Preparation method of plant hydrolat as well as product and application of plant hydrolat

Abstract

The invention provides a preparation method of plant hydrolat as well as a product and application of the plant hydrolat. The preparation method comprises the following steps: (1) carrying out pulping and wall breaking treatment on plant raw materials to obtain plant pulp; (2) carrying out enzymolysis treatment on the plant pulp to obtain enzymatic hydrolysate; and (3) carrying out distillation treatment on the enzymatic hydrolysate, and collecting distillation condensate to obtain the plant hydrolat. According to the method disclosed by the invention, besides conventional crushing, deep pulping wall breaking and enzymolysis treatment are carried out on the plant raw materials, the plant raw materials can be better dispersed in a solvent through pulping wall breaking, active substances in the plant materials can be fully dissolved out through enzymolysis treatment, and meanwhile, the enzymatic hydrolysate is distilled, so that the yield of the plant materials is increased. The active ingredients can be better carried and extracted, so that the content of the active ingredients of the final product can be increased.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics, and in particular relates to a preparation method of a plant hydrosol, a product thereof and an application thereof. Background Art

[0002] The condensed liquid collected after the flowers, leaves, rhizomes and other materials of plants are extracted through steam distillation is called hydrosol, which contains a small amount of essential oils and other water-soluble substances, such as monoterpene alcohols, organic acids, etc., and does not contain fragrances and alcohol. It has the excellent characteristics of being mild, non-irritating and easily absorbed by the skin, so it is widely used in various skin care products. For example, rose hydrosol has the effects of whitening, moisturizing and anti-wrinkle; jasmine hydrosol can whiten, moisturize and shrink pores; lavender hydrosol is suitable for acne removal and anti-inflammatory.

[0003] Distillation is a method of preparing hydrosols. The specific steps are: add fresh plant materials and distilled water into a distiller in a certain proportion, heat to boiling, use water vapor to carry out plant essential oils and other active ingredients, convert the steam into liquid through a condenser, and then separate and remove the saturated excess essential oils to obtain the corresponding hydrosol.

[0004] CN114032145A discloses a grape seed hydrosol and a preparation method thereof, belonging to the technical field of plant hydrosol extraction. The method comprises the following steps: selecting uniform grape seeds without shrunkenness, washing and drying; freeze-drying the grape seeds; steam distillation: bagging the grape seeds, and after loading an appropriate amount of fragments, tying the bag tightly, putting it into a distillation device, adding deionized water and extraction aids, stirring evenly, heating, and distilling; condensing the mixed gas of the distilled hydrosol and steam, and collecting the condensate; separating the condensate from oil and water, separating the lower layer of hydrosol from the upper layer of essential oil, and obtaining a crude hydrosol; storing the crude hydrosol at a low temperature of 2-4° for 24 hours, and then filtering under pressure with a filter device with a pore size of 2 microns to obtain a fine hydrosol; thermally sterilizing the fine hydrosol; filling in a sterile environment to obtain a grape seed hydrosol.

[0005] CN112156049A discloses a plant hydrosol and a preparation method thereof, comprising the following steps: S1 processing raw materials; S2 water vapor distillation; S3 collecting condensate; S4 oil-water separation; S5 ultrafiltration of crude hydrosol; S6 sterilization; S7 mixing; S8 filling and delivery. The plant hydrosol prepared by the invention has a high essential oil content, has a good moisturizing effect on the skin after use, can improve skin closure, shrink pores, and improve skin fineness.

[0006] However, there are two major defects in the above-mentioned traditional hydrosol preparation process: long-term high-temperature boiling can easily cause some active substances to denature and become ineffective; the extraction efficiency of water vapor on plant materials is low, resulting in a low content of active substances in the hydrosol, which is difficult to meet the efficacy requirements. Therefore, it is of great significance to provide a process method for increasing the content of active ingredients in the hydrosol. Summary of the invention

[0007] In view of the deficiencies in the prior art, the object of the present invention is to provide a method for preparing a plant hydrosol, a product thereof and an application thereof.

