Composition containing tea leaf extract and preparation method thereof

Abstract

The invention relates to a composition containing a tea leaf extract and a preparation method thereof, and belongs to the technical field of cosmetics. According to the composition containing the tea leaf extract and the preparation method of the composition, the inorganic acid is used for extracting old leaves of the southern Kunshan Maotai tea tree, tea residues of the southern Kunshan Maotai tea, stems of the southern Kunshan Maotai tea tree and the like, so that effective components embedded in insoluble substances (such as plant fibers and lignin) are extracted, waste is turned into wealth, plant raw materials are fully utilized, and the production cost is reduced. The components are safe, the production cost of functional cosmetics can be greatly reduced, and the extract has good effects of diminishing inflammation, tendering skin, whitening and removing freckles.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics and relates to a composition containing tea extract and a preparation method thereof. Background Art

[0002] In today's cosmetics industry, consumers are paying more and more attention to the naturalness and safety of products. As people's pursuit of health and beauty continues to improve, cosmetics at this stage are increasingly inclined to add natural plant extracts in the selection of ingredients. Among the many plant extracts, the active ingredients in tea stand out and become the first choice for many cosmetics brands. Tea is rich in a variety of ingredients that are beneficial to the skin, such as tea polyphenols, caffeine, etc., which have antioxidant, anti-inflammatory, moisturizing and other effects, and can bring many benefits to the skin.

[0003] Traditional plant extraction technology uses solvents, such as water, polar and non-polar organic solvents, weak acids (such as acetic acid) and weak bases, to soak plants, heat and extract them, etc., to dissolve the active ingredients in plants. This extraction method can only extract soluble substances with relatively small molecular weight (such as water-soluble and oil-soluble) in plants, while insoluble substances with larger molecular weight (such as plant fibers, lignin, etc.) become residues and are abandoned. However, these insoluble substances still contain a large number of useful monomers, such as sugars, polyphenols and amino acids. Because of this, in the past research on plant extracts, the research, development and application of these active ingredients contained in the insoluble substances were often ignored. Summary of the invention

[0004] The purpose of the present invention is to provide a composition containing tea extract and a preparation method thereof. The present invention utilizes inorganic acid to extract old leaves of Nankunshan Maocha tree, Nankunshan Maocha residue, and stalks of Nankunshan Maocha tree, which is helpful to extract effective components embedded in insoluble substances (such as plant fiber and lignin). Not only is the yield of sugar higher, but the composition of sugar is also simpler, and the selectivity of hydrolysis reaction is also better, so that plant raw materials are fully utilized, and plant extraction efficiency and plant utilization rate are improved; in addition, the effective components extracted by the scheme can act on the compatibility of functional cosmetics, and can synergistically improve the beneficial effects of the products, thereby reducing the use of additives. Not only are the ingredients safe, but the production cost of functional cosmetics can also be greatly reduced, and the extract has good anti-inflammatory, skin rejuvenation, whitening and freckle removal effects.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] A composition containing tea extract, the composition is selected from one or more of Nankunshan raw tea extract, a hydrolyzate composition of Nankunshan raw tea old leaves, a hydrolyzate composition of Nankunshan raw tea stems, a hydrolyzate composition of Nankunshan raw tea residues, a hydrolyzate composition of Yingde black tea, a hydrolyzate composition of Yingde black tea residues, a hydrolyzate composition of Platycladus orientalis leaves, and a hydrolyzate composition of Artemisia argyi.

[0007] Furthermore, the preparation method of the hydrolyzate composition of the Nankunshan raw tea old leaves is:

[0008] The old leaves of the Nankunshan raw tea tree are ground into powder, mixed with 0.1M hydrochloric acid solution at a ratio of 1:70-80g / mL, refluxed at 100-101°C for 8-12h, cooled to room temperature, and filtered with a 400-mesh nylon mesh. Sodium carbonate is added to the filtrate to adjust the pH to 2.5-3.5 to obtain a hydrolyzate composition of the old leaves of the Nankunshan raw tea.

