cherry cell water comprises the following steps: adding no solvent, primarily extracting the oriental cherry at the temperature of 30-65 ℃ and under the pressure of-60 kPa to-101 kPa, forming oriental cherry cell water into steam, condensing and collecting liquid, extracting for 1-2 hours to obtain primary extracted cell water and primary extracted oriental cherry residues, adding 0.2-0.4 percent of cellulase and 0-0.1 percent of pectinase based on the total weight of the primary oriental cherry into the primary extracted cell water, then pouring the mixture into the primary extracted oriental cherry residues, extracting for 4-6 hours again under the conditions of the temperature of 35-50 ℃ and the pressure of-80 kPa to-101 kPa, and collecting the oriental cherry cell water.
Preferably, the temperature of the primary extraction is 35-50 ℃, and the pressure is-80 kPa to-101 kPa. The preferred temperature and pressure are such that the cellular water is better able to seep and evaporate, while retaining the activity of the volatilized cellular water at lower temperatures.
According to the invention, a certain amount of enzyme is added into the primary cell extraction water, and the primary cell extraction water is put into the container again to extract the oriental cherry residues, so that the method has the following beneficial advantages: firstly, the surface tension of primary extracted cell water is low, and the permeability is good; secondly, the pH of the primary cell extracting water is 3-7, and the pH does not need to be additionally adjusted, so that the enzyme activity is favorably improved; thirdly, the enzymolysis can accelerate the wall breaking; fourth, low temperature vacuum technique. Through the synergy of the four effects, the enzymolysis speed can be controlled at a lower temperature (35-50 ℃), and the cell sap outflow speed is accelerated. The primary extraction cell water poured back into the container is firstly steamed in about the first 1 hour in the secondary extraction step, the enzymolysis speed is high in the period, the enzymolysis time is controlled by the amount of the primary extraction liquid and the technological conditions of secondary extraction (at the moment, the amount of the primary extraction liquid is important, the enzymolysis time is prolonged, the enzymolysis is excessive, the enzymolysis time is shortened, the enzymolysis is insufficient), and the problems that the extracting solution is diluted due to the addition of a large amount of water and the odor is stimulated due to the excessive enzymolysis in the traditional enzymolysis method are solved. Therefore, the primary extraction time is one of the key parameters, if the time is too short, the cell water of the primrose is too little, and the cell water is difficult to infiltrate the cherry residue after the enzyme is added, so that the enzymolysis can not be normally carried out. If the primary extraction time is too long, cell water flows out too much, so that the enzymolysis time is prolonged, and the risk of excessive enzymolysis is brought; and simultaneously, the subsequent extraction efficiency is reduced.
The permeability of the initial extraction cherry blossom cell water is better than that of pure water, and experiments show that when the cherry blossom residues are extracted by a solvent method, more macromolecular substances such as flavone and polysaccharide and volatile active ingredients can be extracted by using the cherry blossom cell water as the solvent than by using the pure water as the solvent; the content of flavone and polysaccharide extracted by cherry blossom cell water is 1.4 times of that extracted by pure water.
Preferably, the addition amount of the cellulase is 0.25-0.35%, and the addition amount of the pectinase is 0.02-0.06%. The enzyme is macromolecular protein, can be adsorbed on the surface of oriental cherry residue cells within the addition range, cannot be volatilized under the low-temperature vacuum condition, and does not need to be subjected to subsequent treatment.
The cherry blossom adopts fresh cherry blossom which is not rotten and mildewed. The petals of the fresh cherry blossom are fresh, tender and full. Generally, fresh flowers picked in the day are extracted, or the fresh flowers are preserved for 2-5 days by using fresh-keeping means such as refrigeration and the like after being picked.
Stirring is carried out in the extraction process, and the stirring speed is 1-150 revolutions per minute. The cherry blossom is uniformly heated, local high temperature is prevented, and the extraction efficiency is accelerated; and the primary extraction cell water added with the enzyme can be uniformly mixed with the cherry blossom residues through stirring in the secondary extraction step, so that all the cherry blossom residues are fully infiltrated, and the enzymolysis is ensured.
Condensing in the collecting process, wherein the condensing temperature is-10-8 ℃.
The extraction method is suitable for extracting the oriental cherry of each variety.
The extraction method of the invention does not need to add other solvents, and 100% of the obtained cherry blossom cell water is extracted from cherry blossom, has high purity, and is green and natural.
The cherry blossom cell water extracted by the method can be applied to the fields of food, health products, medicines and cosmetics.