[0008] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides a method for preparing a plant hydrosol, the preparation method comprising:

[0010] (1) beating and breaking the plant raw materials to obtain plant slurry;

[0011] (2) subjecting the plant slurry to enzymatic hydrolysis to obtain an enzymatic hydrolyzate;

[0012] (3) The enzymatic hydrolyzate is subjected to distillation treatment, and the distillation condensate is collected to obtain the plant hydrosol.

[0013] The method of the present invention processes plant raw materials by performing deep pulping, wall breaking and enzymatic hydrolysis in addition to conventional crushing, wherein pulping and wall breaking can better disperse the plant raw materials in the solvent, and enzymatic hydrolysis can fully dissolve the active substances in the plant materials. At the same time, the enzymatic hydrolyzate is distilled, and the active ingredients can be better carried and extracted, thereby increasing the active ingredient content of the final product.

[0014] Preferably, the plant material in step (1) includes any one of the flowers, leaves or rhizomes of plants, or a combination of at least two of them.

[0015] Preferably, the plant comprises any one of rose, jasmine, peony, chrysanthemum, bitter orange flower, lavender, Centella asiatica or ginkgo leaf, or a combination of at least two thereof.

[0016] Preferably, the pulping and wall breaking process is carried out in a wall breaking machine.

[0017] Preferably, purified water is added during the pulping and wall breaking process.

[0018] Preferably, the amount of purified water added is 5-10 times the total mass of the plant raw material, for example, 6 times, 7 times, 8 times or 9 times, etc.

[0019] Preferably, the temperature of the enzymatic hydrolysis treatment in step (2) is 40-60°C (for example, it can be 42°C, 44°C, 46°C, 48°C, 50°C, 52°C, 54°C, 56°C or 58°C, etc.), and the time is 20-40min (for example, it can be 22min, 24min, 26min, 28min, 30min, 32min, 34min, 36min or 38min, etc.).

[0020] Preferably, the enzyme used in the enzymatic treatment in step (2) is pectinase and / or cellulase.

[0021] Preferably, the enzyme is added in an amount of 0.05-0.2% of the total mass of the plant raw material, for example, 0.06%, 0.07%, 0.08%, 0.09%, 0.1%, 0.11%, 0.12%, 0.13%, 0.14%, 0.15%, 0.16%, 0.17%, 0.18% or 0.19%, etc.

[0022] Preferably, the enzymes used in the enzymatic treatment are pectinase and cellulase.

[0023] Preferably, the mass ratio of pectinase to cellulase is 1:(1-2), for example, it can be 1:1.1, 1:1.2, 1:1.3, 1:1.4, 1:1.5, 1:1.6, 1:1.7, 1:1.8 or 1:1.9, etc.

[0024] Preferably, the enzymatic hydrolysate is subjected to extraction treatment before the distillation treatment in step (3).

[0025] Preferably, the extraction treatment step is: adding isopropanol to the enzymatic hydrolysate for extraction, and then collecting the extract.

[0026] Preferably, the amount of isopropanol added is 5-10% of the total mass of the enzymatic hydrolysate, for example, it can be 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9% or 9.5%.

[0027] Preferably, the extraction temperature is 70-80°C (for example, 71°C, 73°C, 75°C, 77°C or 79°C, etc.), and the extraction time is 1-2h (for example, 1.1h, 1.3h, 1.5h, 1.7h or 1.9h, etc.).

[0028] Preferably, the distillation temperature in step (3) is 70-80°C, for example, 71°C, 73°C, 75°C, 77°C or 79°C.

[0029] Preferably, the pressure during the distillation is -0.05 to -0.15 MPa, for example, it can be -0.06 MPa, -0.07 MPa, -0.08 MPa, -0.09 MPa, -0.1 MPa, -0.11 MPa, -0.12 MPa, -0.13 MPa or -0.14 MPa.