[0009] Furthermore, the preparation method of the hydrolyzate composition of Nankunshan raw tea stems is:

[0010] The stems of the air-dried Nankunshan tea tree are chopped and ground, mixed with 1.0M hydrochloric acid solution at a ratio of 1:70-80g / mL, refluxed at 100-101°C for 8-12h, cooled to room temperature, and filtered with a 400-mesh nylon mesh. Sodium carbonate is added to the filtrate to adjust the pH to 2.5-3.5 to obtain a hydrolyzate composition of the Nankunshan tea stems.

[0011] Furthermore, the preparation method of the hydrolyzate composition of Nankunshan raw tea residue is:

[0012] The Nankunshan raw tea made from normal tender buds and leaves was ground into powder, mixed with pure water at a ratio of 1:70-80 g / mL, refluxed at 100° C. for 20-40 min, cooled to room temperature, and filtered out the liquid with filter paper to obtain Nankunshan raw tea water extract residue, and an equal volume of 15-25wt% acetic acid aqueous solution and the above-mentioned pure water were added to the Nankunshan raw tea water extract residue, refluxed at 100-102° C. for 20-40 min, cooled to room temperature, and filtered out the liquid with filter paper to obtain Nankunshan raw tea acid extract residue, and an equal volume of 92-98wt% ethanol solution and the above-mentioned pure water were added to the Nankunshan raw tea acid extract residue. , reflux at 78-79°C for 20-40min, cool to room temperature, and filter out the liquid with filter paper to obtain Nankunshan raw tea alcohol extraction residue, add 1 / 2 of the above-mentioned pure water volume of 0.1M sulfuric acid solution to the final residue, reflux at 100-101°C for 8-12h, cool to room temperature, and filter with a 400-mesh nylon mesh to obtain a filtrate, add calcium oxide to the above filtrate to adjust the pH to 6.5-7.5, let it stand overnight, filter out the precipitate with filter paper to obtain a filtrate, add acetic acid to the filtrate to adjust the pH to 2.5-3.5, and obtain a hydrolyzate composition of Nankunshan raw tea residue.

[0013] Furthermore, the preparation method of the Yingde black tea hydrolysate composition is:

[0014] The Yingde black tea was ground into powder, mixed with 0.1M hydrochloric acid solution at a ratio of 1:70-80g / mL, refluxed at 100-101°C for 8-12h, cooled to room temperature, and filtered with a 400-mesh nylon mesh. Sodium hydroxide was added to the filtrate to adjust the pH to 2.5-3.5 to obtain a hydrolyzate composition of the Yingde black tea.

[0015] Furthermore, the preparation method of the hydrolyzate composition of Yingde black tea residue is:

[0016] After grinding Yingde black tea, mix it with pure water at a ratio of 1:70-80g / mL, reflux at 100°C for 20-40min, cool to room temperature, filter out the liquid with filter paper to obtain Yingde black tea water extract residue, add 15-25wt% acetic acid aqueous solution with the same volume as the above pure water to the Yingde black tea water extract residue, reflux at 100-102°C for 20-40min, cool to room temperature, filter out the liquid with filter paper to obtain Yingde black tea acid extract residue, add 15-25wt% acetic acid aqueous solution with the same volume as the above pure water to the Yingde black tea acid extract residue A 92-98wt% ethanol solution is prepared, refluxed at 78-79°C for 20-40min, cooled to room temperature, and filtered with filter paper to obtain the Yingde black tea alcohol extraction residue, to the final residue is added 1 / 2 of the volume of the above pure water 0.1M hydrochloric acid solution, refluxed at 100-101°C for 8-12h, cooled to room temperature, and filtered with a 400-mesh nylon mesh to obtain a filtrate, sodium hydroxide is added to the above filtrate to adjust the pH to 2.5-3.5 to obtain a hydrolyzate composition of Yingde black tea residue.