Compared with the prior art, the invention has the following beneficial effects:
the method extracts the cherry blossom cell water by organically combining a low-temperature vacuum (reduced pressure) technology and an enzymolysis technology, and has simple process and high extraction rate. Compared with a single low-temperature-vacuum (reduced pressure) extraction technology, the extraction rate of cell water is higher, and more volatile active ingredients can be extracted; meanwhile, the problem that the traditional enzymolysis method is easy to carry out enzymolysis excessively so that the extracting solution has foreign flavor is avoided.
The cherry blossom cell water extracted by the method is colorless, clear and transparent; is rich in more than 40 volatile active ingredients; the fragrance is strong, the safety is high, and the antibacterial activity is certain; has high utilization value, and can be applied to the fields of food, health products, medicines, cosmetics and the like.
Drawings
FIG. 1 is a histogram of water safety test data for cherry blossom cells of example 1.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Examples and comparative examples extraction experiments were performed using fresh cherries harvested on the day from Guangdong (petals fresh, tender, full, not rotten, and not mildewed).
Example 1:
putting 50kg of oriental cherry into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 45 ℃ under the pressure of-90 kPa, forming vapor by oriental cherry cell water, condensing and collecting liquid, extracting for 1.5 hours to obtain primary extracted cell water and primary extracted residue, adding 150g of cellulase and 25g of pectinase into the primary extracted cell water, pouring into the primary extracted residue, and extracting again for 5 hours at 45 ℃ under the pressure of-90 kPa; stirring the mixture in the whole process at 30 revolutions per minute, and condensing the mixture at-5 ℃; 35.1kg of cherry blossom cell water is collected, colorless, clear and transparent, and has strong fragrance. The extraction rate was 70.2%.
Example 2:
putting 50kg of oriental cherry into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 30 ℃ and under the pressure of-100 kPa, forming vapor by oriental cherry cell water, condensing and collecting liquid, extracting for 1.5 hours to obtain primary extracted cell water and primary extracted residue, adding 175g of cellulase and 20g of pectinase into the primary extracted cell water, pouring into the primary extracted residue, and extracting again for 4 hours at 50 ℃ and under the pressure of-85 kPa; stirring at 45 r/min in the whole process, and condensing at-5 deg.C; 34.7kg of cherry blossom cell water is collected, colorless, clear and transparent, and has strong fragrance. The extraction rate was 69.4%.
Example 3:
putting 50kg of oriental cherry into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 65 ℃ and under the pressure of-70 kPa, forming vapor by oriental cherry cell water, condensing and collecting liquid, extracting for 1.5 hours to obtain primary extracted cell water and primary extracted residue, adding 125g of cellulase and 30g of pectinase into the primary extracted cell water, pouring into the primary extracted residue, and extracting for 6 hours again at 35 ℃ and under the pressure of-100 kPa; stirring at 60 r/min and condensing at-5 deg.c; 37.3kg of cherry blossom cell water is collected, colorless, clear and transparent, and has strong fragrance. The extraction rate was 74.6%.
Example 4:
putting 50kg of oriental cherry into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 45 ℃ under the pressure of-90 kPa, forming vapor by oriental cherry cell water, condensing and collecting liquid, extracting for 1.8 hours to obtain primary extracted cell water and primary extracted residue, adding 175g of cellulase and 25g of pectinase into the primary extracted cell water, pouring into the primary extracted residue, and extracting again for 5 hours at 45 ℃ under the pressure of-90 kPa; stirring the mixture in the whole process at 30 revolutions per minute, and condensing the mixture at-5 ℃; 35.8kg of cherry blossom cell water is collected, colorless, clear and transparent, and has strong fragrance. The extraction rate was 71.6%.
Example 5:
putting 50kg of oriental cherry into 150L low-temperature extraction equipment, adding no solvent, primarily extracting under 45 ℃ and-90 kPa, allowing oriental cherry cell water to form steam and condensing to collect liquid, extracting for 2 hours to obtain primary extracted cell water and primary extracted residue, adding 150g of cellulase and 25g of pectinase into the primary extracted cell water, pouring into the primary extracted residue, and extracting under 35 ℃ and-100 kPa for 6 hours again; stirring the mixture in the whole process at 30 revolutions per minute, and condensing the mixture at-5 ℃; 37.6kg of cherry blossom cell water is collected, colorless, clear and transparent, and has strong fragrance. The extraction rate was 75.2%.