[0030] Preferably, the temperature of the circulating condensate during the distillation is -10°C to 10°C, for example, -8°C, -6°C, -4°C, -2°C, 0°C, 2°C, 4°C, 6°C or 8°C.

[0031] Any specific point value within the above numerical range can be selected, and will not be described in detail here.

[0032] In a second aspect, the present invention provides a plant hydrosol, which is prepared by the method described in the first aspect.

[0033] In a third aspect, the present invention provides a use of the plant hydrosol as described in the second aspect in the preparation of cosmetics.

[0034] Any specific point value within the above numerical range can be selected, and will not be described in detail here.

[0035] Compared with the prior art, the present invention has the following beneficial effects:

[0036] (1) The method of the present invention processes the plant raw materials by performing deep pulping, wall breaking and enzymatic hydrolysis in addition to conventional crushing, which can make the active ingredients more soluble or dispersed in the solvent, thereby increasing the active ingredient content of the final product.

[0037] (2) The method of the present invention extracts the enzymatic hydrolysate before distillation, that is, isopropanol is added to the liquid to be distilled. At this time, the distillation solvent is not pure water. The boiling point is lowered by forming an azeotrope with isopropanol and water. At the same time, the addition of isopropanol can also enhance the dissolution and evaporation carrying capacity of the active substance.

[0038] (3) In the preparation method of the present invention, negative pressure distillation is used in the distillation process. The negative pressure condition can further reduce the boiling point of the liquid to be distilled, while isolating oxygen to prevent the active ingredients from being oxidized. DETAILED DESCRIPTION

[0039] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0040] The raw materials used in the following examples can be used as long as they are purchased from regular dealers.

[0041] Plant raw materials: Rose, jasmine, peony, Italian immortelle, bitter orange flower, lavender, Centella asiatica, and ginkgo leaf are prepared into plant hydrosols by the methods shown in Examples 1-8 and Comparative Examples 1-2, respectively.

[0042] Example 1

[0043] This embodiment provides a method for preparing a plant hydrosol, the preparation method comprising:

[0044] (1) Take 200 g of fresh plant material and put it into a wall breaking machine, then add 1500 g of pure water for pulping and wall breaking;

[0045] (2) adding 0.2 g of pectinase and 0.2 g of cellulase to the pulp after pulping and breaking, and performing enzymolysis at 50° C. for 30 min to obtain an enzymolysis solution;

[0046] (3) Add 150 g of isopropanol to the enzymatic hydrolysate and stir at 75 °C for 1.5 h;

[0047] (4) distilling the extract at a temperature of 75° C. and a pressure of −0.08 MPa, adjusting the circulating condensate to −10° C., and collecting the distilled condensate to obtain the plant hydrosol.

[0048] Example 2

[0049] This embodiment provides a method for preparing a plant hydrosol, the preparation method comprising:

[0050] (1) Put 200 g of fresh plant material into a wall breaking machine, and then add 1000 g of pure water for pulping and wall breaking;

[0051] (2) adding 0.1 g pectinase and 0.2 g cellulase to the pulp after pulping and breaking, and performing enzymolysis at 40° C. for 40 min to obtain an enzymolysis solution;

[0052] (3) Add 100 g of isopropanol to the enzymatic hydrolysate and stir at 70°C for 2 h;

[0053] (4) distilling the extract at a temperature of 80° C. and a pressure of −0.06 MPa, adjusting the circulating condensate to −5° C., and collecting the distilled condensate to obtain the plant hydrosol.

[0054] Example 3

[0055] This embodiment provides a method for preparing a plant hydrosol, the preparation method comprising:

[0056] (1) Take 200 g of fresh plant material and put it into a wall breaking machine, then add 2000 g of pure water for pulping and wall breaking;

[0057] (2) adding 0.2 g pectinase and 0.1 g cellulase to the pulp after pulping and breaking, and performing enzymolysis at 50° C. for 20 min to obtain an enzymolysis solution;

[0058] (3) Add 200 g of isopropanol to the enzymatic hydrolysate and stir at 80°C for 1 h;

[0059] (4) distilling the extract at a temperature of 70°C and a pressure of -0.1 MPa, adjusting the circulating condensate to 0°C, and collecting the distilled condensate to obtain the plant hydrosol.