[0017] Furthermore, the preparation method of the hydrolyzate composition of Platycladus orientalis leaves is:

[0018] The Platycladus orientalis leaf powder and 0.1M hydrochloric acid solution are mixed at a ratio of 1:140-160g / mL, refluxed at 100-101°C for 3-7h, cooled to room temperature, and filtered through a 400-mesh nylon mesh. Sodium hydroxide is added to the filtrate to adjust the pH to 6.5-7.5 to obtain a hydrolyzate composition of the Platycladus orientalis leaves.

[0019] Furthermore, the preparation method of the hydrolyzate composition of wormwood is:

[0020] After grinding the mugwort leaves, mix it with 0.1M hydrochloric acid solution at a ratio of 1:140-160g / mL, reflux it at 100-101°C for 3-7h, cool it to room temperature, filter it with a 400-mesh nylon mesh, add sodium hydroxide to the filtrate to adjust the pH to 6.5-7.5, and obtain a hydrolyzate composition of mugwort leaves.

[0021] Beneficial effects of the present invention:

[0022] The present invention utilizes inorganic acid to extract old leaves of Nankun Mountain Tea Tree, Nankun Mountain Tea Residue, and the stems of Nankun Mountain Tea Tree, which helps to extract effective ingredients embedded in insoluble substances (such as plant fiber and lignin). Not only is the sugar yield higher, but the sugar composition is also simpler, and the selectivity of the hydrolysis reaction is also better, thereby making full use of plant raw materials, improving plant extraction efficiency and plant utilization. In addition, the effective ingredients extracted by this solution can be used in the compatibility of functional cosmetics, which can synergistically improve the beneficial effects of the products, thereby reducing the use of additives. Not only are the ingredients safe, but the production cost of functional cosmetics can also be greatly reduced. The extract has good anti-inflammatory, skin rejuvenation, whitening and freckle removal effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to facilitate understanding by those skilled in the art, the present invention is further described below with reference to the accompanying drawings.

[0024] Figure 1 The HPLC spectrum of the composite extract (1) of Nankunshan raw tea and the hydrolyzate composition (2) of Nankunshan raw tea residue in Example 1;

[0025] Figure 2 HPLC spectra of the hydrolyzate composition (1) of Nankunshan raw tea residue, the hydrolyzate composition (2) of Nankunshan raw tea old leaves, and the hydrolyzate composition (3) of Nankunshan raw tea stems in Example 1;

[0026] Figure 3HPLC spectra of the Nankunshan tea extract (1), the hydrolyzate composition of Nankunshan tea residue (2), the hydrolyzate composition of Nankunshan tea old leaves (3), and the hydrolyzate composition of Nankunshan tea stems (4) obtained by ELSD detection in Example 1;

[0027] Figure 4 This is the hydrolysis curve of Nankunshan raw tea residue under the catalysis of 0.1M HCl (the relationship between sugar content and hydrolysis time);

[0028] Figure 5 is the working curve of glucose standard;

[0029] Figure 6 It is the calibration curve for determining sugar content by HPLC;

[0030] Figure 7 The hydrolysis curve of Nankunshan raw tea residue under different sulfuric acid concentrations (the relationship between sugar content and hydrolysis time);

[0031] Figure 8 Comparison of hydrolysis curves of Nankunshan raw tea residue catalyzed by different types and concentrations of acid;

[0032] Fig. 9 Comparison of the composition of sugars in the hydrolysis products of Nankunshan raw tea residue catalyzed by 0.1M HCl (1) and 5% acetic acid (2). DETAILED DESCRIPTION

[0033] In order to further explain the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the specific implementation methods, structures, features and effects of the present invention are described in detail below in conjunction with the accompanying drawings and preferred embodiments.

[0034] Example 1

[0035] A composition containing tea extract, the composition of this embodiment is composed of a Nankunshan raw tea extract, a hydrolyzate composition of Nankunshan raw tea old leaves, a hydrolyzate composition of Nankunshan raw tea stems, and a hydrolyzate composition of Nankunshan raw tea residues in a mass ratio of 1:1:1:1.

