CN113439834A - Preparation method of water lily flower cell water and application of water lily flower cell water - Google Patents
Preparation method of water lily flower cell water and application of water lily flower cell water Download PDFInfo
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/06—Enzymes
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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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
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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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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- Polymers & Plastics (AREA)
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- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a preparation method of water lily flower cell water, which combines a low-temperature vacuum extraction technology with an enzymolysis technology, does not need to add any solvent, and can obtain pure natural water lily flower cell water at a lower temperature (30-55 ℃). The water lily flower cell water obtained by the method has high quality, is clear and transparent, contains more than 70 volatile active ingredients, and has fresh and pleasant sweet fragrance. Can be used as green natural raw material in the fields of food, health product, medicine and cosmetic.
Description
Technical Field
The invention relates to the technical field of agricultural product treatment, in particular to a preparation method of water lily flower cell water and application of the water lily flower cell water.
Background
Water lily, perennial aquatic herbs, thick rhizomes, distributed from northeast to Yunnan, west to Xinjiang, korean, japan, india, russia, north america, and the like. Grow in still water bodies such as ponds, lakes and the like. The water body in many parks is cultivated as an ornamental plant, and the rhizome is eaten or brewed with wine and is used as a medicine, so that the infantile chronic infantile convulsion can be treated; the whole grass can be used as green manure. Experimental research shows that the water lily has the function of adsorbing heavy metals. The water lily leachate has a certain inhibition effect on the growth of microcystis aeruginosa and shows an obvious phenomenon of low promotion and high inhibition. According to the analysis of the nutritional components of the water lily, the result shows that the water lily is rich in 17 amino acids, and the water lily protein belongs to high-quality protein. The analysis result also shows that the water lily contains rich VC, flavonoid glycoside and trace element zinc, and the combination of the two has strong lead-removing function. Animal acute toxicity experiments, micronucleus experiments and sperm aberration experiments show that the water lily is a safe and reliable substance without any toxic and side effects. The water lily pollen is rich in nutrition, has the characteristics of completeness, balance, concentration and the like, and is a natural nutrient source with development and utilization prospects.
At the present stage, the main extraction methods of the water lily flower comprise a distillation method, an extraction method and a supercritical carbon dioxide extraction method, wherein the distillation method is long in time consumption and high in energy consumption, and other solvents are added in the other two methods, so that the storage and the use of the water lily flower extract are limited.
Enzymatic methods are also commonly used in the extraction of plant cell sap. 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 enzymolysis on the residue 2 and then carrying out rotary evaporation to obtain cell water 3. And mixing the juice and the cell water 1/2 to obtain the peony cell water with high yield. 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 later stage of the process is matched with other plants for distillation, so that the problem of corrosion resistance is solved, but the original water components and smell of the peony cells are easily changed! The quality of the product cannot be controlled in the later period.
Disclosure of Invention
The invention aims to overcome the technical defects and provide a method for extracting water containing water lily cells, wherein the obtained water lily cells contain more than 70 volatile active ingredients, have fresh and pleasant sweet fragrance and are colorless and transparent liquid.
The invention is realized by the following technical scheme:
a preparation method of water lily flower cell water comprises the following steps: adding no solvent, primarily extracting the water lily flower at the temperature of 30-55 ℃ and under the pressure of-70 kPa to-101 kPa, forming water lily flower cell water into steam, condensing and collecting liquid, and extracting for 1-3 hours to obtain primary extracted cell water and primary extracted water lily flower residue; adding 0.2-0.4% of cellulase and 0-0.1% of pectinase based on the total mass of the water lily flower into primary water, adding the primary water into the primary water lily flower residue, extracting again at 35-50 ℃ under the pressure of-80 kPa to-101 kPa for 3-7 hours, and collecting the water lily flower cell water.
The primary extraction time is one of key parameters, if the time is too short, the extracted water of the water lily cells is too little, and the water of the cells after the enzyme is added is difficult to wet the surface of the water lily, 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 subsequent extraction efficiency is reduced, and the risk of excessive enzymolysis caused by enzymolysis time is increased. The method adds a certain amount of enzyme into the primary cell extraction water, and puts the primary cell extraction water into the container again to extract the water lily flower residues, and has the following 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 ℃) to accelerate the cell sap outflow speed. About the first 1 hour in the re-extraction step, the primary cell water poured back into the container can be steamed off, the enzymolysis speed is accelerated, the enzymolysis time is shortened (at the moment, the amount of the primary liquid is very important, the enzymolysis time is prolonged, and the enzymolysis time is shortened), and the problems that the traditional enzymolysis method needs to add a large amount of water to dilute the cell liquid and the pungent smell caused by excessive enzymolysis is avoided.
