CN113577151A - Extraction method of oriental cherry root cell water and application of oriental cherry root cell water - Google Patents
Extraction method of oriental cherry root cell water and application of oriental cherry root cell water Download PDFInfo
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Abstract
The invention discloses a method for extracting sakura root cell water, which organically combines a low-temperature vacuum (reduced pressure) extraction technology with an enzymolysis technology, does not need to add any solvent, firstly carries out primary extraction on sakura roots by the low-temperature vacuum (reduced pressure) technology to obtain primary extracted cell water, adds a certain amount of cellulase and pectinase into the primary extracted cell water, then pours the primary extracted sakura roots residues back to the primary extracted cell water for low-temperature vacuum (reduced pressure) extraction again, and collects the sakura root cell water. The cherry blossom root cell water obtained by the method has high quality, is rich in more than 40 volatile active ingredients, has aromatic and soft smell, is high in safety to human bodies, and has a certain antibacterial effect; has high utilization value, and can be used as green natural raw material in the fields of food, health products, medicines, cosmetics, etc.
Description
Technical Field
The invention relates to the technical field of agricultural product treatment, in particular to an extraction method of oriental cherry root cell water and application of the obtained oriental cherry root cell water.
Background
The flowers of the cherry blossom are bright and bright, and the branches and leaves are luxuriant, so the cherry blossom is an important flower-viewing tree species in early spring and is commonly used for garden appreciation. The flowers, leaves, fruits, roots and the like of the oriental cherry are rich in active ingredients and have high utilization value, so the oriental cherry is a high-value plant resource. At present, in order to realize the development and utilization of comprehensive resources of oriental cherry, the research on flowers, fruits and leaves is mainly focused, and the research on the utilization of oriental cherry roots is less. The invention realizes the utilization of the cherry blossom roots from the direction of extracting the cell water of the cherry blossom roots. At present, no relevant report of extracting cherry blossom root cell water exists.
For the extraction of other plant cell water, the Chinese patent application CN106562908A discloses a method for extracting rose cell water, specifically, the rose is subjected to rotary dry distillation in a rotary evaporator under the conditions of 58-62 ℃ and 0.08-0.10 Mpa, a part of cell sap permeated from the rose is evaporated, condensed, collected and a part of the cell sap is retained in a rotary evaporation bottle and needs to be filtered out; 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. And the plant rootstocks are more difficult to extract than the petals, and the patent method is not suitable for extracting the roots of the oriental cherries.
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 root cell water, which has simple process and high extraction rate; can extract and obtain the oriental cherry root 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 root cell water comprises the following steps: adding no solvent, primarily extracting the cherry blossom roots at the temperature of 30-65 ℃ and under the pressure of-60 kPa to-101 kPa, forming vapor by cherry blossom root cell water, condensing and collecting liquid, extracting for 1.8-2.5 hours to obtain primary extracted cell water and primary extracted cherry blossom root residues, adding 0.2-0.45 percent of cellulase and 0-0.1 percent of pectinase based on the total weight of the primary cherry blossom roots into the primary extracted cell water, then pouring the mixture back into the primary extracted cherry blossom root residues, extracting for 5-7 hours again under the conditions of the temperature of 35-50 ℃ and the pressure of-85 kPa to-101 kPa, and collecting to obtain the cherry blossom root cell water.
The cherry blossom root slices are extracted again for 1-10 mm in thickness, and the extraction of cell water is facilitated.
Under the temperature and pressure conditions, cell water can be well exuded and evaporated out to be condensed and collected, and meanwhile, the loss of volatile active ingredients can be reduced by extracting at a lower temperature. Preferably, the temperature of the primary extraction is 35-50 ℃, and the pressure is-85 kPa-101 kPa.
The method extracts the oriental cherry root residues after adding a certain amount of enzyme into the primary cell extraction water, and 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 roots is too little, and the cell water is difficult to infiltrate the cherry root residues after the enzyme is added, so that the enzymolysis cannot 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.
With respect to the permeability of the water of the cherry blossom root cells, it was found through experimental comparison that when the cherry blossom root residue is extracted by the solvent method, the content of flavone and polysaccharide extracted by the water of the cherry blossom root cells is about 1.6 times that extracted by pure water.