[0036] The preparation method of the Camellia sinensis extract of this embodiment is as follows:

[0037] (1) Grinding Nankunshan raw tea for 18 minutes, introducing oxygen at a rate of 2.5 L / min during the grinding process, and then heating and refluxing at 100° C. under the condition that deionized water is introduced with oxygen at a flow rate of 4 L / min, and the mass ratio of Nankunshan raw tea to deionized water is controlled to be 1:100, and the obtained extract is concentrated to 20% of the volume of the original extract by vacuum distillation to obtain a water extract;

[0038] (2) Grinding raw tea from Nankun Mountain for 15 minutes, introducing oxygen at a flow rate of 2 L / min during the grinding process, and then heating and reflux extraction at 110° C. for 2 hours with acetic acid under the condition of introducing oxygen at a flow rate of 2 L / min, controlling the mass ratio of raw tea from Nankun Mountain to acetic acid to be 1:6, and concentrating the obtained extract to 15% of the volume of the original extract by vacuum distillation to obtain an acetic acid extract;

[0039] (3) Grinding raw tea from Nankun Mountain in the dark for 12 minutes, extracting it with ethanol under reflux at 78.3° C. for 2.5 hours in the dark, controlling the mass ratio of raw tea from Nankun Mountain to ethanol to be 1:80, concentrating the extract to 10% of the volume of the original extract, obtaining extract A and tea residues, extracting the tea residues with ethanol under reflux at 78.3° C. for 3 hours under the condition of passing oxygen at a flow rate of 5 L / min, controlling the mass ratio of tea residue to ethanol to be 1:50, concentrating the extract to 15% of the volume of the original extract, obtaining extract B, combining extract A and extract B to obtain ethanol extract;

[0040] (4) The water extract, the acetic acid extract and the ethanol extract are successively added to the mixture of acetic acid, ethanol and deionized water, and the volume ratio of the water extract, the acetic acid extract, the ethanol extract, the acetic acid, the ethanol and the deionized water is controlled to be 5:1:2:3:7:230 to obtain the Nankunshan raw tea extract.

[0041] The preparation method of the hydrolyzate composition of Nankunshan raw tea old leaves in this embodiment is as follows:

[0042] The old leaves of the Nankunshan raw tea tree were ground into powder, mixed with 0.1M hydrochloric acid solution at a ratio of 1:75g / mL, refluxed at 100.3°C for 10 hours, cooled to room temperature, and filtered with a 400-mesh nylon mesh. Sodium carbonate was added to the filtrate to adjust the pH to 3 to obtain a hydrolyzate composition of the old leaves of the Nankunshan raw tea.

[0043] The preparation method of the hydrolyzate composition of Nankunshan raw tea stems in this embodiment is as follows:

[0044] The stems of the air-dried Nankunshan tea tree were chopped and ground, mixed with 1.0M hydrochloric acid solution at a ratio of 1:75g / mL, refluxed at 100.6°C for 10 hours, cooled to room temperature, and filtered through a 400-mesh nylon mesh. Sodium carbonate was added to the filtrate to adjust the pH to 3 to obtain a hydrolyzate composition of the Nankunshan tea stems.

[0045] The preparation method of the hydrolyzate composition of Nankunshan raw tea residue in this embodiment is as follows:

[0046] The Nankunshan raw tea made from normal tender buds and leaves was ground into powder, mixed with pure water at a ratio of 1:75 g / mL, refluxed at 100°C for 30 min, cooled to room temperature, and filtered out the liquid with filter paper to obtain Nankunshan raw tea water extract residue, and a 20 wt % acetic acid aqueous solution having an equal volume to the above-mentioned pure water was added to the Nankunshan raw tea water extract residue, refluxed at 101°C for 30 min, cooled to room temperature, and filtered out the liquid with filter paper to obtain Nankunshan raw tea acid extract residue, and a 95 wt % ethanol solution having an equal volume to the above-mentioned pure water was added to the Nankunshan raw tea acid extract residue, Reflux at 78.2°C for 30 minutes, cool to room temperature, and filter out the liquid with filter paper to obtain Nankunshan raw tea alcohol extraction residue; add 0.1M sulfuric acid solution with 1 / 2 volume of the above pure water to the final residue, reflux at 100.3°C for 8-12 hours, cool to room temperature, and filter with a 400-mesh nylon mesh to obtain a filtrate, add calcium oxide to the above filtrate to adjust the pH to 7, let it stand overnight, filter out the precipitate with filter paper to obtain a filtrate, add acetic acid to the filtrate to adjust the pH to 3, and obtain a hydrolyzate composition of Nankunshan raw tea residue.