Regarding the permeability of the initially extracted liquid, experiments show that when the water lily flower residue is extracted by using cell sap as a solvent of a solvent method, a large amount of macromolecular substances such as flavone and polysaccharide and volatile active ingredients can be brought. Compared with pure water as a solvent, the cell water as the solvent can extract more active ingredients such as flavone and polysaccharide.
Preferably, the temperature of the initial extraction stage is 40-50 ℃, and the pressure is-80 kPa-101 kPa.
Preferably, the re-extraction time is 3.5 hours to 5 hours.
Due to the thinness of the petals of the pythosiphon stamineus, the re-extraction time can be compressed to less than 5 hours.
Stirring is carried out during the extraction process, and the stirring speed is 1-150 revolutions per minute.
Condensing in the collection process, wherein the temperature is-10-8 ℃.
The flos Nymphaeae is selected from flos Nymphaeae petal, and is fresh, mildew-free, and rot-free. Can be fresh flos Nymphaeae in Guangxi Dingxian, and is fresh, tender and succulent, and has no attached impurities after washing. Generally, the water lily can be kept fresh within 7 days after being picked, or the water lily after being subjected to preservative treatment such as freezing and the like can be stored for several months.
The water lily flower cell water obtained by the method is applied to skin care products, foods, health care products and the like. The cell water contains more than 70 volatile active ingredients (mainly through GC-MS), and the high-quality cell water is suitable for high-end and high-added-value applications.
Compared with the prior art, the invention has the following beneficial effects:
the invention firstly extracts a certain amount of cell sap by a low-temperature vacuum extraction technology, then utilizes the high permeability of the primary extracted cell sap, adds enzyme and then extracts the water lily flower residues again. Can accelerate the extraction efficiency of cell water, avoids the problem of excessive enzymolysis caused by the traditional enzymolysis method, and can obtain more active ingredients and more water lily flower cell sap compared with the low-temperature vacuum extraction technology. The water lily flower cell water obtained by the method has high quality: clear and transparent, high-purity, fresh and pleasant sweet fragrance (more than 70 active ingredients), has antioxidant and anti-inflammatory effects, does not need any external preservative, and can also play a self-preservative role. And the water lily flower cells do not contain polysaccharide and flavone, so that the stability is good.
Drawings
FIG. 1: example 1 test result of water safety of human nymphaea tetragona cells.
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 flower petals of the water lily used in the embodiment and the comparative example are fresh and do not mildew, and the extraction experiment is carried out after the flower petals of the water lily are cleaned and drained.
Example 1: putting 50kg of flos Nymphaeae petal into a container, adding no solvent, primarily extracting at 50 deg.C under-100 kPa, condensing flos Nymphaeae cell water to form vapor, collecting liquid (condensation temperature is-5 deg.C), and extracting for 2 hr to obtain primary extracted cell water and primary extracted flos Nymphaeae residue; adding 100g cellulase and 50g pectinase into the primary water, adding the primary water into the primary water, extracting again at 40 deg.C under-90 kPa under stirring at 60 rpm for 4.5 hr, and collecting the water. The weight is 36kg, and the cell sap is clear and transparent, and has fresh and pleasant sweet flavor.
Example 2: putting 50kg of flos Nymphaeae petal into a container, adding no solvent, primarily extracting at 35 deg.C and-90 kPa, condensing flos Nymphaeae cell water to form vapor, collecting liquid (condensation temperature is-5 deg.C), and extracting for 2.5 hr to obtain primary extracted cell water and primary extracted flos Nymphaeae residue; adding 150g cellulase and 30g pectinase into the primary water, adding the primary water into the primary water, extracting again under 40 deg.C and-90 kPa with stirring at 60 r/min for 5 hr, and collecting the water. The weight is 36.8kg, and the cell sap is clear and transparent and has fresh and pleasant sweet flavor.
Example 3: putting 50kg of flos Nymphaeae petal into a container, adding no solvent, primarily extracting at 45 deg.C under-95 kPa, condensing cell water to form vapor, collecting liquid (condensation temperature is-5 deg.C), and extracting for 3 hr to obtain primary extracted cell water and primary extracted flos Nymphaeae residue; adding 120g of cellulase and 40g of pectinase into the primary water, adding the primary water into the primary water, extracting again under 45 ℃ and-90 kPa with stirring at 60 r/min for 6 hours, and collecting the water. The weight is 38.1kg, and the cell sap is clear and transparent and has fresh and pleasant sweet flavor.