[0060] Example 4

[0061] This embodiment provides a method for preparing a plant hydrosol. The difference between the preparation method and Example 1 is that the enzyme used in step (2) is only pectinase, and the total amount of the enzyme is kept unchanged. The remaining steps are consistent with Example 1.

[0062] Example 5

[0063] This embodiment provides a method for preparing a plant hydrosol. The difference between the preparation method and Example 1 is that the enzyme used in step (2) is only cellulase, and the total amount of enzyme is kept unchanged. The remaining steps are consistent with Example 1.

[0064] Example 6

[0065] This embodiment provides a method for preparing a plant hydrosol, the preparation method comprising:

[0066] (1) Take 200 g of fresh plant material and put it into a wall breaking machine, then add 1500 g of pure water for pulping and wall breaking;

[0067] (2) adding 0.2 g of pectinase and 0.2 g of cellulase to the pulp after pulping and breaking, and performing enzymolysis at 50° C. for 30 min to obtain an enzymolysis solution;

[0068] (3) distilling the enzymatic hydrolysate at a temperature of 75° C. and a pressure of −0.08 MPa, adjusting the circulating condensate to −10° C., and collecting the distilled condensate to obtain the plant hydrosol.

[0069] Example 7

[0070] This embodiment provides a method for preparing a plant hydrosol. The difference between the preparation method and Example 1 is that step (3) is to add 150 g of ethanol to the enzymatic hydrolyzate and stir and extract at 75° C. for 1.5 h; the remaining steps are the same as those in Example 1.

[0071] Example 8

[0072] This embodiment provides a method for preparing a plant hydrosol. The difference between the preparation method and Example 1 is that the distillation pressure in step (4) is 0.1 MPa, and the total amount of enzyme is kept unchanged. The remaining steps are consistent with Example 1.

[0073] Comparative Example 1

[0074] This comparative example provides a method for preparing a plant hydrosol, the preparation method comprising:

[0075] (1) Take 200 g of fresh plant material and put it into a wall breaking machine, then add 1500 g of pure water for pulping and wall breaking;

[0076] (2) Add 150 g of isopropanol to the pulp after pulping and extract with stirring at 75° C. for 1.5 h;

[0077] (3) distilling the extract at a temperature of 75° C. and a pressure of −0.08 MPa, modulating the circulating condensate at −10° C., and collecting the distilled condensate to obtain the plant hydrosol.

[0078] Comparative Example 2

[0079] This comparative example provides a method for preparing a plant hydrosol, the preparation method comprising:

[0080] (1) Take 200 g of fresh plant material and cut it into pieces of about 2 cm;

[0081] (2) The fragments were placed in a distiller and 1000 g of pure water was added;

[0082] (3) Raise the temperature of the distiller to boiling and perform distillation extraction. The test temperature is 103°C;

[0083] (4) The circulating condensate was adjusted to -10°C and 500 g of distilled condensate was collected.

[0084] Test Case

[0085] The hydrosols collected in the examples and comparative examples were tested for active substance content using a GC-MS method with the unit being PPM.

[0086] GC-MS conditions:

[0087] Chromatographic conditions: HP-5MS (30m×0.25mm×0.25μm) quartz capillary column for separation; carrier gas was pure helium (99.999%), flow rate 1.2ml / min, no split;

[0088] The mass spectrometry conditions were as follows: the transmission line temperature was 250°C, the ion temperature was 220°C, the electron energy in the EI ionization mode was 70EV, and the mass spectrum range scanned was 45-450amu.

[0089] GC / MS data acquisition was performed on the internal standard sample under the same conditions.

[0090] The results are shown in Table 1.