Preferably, the addition amount of the cellulase is 0.25-0.4%, and the addition amount of the pectinase is 0.02-0.06%. The enzyme is macromolecular protein, can be adsorbed on the cell surface of the oriental cherry root residue in the required addition range, is difficult to volatilize under the low-temperature vacuum condition, and does not need subsequent treatment.
The cherry blossom roots are fresh cherry blossom rhizomes which are not mildewed and rotten. The fresh cherry blossom rhizomes are full in moisture, namely, the fresh cherry blossom rhizomes are not treated by means of sun drying or baking and the like.
Stirring is carried out in the extraction process, and the stirring speed is 1-150 revolutions per minute. Local high temperature is prevented, which is beneficial to accelerating the extraction efficiency; and the primary extraction cell water added with the enzyme can be uniformly mixed with the oriental cherry root residues through stirring in the secondary extraction step, and the mixture is fully infiltrated, so that the enzymolysis is ensured.
Condensing in the collecting process, wherein the condensing temperature is-10-8 ℃.
The extraction method of the invention does not need to add other solvents, and 100% of the obtained cherry blossom root cell water is extracted from the cherry blossom roots, thus being green and natural.
The cherry blossom root 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 cherry blossom root cell water is extracted by organically combining a low-temperature vacuum (reduced pressure) technology and an enzymolysis technology, a certain amount of cell water is extracted firstly, then the high permeability of the primary extraction liquid is utilized, the cherry blossom root residue is extracted again after enzyme is added, and the enzymolysis and the low-temperature vacuum (reduced pressure) extraction are carried out simultaneously, so that the cell water extraction efficiency can be accelerated, and the problem of excessive enzymolysis caused by the traditional enzymolysis method is avoided; compared with a single low-temperature-vacuum extraction technology, the extraction rate of cell water is higher, and more volatile active ingredients can be extracted.
The cherry blossom root cell water extracted by the method is light yellow transparent liquid; is rich in more than 40 volatile active ingredients; the smell is fragrant and soft, the safety is high, and a certain antibacterial effect is achieved; 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 root 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.
The examples and comparative examples were conducted by using fresh roots of Kakura japonica (which was not mildewed and not rotten), washing, draining off water, and slicing into 3 to 5mm thick pieces.
Example 1:
putting 50kg of cherry blossom roots into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 45 ℃ under the pressure of-90 kPa, forming vapor by cherry blossom root cell water, condensing and collecting liquid, extracting for 2 hours to obtain primary extracted cell water and primary extracted residues, adding 160g of cellulase and 25g of pectinase into the primary extracted cell water, pouring into the primary extracted residues, and extracting again for 6 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-8 ℃; 36.8kg of cherry blossom root cell water is collected, and the cherry blossom root cell water is light yellow, transparent and fragrant and soft in smell. The cell water yield was 73.6%.
Example 2:
putting 50kg of cherry blossom roots into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 30 ℃ and under the pressure of-100 kPa, forming vapor by cherry blossom root cell water, condensing and collecting liquid, extracting for 2 hours to obtain primary extracted cell water and primary extracted residues, adding 125g of cellulase and 30g of pectinase into the primary extracted cell water, pouring into the primary extracted residues, and extracting for 5 hours again at 35 ℃ and under the pressure of-100 kPa; stirring at 45 r/min in the whole process, and condensing at-8 deg.C; 36.0kg of cherry root flower cell water is collected, and the cherry root flower cell water is light yellow, transparent and fragrant and soft in smell. The cell water yield was 72.0%.
Example 3:
putting 50kg of cherry blossom roots into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 65 ℃ and under the pressure of-75 kPa, forming vapor by cherry blossom root cell water, condensing and collecting liquid, extracting for 1.8 hours to obtain primary extracted cell water and primary extracted residues, adding 175g of cellulase and 20g of pectinase into the primary extracted cell water, pouring into the primary extracted residues, and extracting for 7 hours again at 50 ℃ and under the pressure of-85 kPa; stirring at 60 r/min in the whole process, and condensing at-8 deg.C; 35.4kg of cherry blossom root cell water is collected, and the cherry blossom root cell water is light yellow, transparent and fragrant and soft in smell. The cell water yield was 70.8%.