Comparative example 1:
putting 50kg of cherry blossom into 150L low-temperature extraction equipment, adding no solvent, extracting at 45 deg.C and-90 kPa, condensing the cell water after forming vapor, collecting the liquid, extracting for 6.5 hr, stirring at 30 r/min, and condensing at-5 deg.C to obtain 30.1kg of cherry blossom cell water, wherein the liquid is colorless, clear and transparent, and has light fragrance. The extraction rate was 60.2%.
Comparative example 2:
50kg of cherry blossom is put into a 150L low-temperature extraction device, mixed with 5kg of water, 150g of cellulase and 25g of pectinase and stirred for 6.5 hours at 45 ℃, the stirring speed is 30 r/min, and then filtration is carried out (double filtration: firstly centrifuge filtration and then filtration by adopting a 0.22 mu m filter membrane) is carried out to obtain 38.2kg of cherry blossom cell water (containing additional 5kg of water), the liquid is light yellow, the fragrance is light, and the peculiar smell is heavy. The extraction yield was 66.4% (minus the weight of 5kg water).
Comparative example 3:
putting 50kg of cherry blossom into 150L low temperature extraction equipment, mixing with 5kg of water, 150g of cellulase and 25g of pectinase, stirring for 50 minutes at 45 ℃, extracting for 5 hours at 45 ℃, forming steam by cherry blossom cell water, condensing to collect liquid, stirring for 30 r/min in the whole process, condensing at-5 ℃, collecting to obtain 39.4kg of cherry blossom cell water (containing additionally added 5kg of water), and obtaining the cherry blossom cell water with colorless, clear and transparent effects, light fragrance and foreign flavor. The extraction yield was 68.8% (minus the weight of 5kg water).
Comparative example 4:
putting 50kg of oriental cherry into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 45 ℃ under the pressure of-90 kPa, forming vapor by oriental cherry cell water, condensing and collecting liquid, extracting for 0.5 h to obtain primary extracted cell water and primary extracted residue, adding 150g of cellulase and 25g of pectinase into the primary extracted cell water, pouring into the primary extracted residue, and extracting again for 5 h at 45 ℃ under the pressure of-90 kPa; stirring the mixture in the whole process at 30 revolutions per minute, and condensing the mixture at-5 ℃; 33.6kg of cherry blossom cell water was collected, colorless, clear, transparent, fragrant but not strong enough. The extraction rate was 67.2%.
The test methods are as follows:
1. analysis of water volatile active ingredients of cherry blossom cells: the headspace gas quality was checked at 80 ℃ injection temperature.
(1) Instrument information: agilent 7980A GC; MS 5975C; 50/30 μm CAR/PDMS/DVB extraction fiber head, SUPELCO USA.
(2) GC-MS conditions: the chromatographic column is HP-INNOWAX capillary column (30m × 0.25mm × 0.25 μm); the carrier gas is He, the flow rate is 1mL/min, and the separation ratio is 5: 1; the sample injection temperature is 250 ℃; the temperature raising procedure is that the initial temperature is 40 ℃, the temperature is kept for 5min, the temperature is raised to 250 ℃ at the speed of 8 ℃/min, and the temperature is kept for 5 min.
Mass spectrum conditions: EI ionization source, energy 70 eV; the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, the interface temperature is 250 ℃, and the scanning range is 30-400 m/z.
(3) Sample pretreatment: 5mL of the sample and 1g of NaCl were placed in a 20mL headspace bottle, and the cap was screwed down. After 5min of equilibrium at 80 ℃ in stirring mode, extracting for 5min at 80 ℃ with a solid phase micro-extraction needle, and then resolving for 5min at the sample inlet.
The data of the results of the water volatile active ingredient analysis of the cherry blossom cells of example 1 are provided and are shown in Table 1.
Table 1: EXAMPLE 1 analysis of Water-volatile active ingredients from cherry blossom cells (the matching degree and the relative amounts of the ingredients are low are not shown)
2. Cherry blossom cell water spray corrosion prevention challenge test
The cherry blossom cell water extracted in examples and comparative examples was added to the following spray formulation (see table 2). Inoculating certain amount of bacteria and fungi, and detecting microbial quantity change at intervals of 0 day, 7 days, 14 days, 21 days and 28 days according to the detection method of the microbial preservative efficacy test of United states Pharmacopeia USP32<51 >. Meanwhile, blank control is carried out, and the cherry blossom cell water is changed into deionized water. The test results are shown in Table 4.
Test data for the water spray preservative challenge for cherry blossom cells of example 1 are provided, see table 3.