[0091] Table 1

[0092]

[0093]

[0094] It can be seen from Table 1 that compared with the conventional plant hydrosol preparation method in Comparative Example 2, the plant hydrosols in Examples 1-3 of the present invention have higher levels of active ingredients. This is because the specific method of the present invention can better dissolve the active ingredients in the plant and avoid oxidation of the active ingredients, so the content is higher.

[0095] The contents of each plant hydrosol in Examples 4 and 5 have decreased, indicating that only when the specific enzyme combination of the present invention is used during the enzymatic hydrolysis process can the active ingredients in the plant be more fully dissolved;

[0096] In Example 6, when the enzymatic hydrolysate is not extracted before distillation, the dissolution of the active substance will be significantly reduced, thereby reducing the active ingredient content of the final plant hydrosol;

[0097] In Example 7, when the extraction solvent is not isopropyl alcohol as specifically used in the present invention, the content of active ingredients in the plant hydrosol is also reduced;

[0098] In Example 8, when distillation is performed under normal pressure, the active ingredient may be oxidized, so the active ingredient content of the final plant hydrosol may also decrease;

[0099] In Comparative Example 1, when no enzymatic hydrolysis treatment is performed, the active substances in the plant material cannot be fully dissolved, thereby reducing the active ingredient content of the final plant hydrosol.

[0100] The applicant declares that the present invention illustrates the preparation method of a plant hydrosol of the present invention and its product and application through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0101] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0102] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A method for preparing a plant hydrosol, characterized in that: The preparation method comprises: (1) beating and breaking the plant raw materials to obtain plant slurry; (2) subjecting the plant slurry to enzymatic hydrolysis to obtain an enzymatic hydrolyzate; (3) The enzymatic hydrolyzate is subjected to distillation treatment, and the distillation condensate is collected to obtain the plant hydrosol.

2. The method for preparing the plant hydrosol according to claim 1, characterized in that: The plant material in step (1) includes any one of the flowers, leaves or rhizomes of a plant, or a combination of at least two of them; Preferably, the plant comprises any one of rose, jasmine, peony, chrysanthemum, bitter orange flower, lavender, Centella asiatica or ginkgo leaf, or a combination of at least two thereof.

3. The method for preparing the plant hydrosol according to claim 1 or 2, characterized in that: The beating and wall breaking process is carried out in a wall breaking machine; Preferably, purified water is added during the pulping and wall breaking process; Preferably, the amount of purified water added is 5-10 times the total mass of the plant raw material.

4. The method for preparing a plant hydrosol according to any one of claims 1 to 3, characterized in that: The temperature of the enzymatic hydrolysis treatment in step (2) is 40-60°C and the time is 20-40min; Preferably, the enzyme used in the enzymatic treatment is pectinase and / or cellulase; Preferably, the enzyme is added in an amount of 0.05-0.2% of the total mass of the plant raw material.

5. The method for preparing the plant hydrosol according to claim 4, characterized in that: The enzymes used in the enzymatic treatment are pectinase and cellulase; Preferably, the mass ratio of pectinase to cellulase is 1:(1-2).

6. The method for preparing the plant hydrosol according to any one of claims 1 to 5, characterized in that: The enzymatic hydrolysate is subjected to extraction treatment before the distillation treatment in step (3); Preferably, the extraction treatment step is: adding isopropanol to the enzymatic hydrolysate for extraction, and then collecting the extract.

7. The method for preparing the plant hydrosol according to claim 6, characterized in that: The amount of isopropanol added is 5-10% of the total mass of the enzymatic hydrolysate; Preferably, the extraction temperature is 70-80°C and the extraction time is 1-2h.

8. The method for preparing the plant hydrosol according to claim 6 or 7, characterized in that: The distillation temperature in step (3) is 70-80°C; Preferably, the pressure during distillation is -0.05 to -0.15 MPa; Preferably, the temperature of the circulating condensate during the distillation is -10°C to 10°C.

9. A plant hydrosol, characterized in that: The plant hydrosol is prepared by the method as described in any one of claims 1-8.

10. Use of the plant hydrosol as claimed in claim 9 in preparing cosmetics.

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