Comparative example 1: putting 50kg of flos Nymphaeae petals into a container, extracting at 55 deg.C under-80 kPa without adding any solvent, condensing and collecting liquid after cell water forms vapor, stirring at 60 r/min, and extracting for 6.5 hr to obtain flos Nymphaeae cell water. 35.4kg, clear and transparent, and light sweet flavor.
Comparative example 2: putting 50kg of water lily flower petals into a container, mixing with 5kg of water, 120g of cellulase and 40g of pectinase, stirring for 45 minutes at 50 ℃, extracting at 50 ℃, under the pressure of-100 kPa, condensing water of water lily flower cells after forming steam, collecting liquid (the condensing temperature is-5 ℃), stirring for 60 revolutions per minute in the whole process, extracting for 6 hours, collecting 42.5kg of water lily flower cell water containing cell sap containing 5kg of water, wherein the liquid is light in color and transparent, and the light sweet fragrance is mixed with a little peculiar smell.
Comparative example 3: putting 50kg of flos Nymphaeae petals into a container, mixing with 5kg of water, 200g of cellulase and 80g of pectinase, extracting at 50 ℃, stirring the whole process at 60 r/min, extracting for 6 hours, filtering (double filtering: filtering by a centrifuge and filtering by a 0.22um filter membrane), and collecting to obtain 44.1kg of flos Nymphaeae cell water (the cell sap contains 5kg of water), wherein a small amount of fine objects are suspended in the cell sap and the foreign flavor is heavy.
Analysis of the process results of the examples and comparative examples:
as can be seen from comparative example 1, the weight of the extracted cell sap was low, the components were less, and the smell was weak only by the low-temperature vacuum extraction technique. As can be seen from comparative example 2, compared with the addition of a certain amount of enzyme and water in comparative example 1, the enzymolysis time is increased, not only is 5kg subtracted from the actual extraction amount, but also the cell sap concentration is reduced, and if higher concentration is obtained, distillation purification is needed, which results in the loss of other volatile organic compounds. As can be seen from the comparative example 3, the water lily flower cell water obtained by the enzyme extraction method in the prior art contains a large amount of polysaccharide and flavone and other colored impurities, has heavy peculiar smell, and has low cell sap concentration and low value due to the addition of 5kg of water.
Table 1: detection results of water lily cell sap extracted in examples and comparative examples
The test methods are as follows:
(1) water-lily flower cell water active ingredient analysis: 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.
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.
Table 2: example 1 Water lily flower cell Water active ingredient Table (ingredients of relatively small content and low degree of matching are not listed)
(2) Water lily flower 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.
Example 1 water lily flower cell water safety test results are shown in figure 1.
(3) Example 1 cellular Water Oxidation resistance of Water lily
By DPPH free radical scavenging method, the alcoholic solution is dark purple and has strong absorption near 517nm according to the stable nitrogen free radical existing in DPPH molecules. When the free radical scavenger exists, absorption of single electrons in molecules is gradually disappeared due to pairing, the fading degree and the number of the electrons received form a quantitative relation, and therefore, the antioxidant effect of the free radical scavenging capacity determination sample can be quantitatively analyzed by determining the reduction of the absorbance at the maximum absorption wavelength of 517 nm. The results are shown in the following table.
| Water lily flower cell Water concentration (%) | DPPH clearance/%) |
| 20 | 15 |
| 40 | 21 |
| 50 | 26 |
| 60 | 30 |
| 80 | 46 |
| 100 | 51 |
As can be seen from the data in the table above, the water lily flower cell water has good antioxidant effect.
(4) Example 1 cellular Water anti-inflammatory efficacy of Water lily flowers
The water lily flower cells have more active ingredients in water, wherein the water lily flower cells have more obvious antibacterial and anti-inflammatory ingredients, such as benzyl alcohol, methyl salicylate and the like, so that the anti-inflammatory effect of the water lily flower cells is tested.
Lipopolysaccharide is the main component of gram-negative bacteria cell wall, and can activate macrophage to release various inflammatory cytokines, so Lipopolysaccharide (LPS) is utilized to stimulate mouse mononuclear-macrophage to establish an in vitro inflammatory reaction model, samples are intervened, dexamethasone is used as a positive control, and enzyme-linked immunosorbent assay (ELISA) is adopted to determine the level change of inflammatory factors IL-6 and TNF-alpha, thereby discussing the in vitro anti-inflammatory action of the samples.