Table 2: experimental spray formula
| Raw materials | Content (wt.) |
| Butanediol | 2.4％ |
| Betaine | 0.04％ |
| Glycyrrhizic acid dipotassium salt | 0.05％ |
| Soluble proteoglycans | 0.05％ |
| Royal jelly extract | 0.05％ |
| Cherry cell water | Balance of |
| Citric acid | Adjusting pH to 6-7 |
Table 3: example 1 preservative challenge test results data for oriental cherry cell water
3. Sakura cell water safety test
The HaCaT cell is a human immortal epidermal cell line, has cytotoxicity to the HaCaT cell, and can be used as reference data for safety of skin. The normal cells are in vigorous metabolism, succinate dehydrogenase in mitochondria can reduce tetrazolium salt substances into colored crystalline substances and deposit the crystalline substances around the cells, OD values can be read by an enzyme labeling instrument according to the change, and the relative growth condition of the cells can be known by comparing the OD values with a blank control group. The results of the safety test for oriental cherry cell water of example 1 are provided, see figure 1.
The data in figure 1 show that the oriental cherry cell water has no toxicity to human body skin cells and high safety.
Analysis of the process results of the examples and comparative examples:
table 4: examples and comparative examples the main volatile active ingredient content of the extracted sakura cell water and the results of the preservation challenge test
Continuing with Table 4:
compared with the comparative example, the cherry blossom is extracted primarily by a low-temperature vacuum (decompression) technology, the high permeability of primary extraction cell liquid is used as an enzymolysis solvent, the primary extraction residue is poured back, and the obtained cherry blossom cell water is extracted again in a low-temperature vacuum (decompression) mode, so that the extraction rate is high, the obtained cherry blossom cell water is rich in volatile active ingredients, and the utilization value is high. In particular, the comparative example 1 adopts a single low-temperature vacuum extraction technology, has low extraction rate, less components and light fragrance. As can be seen from comparative example 2, the cell water obtained by the single enzyme extraction method contained many impurities, had a heavy odor, and had poor preservation properties; and water is additionally added as an enzymolysis solvent to dilute the extracting solution, and meanwhile, the extracted volatile active ingredients are few, so that the fragrance is light, and the application value is not high. Comparative example 3 enzymolysis is performed on the oriental cherry for a period of time, and then low-temperature-vacuum (reduced pressure) technology is adopted for extraction, so that the problem of foreign flavor caused by excessive enzymolysis can be solved; and water is used as an enzymolysis solvent, and due to poor water permeability and dilution of the extracting solution by additional water, the defects of low extraction rate, light cell water flavor and the like are caused. As can be seen from comparative example 4, since the initial extraction time was too short, the initial extraction cell water was too small, resulting in too low a degree of enzymatic hydrolysis, lower extraction rate compared to example 1, and less active ingredient content resulting in less flavor.
Claims (7)
1. A method for extracting cherry blossom cell water is characterized by comprising the following steps: adding no solvent, primarily extracting the oriental cherry at the temperature of 30-65 ℃ and under the pressure of-60 kPa to-101 kPa, forming oriental cherry cell water into steam, condensing and collecting liquid, extracting for 1-2 hours to obtain primary extracted cell water and primary extracted oriental cherry residues, adding 0.2-0.4 percent of cellulase and 0-0.1 percent of pectinase based on the total weight of the primary oriental cherry into the primary extracted cell water, then pouring the mixture into the primary extracted oriental cherry residues, extracting for 4-6 hours again under the conditions of the temperature of 35-50 ℃ and the pressure of-80 kPa to-101 kPa, and collecting the oriental cherry cell water.
2. The method for extracting sakura cell water according to claim 1, wherein the preliminary extraction temperature is 35 to 50 ℃ and the pressure is-80 to-101 kPa.
3. The method for extracting cherry blossom cell water as claimed in claim 1, wherein the addition amount of cellulase is 0.25-0.35%, and the addition amount of pectinase is 0.01-0.06%.
4. The method for extracting cherry blossom cell water according to claim 1, wherein stirring is performed during the extraction process, and the stirring speed is 1 to 150 rpm.
5. The extraction method of sakura cell water according to claim 1, wherein condensation is performed during collection at a temperature of-10 ℃ to 8 ℃.
6. The method for extracting cherry blossom cellular water as claimed in claim 1, wherein the cherry blossom is not rotted and moldy.
7. Use of the cherry blossom cell water obtained by the extraction method according to any one of claims 1 to 6, characterized in that it is used in the fields of food, health products, pharmaceuticals and cosmetics.
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