Example 4:
putting 50kg of cherry blossom roots into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 30 ℃ and under the pressure of-90 kPa, forming vapor by cherry blossom root cell water, condensing and collecting liquid, extracting for 2 hours to obtain primary extracted cell water and primary extracted residues, adding 175g of cellulase and 25g of pectinase into the primary extracted cell water, pouring into the primary extracted residues, and extracting for 5 hours again at 45 ℃ and under the pressure of-90 kPa; stirring the mixture in the whole process at 30 revolutions per minute, and condensing the mixture at-8 ℃; 35.1kg of cherry blossom root cell water is collected, and the cherry blossom root cell water is light yellow, transparent and fragrant and soft in smell. The cell water yield was 70.2%.
Example 5:
putting 50kg of cherry blossom roots into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 45 ℃ under the pressure of-90 kPa, forming vapor by cherry blossom root cell water, condensing and collecting liquid, extracting for 2.5 hours to obtain primary extracted cell water and primary extracted residues, adding 160g of cellulase and 25g of pectinase into the primary extracted cell water, pouring into the primary extracted residues, and extracting for 6 hours again 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-8 ℃; 37.6kg of cherry blossom root cell water is collected, and the cherry blossom root cell water is light yellow, transparent and fragrant and soft in smell. The cell water yield was 75.2%.
Comparative example 1:
putting 50kg of cherry blossom roots into 150L low-temperature extraction equipment, adding no solvent, extracting at 45 ℃, under-90 kPa, condensing and collecting liquid after the cherry blossom root cell water forms steam, extracting for 8 hours, stirring at 30 r/min in the whole process, and condensing at-8 ℃ to obtain 28.7kg of cherry blossom root cell water, which is light yellow, transparent and light in fragrance. The cell water yield was 57.4%.
Comparative example 2:
50kg of cherry blossom roots are put into a 150L low-temperature extraction device, mixed with 5kg of water, 160g of cellulase and 25g of pectinase and stirred for 8 hours at 45 ℃, the stirring speed is 30 r/min, and then filtration is carried out (double filtration: filtration by a centrifuge and then filtration by a 0.22 mu m filter membrane) is finished, so that 40.1kg of cherry blossom root cell water (containing additional 5kg of water) is obtained, the liquid is brownish yellow, slightly turbid, light in fragrance and heavy in peculiar smell. The cell water yield was 70.2% (minus the weight of 5kg water).
Comparative example 3:
putting 50kg of oriental cherry roots into 150L low-temperature extraction equipment, mixing with 5kg of water, 160g of cellulase and 25g of pectinase, stirring for 50 minutes at 45 ℃, extracting for 8 hours at 45 ℃, under-90 kPa, condensing and collecting liquid after oriental cherry root cell water forms steam, stirring for 30 revolutions per minute in the whole process, condensing at-8 ℃, and collecting to obtain 40.8kg of oriental cherry root cell water (containing additionally added 5kg of water), wherein the yellow color is transparent, the fragrance is light, and the taste is foreign. The cell water yield was 71.6%.
Comparative example 4:
putting 50kg of cherry blossom roots into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 45 ℃ under the pressure of-90 kPa, forming vapor by cherry blossom root cell water, condensing and collecting liquid, extracting for 0.5 h to obtain primary extracted cell water and primary extracted residues, adding 160g of cellulase and 25g of pectinase into the primary extracted cell water, pouring into the primary extracted residues, and extracting for 6 h again 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-8 ℃; 32.5kg of cherry blossom root cell water was collected, light yellow, transparent, and slightly fragrant. The cell water yield was 65.0%.
The test methods are as follows:
1. analysis of water volatile active ingredients of oriental cherry root 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 analytical results are shown in Table 4.
2. Cherry blossom root cell water spray anticorrosion challenge test
The cherry blossom root cell water extracted in examples and comparative examples was added to the following spray formulation (see table 1). 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 water of the cherry blossom root cells is changed into deionized water. The test results are shown in Table 4.
Table 1: experimental spray formula
3. Sakura root 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 effect on cell growth was tested with different concentrations of sakura root cell water. The test results are shown in figure 1.