The raw water of the water lily flower cells is prepared into different concentrations for testing, and the test results are shown in the following table.
| Water concentration of water lily flower cell | IL-6(pg/mL) | TNF-α(pg/mL) |
| 100％ | 26 | 150 |
| 80％ | 26 | 155 |
| 40％ | 31 | 165 |
| 15％ | 39 | 170 |
| 10％ | 42 | 174 |
| 5％ | 47 | 196 |
| Blank space | 25 | 150 |
| LPS stimulation | 50 | 260 |
| Dexamethasone | 45 | 206 |
From the above table, it can be known that the water lily flower cell water with the concentration of 80% can reduce the IL-6 expression factor to the normal range after the skin is stimulated by LPS, and has obvious anti-inflammatory effect; the water lily flower cell water with 100% concentration can reduce the TNF-alpha expression factor of the skin stimulated by LPS to be within a normal range.
(5) Example 1 Water lily flower cell Water preservation Condition test
The water lily flower cells contain more active ingredients in water, and the storage is very important for preventing the quality of products from being reduced due to fungus reproduction. The physicochemical values and the fungus reproduction of the water lily cells in the example 1 were examined for one month at room temperature, 4 ℃ and under two storage conditions by adding a certain amount of preservative phenoxyethanol.
1) No preservative is added at room temperature
2) No antiseptic at 4 deg.C
3) Adding preservative at room temperature
4) Adding antiseptic at 4 deg.C
From the data, the water lily flower cell water without preservative at room temperature is easy to grow bacteria, the water lily flower cell water without preservative at 4 ℃ has slightly increased conductivity, but the micro-detection is within the standard range, the water lily flower cell water with a certain amount of preservative is stored at room temperature and 4 ℃, the physicochemical data are stable, and the total number of microbial colonies reaches the standard. In conclusion, the conditions of no preservative at 4 ℃, preservative at room temperature and preservative at 4 ℃ are all suitable for the preservation of the water lily cell water, and for the sake of safety, the water lily cell water is recommended to be preserved stably under the condition of adding a certain amount of preservative at room temperature and 4 ℃.
Claims (7)
1. A preparation method of water lily flower cell water is characterized by comprising the following steps: adding no solvent, primarily extracting flos Nymphaeae at 30-55 deg.C under-70 kPa to-101 kPa to form vapor of flos Nymphaeae cell water, condensing to collect liquid, and extracting for 1-3 hr to obtain primary extracted cell water and primary extracted flos Nymphaeae residue; adding 0.2-0.4% of cellulase and 0-0.1% of pectinase which are based on the total mass of the initial water lily flower into the initial water lily flower cell water, then adding the initial water lily flower cell water into the initial water lily flower residue, extracting again under the conditions of 35-50 ℃ and the pressure of-80 kPa to-101 kPa, finishing the extraction for 3-7 hours, and collecting the water lily flower cell water.
2. The method for preparing nymphaea tetragona cell water according to claim 1, wherein the temperature in the initial extraction stage is 40-50 ℃ and the pressure is-80 kPa-101 kPa.
3. The method for preparing nymphaea tetragona cell water according to claim 1, wherein the re-extraction time is 3.5-5 hours.
4. The method for preparing nymphaea tetragona cell water according to claim 1, wherein stirring is performed during the extraction process, and the stirring speed is 1-150 rpm.
5. The method for preparing water lily flower cell water according to claim 1, wherein condensation is performed during collection at-10-8 ℃.
6. The method for preparing nymphaea tetragona cell water according to claim 1, wherein nymphaea tetragona is nymphaea tetragona petal.
7. The use of nymphaea tetragona cell water according to any one of claims 1-6, wherein the nymphaea tetragona cell water is used in skin care products, food products, health care products and the like.
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| CN106562908A (en) * | 2016-11-01 | 2017-04-19 | 新疆天然芳香农业科技有限公司 | Aromatic plant rose cell water extraction method |
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106562908A (en) * | 2016-11-01 | 2017-04-19 | 新疆天然芳香农业科技有限公司 | Aromatic plant rose cell water extraction method |
| CN108315098A (en) * | 2018-03-14 | 2018-07-24 | 海南大学 | A kind of Nymphaea caerulea method of extraction of essential oil and its application |
| 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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