The test results and analysis:
1. the data for the water volatile active ingredient analysis of the cherry blossom root cells of example 1 are provided and are shown in table 2.
Table 2: example 1 analysis of Water volatile active ingredients from cherry root cells (Low match and relative amounts of ingredients not listed)
2. Test data for the water spray preservation challenge for the cherry blossom root cells of example 1 are provided, see table 3.
Table 3: example 1 preservative challenge test results data for oriental cherry root cell water
Through the corrosion prevention challenge test of the spray with the 28-day water agent formula, the spray added with the cherry blossom root cell water in the example 1 passes the corrosion prevention challenge test without adding other preservatives for 7 days, and the cherry blossom root cell water extracted by the method has a certain corrosion prevention effect.
3. The data in FIG. 1 (histogram of water safety test data of cherry blossom root cells in example 1) shows that the water of cherry blossom root cells is basically non-toxic to human body skin cells and has high safety.
4. The process results of the examples and the comparative examples are comprehensively analyzed:
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 root cell water is obtained by firstly carrying out primary extraction on the cherry blossom roots by a low-temperature vacuum (reduced pressure) technology, then using the high permeability of primary extraction cell liquid as an enzymolysis solvent, pouring the enzymolysis solvent back into primary extraction residues and carrying out low-temperature vacuum (reduced pressure) extraction again, is a light yellow transparent solution rich in volatile active ingredients, and has the advantages of corrosion prevention effect and high utilization value. In particular, comparative example 1 employs a single low temperature-vacuum (reduced pressure) extraction technique, with lower extraction yield, fewer components, and a bland flavor. As can be seen from comparative example 2, the cell water obtained by the single enzyme extraction method contains more impurities, has heavy odor and poor corrosion resistance; 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 cherry blossom roots 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 enzymolysis, lower extraction rate compared to example 1, and less content of active ingredient resulted in less flavor.
Claims (8)
1. A method for extracting oriental cherry root cell water is characterized by comprising the following steps: adding no solvent, primarily extracting the cherry blossom roots at the temperature of 30-65 ℃ and under the pressure of-60 kPa to-101 kPa, forming vapor by cherry blossom root cell water, condensing and collecting liquid, extracting for 1.8-2.5 hours to obtain primary extracted cell water and primary extracted cherry blossom root residues, adding 0.2-0.45 percent of cellulase and 0-0.1 percent of pectinase based on the total weight of the primary cherry blossom roots into the primary extracted cell water, then pouring the mixture back into the primary extracted cherry blossom root residues, extracting for 5-7 hours again under the conditions of the temperature of 35-50 ℃ and the pressure of-85 kPa to-101 kPa, and collecting to obtain the cherry blossom root cell water.
2. The method for extracting sakura root cell water according to claim 1, wherein the preliminary extraction temperature is 35 to 50 ℃ and the pressure is-85 to-101 kPa.
3. The method for extracting sakura root cell water according to claim 1, wherein the amount of cellulase added is 0.25% to 0.4%, and the amount of pectinase added is 0.02% to 0.06%.
4. The method for extracting sakura root cell water according to claim 1, wherein stirring is performed at a stirring speed of 1 to 150 rpm during the extraction process.
5. The method for extracting sakura root cell water according to claim 1, wherein condensation is performed during collection at a temperature of-10 ℃ to 8 ℃.
6. The method for extracting sakura root cellular water according to claim 1, wherein the sakura root is not mildewed and not rotten.
7. The method for extracting cherry blossom root cell water as claimed in claim 1, wherein the slice of cherry blossom root is 1-10 mm thick.
8. Use of the sakura root cell water obtained by the extraction method according to any one of claims 1 to 7, in the fields of food, health products, pharmaceuticals and cosmetics.
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| CN109730948A (en) * | 2019-01-24 | 2019-05-10 | 山东贝世康生物科技有限公司 | The method and application of fresh peony flower cellular water are extracted from fresh peony flower |
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| CN109730948A (en) * | 2019-01-24 | 2019-05-10 | 山东贝世康生物科技有限公司 | The method and application of fresh peony flower cellular water are extracted from fresh peony flower |
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