[0047] The water extract, acid extract and alcohol extract of Nankunshan raw tea were mixed in a volume ratio of 1:1:1 to obtain a composite extract of Nankunshan raw tea, and 1 mL was filtered through a 0.22 μm pore size filter and injected into HPLC to analyze its composition; and 1 mL of the hydrolyzate composition of Nankunshan raw tea residue in this embodiment was extracted and filtered through a 0.22 μm pore size filter and injected into HPLC to analyze its composition; wherein the detector was a UV detector with a detection wavelength of 275 nm; the HPLC spectra of the composite extract of Nankunshan raw tea and the hydrolyzate composition of Nankunshan raw tea residue were compared as shown in the attached figure. Figure 1 As shown, it can be clearly seen that they have obvious differences: the three main components contained in the hydrolyzate composition of Nankunshan raw tea residue are: Figure 1 (2) At Rt≈6.4min, 9.0min, and 12.0min, none of them appeared in the HPLC chromatogram of the composite extract of Nankunshan raw tea ( Figure 1 (1)), it can be seen that these components come from the hydrolysis of tea insoluble matter (tea residue) and are unique components of tea insoluble matter.

[0048] 1 mL of the hydrolyzate composition of Nankunshan Maocha old leaves, the hydrolyzate composition of Nankunshan Maocha stems and the hydrolyzate composition of Nankunshan Maocha residues were respectively taken, filtered through a 0.22 μm pore size filter and injected into HPLC for composition analysis, wherein the detector was a UV detector with a detection wavelength of 275 nm; the HPLC spectra of the hydrolyzate composition of Nankunshan Maocha old leaves, the hydrolyzate composition of Nankunshan Maocha stems and the hydrolyzate composition of Nankunshan Maocha residues were compared. Figure 2It can be seen that the main components of the three are basically the same, but the relative contents are different. The component at Rt≈12min has the highest content in the stems, followed by the old leaves, and the least in the Nankunshan raw tea residue made from normal young buds and leaves; the component at Rt≈9.0min has similar contents in the old leaves and the Nankunshan raw tea residue made from normal young buds and leaves, but its content in the stems is extremely low and can be almost ignored; the component at Rt≈6.4min has almost the same content in the old leaves, young buds and leaves, and stems.

[0049] The HPLC spectra of the sugar substances contained in the above-obtained Nankunshan tea extract, the hydrolyzate composition of Nankunshan tea old leaves, the hydrolyzate composition of Nankunshan tea stems and the hydrolyzate composition of Nankunshan tea residues were detected by ELSD detector. Figure 3 ,Depend on Figure 3 It can be seen that the component at Rt≈1.54min is the water-soluble Nankunshan raw tea polysaccharide, and the component at Rt≈2.16min is the main sugar obtained by hydrolysis of Nankunshan raw tea residue, which exists in the residue of young buds and leaves, old leaves and stems.

[0050] Example 2

[0051] A composition containing tea extract, the composition of this embodiment is a hydrolyzate composition of Nankunshan raw tea residue.

[0052] The preparation method of the hydrolyzate composition of Nankunshan raw tea residue in this embodiment is as follows:

[0053] The Nankunshan raw tea made from normal young buds and leaves was ground into powder, mixed with pure water at a ratio of 1:75 g / mL, refluxed at 100°C for 30 min, cooled to room temperature, and filtered out the liquid with filter paper to obtain the Nankunshan raw tea water extract residue. A 20 wt % acetic acid aqueous solution having an equal volume to the above-mentioned pure water was added to the Nankunshan raw tea water extract residue, refluxed at 101°C for 30 min, cooled to room temperature, and filtered out the liquid with filter paper to obtain the Nankunshan raw tea acid extract residue. A 95 wt % ethanol solution having an equal volume to the above-mentioned pure water was added to the Nankunshan raw tea acid extract residue. , reflux at 78.2°C for 30 minutes, cool to room temperature, and filter out the liquid with filter paper to obtain Nankunshan raw tea alcohol extraction residue, add 1 / 2 of the above-mentioned pure water volume of 0.1M sulfuric acid solution to the final residue, reflux at 100.3°C for 10 hours, cool to room temperature, and filter with a 400-mesh nylon mesh to obtain a filtrate, add calcium oxide to the above filtrate to adjust the pH to 7, let it stand overnight, and filter out the precipitate with filter paper to obtain a filtrate, add acetic acid to the filtrate to adjust the pH to 3, and obtain a hydrolyzate composition of Nankunshan raw tea residue.

[0054] The sugar yield in the hydrolyzate composition of the Nankunshan raw tea residue treated with 0.1M sulfuric acid solution and 0.1M hydrochloric acid solution was determined by the "phenol-sulfuric acid" method and the HPLC method, and the hydrolysis time was calculated from the moment the liquid began to boil to the moment the heating was stopped. Figure 4 As shown, the results obtained using sulfuric acid solution or hydrochloric acid solution have good consistency. As the hydrolysis time increases, the sugar concentration gradually increases, and the sugar concentration reaches a maximum concentration of about 6 g per liter when the hydrolysis time reaches or exceeds 1000 min.

[0055] Example 3

[0056] A composition containing tea extract, the composition of this embodiment is a hydrolyzate composition of old Nankunshan raw tea leaves.

[0057] The preparation method of the hydrolyzate composition of Nankunshan raw tea old leaves in this embodiment is as follows:

[0058] The old leaves of the Nankunshan raw tea tree were ground into powder, mixed with 0.1M hydrochloric acid solution at a ratio of 1:75g / mL, refluxed at 100.3°C for 10 hours, cooled to room temperature, and filtered with a 400-mesh nylon mesh. Sodium carbonate was added to the filtrate to adjust the pH to 3 to obtain a hydrolyzate composition of the old leaves of the Nankunshan raw tea.

[0059] Example 4

[0060] A composition containing tea extract, the composition of this embodiment is a hydrolyzate composition of Nankunshan raw tea stems.

[0061] The preparation method of the hydrolyzate composition of Nankunshan raw tea stems in this embodiment is as follows:

[0062] The stems of the air-dried Nankunshan tea tree were chopped and ground, mixed with 1.0M hydrochloric acid solution at a ratio of 1:75g / mL, refluxed at 100.6°C for 10 hours, cooled to room temperature, and filtered through a 400-mesh nylon mesh. Sodium carbonate was added to the filtrate to adjust the pH to 3 to obtain a hydrolyzate composition of the Nankunshan tea stems.

[0063] Example 5

[0064] A composition containing tea extract, the composition of this embodiment is a Yingde black tea hydrolyzate composition.

[0065] The preparation method of the hydrolyzate composition of Yingde black tea in this embodiment is:

[0066] The Yingde black tea was ground into powder, mixed with 0.1M hydrochloric acid solution at a ratio of 1:75 g / mL, refluxed at 100.3°C for 10 hours, cooled to room temperature, and filtered through a 400-mesh nylon mesh. Sodium hydroxide was added to the filtrate to adjust the pH to 3, thereby obtaining a hydrolyzate composition of the Yingde black tea.

[0067] Example 6

[0068] A composition containing tea extract is a hydrolyzate composition of Yingde black tea residue.

[0069] The preparation method of the hydrolyzate composition of Yingde black tea residues in this embodiment is as follows:

[0070] After grinding the Yingde black tea, the mixture was mixed with pure water at a ratio of 1:75 g / mL, and the mixture was refluxed at 100° C. for 30 min. After cooling to room temperature, the mixture was filtered out with filter paper to obtain the Yingde black tea water extract residue. A 20 wt % acetic acid aqueous solution having an equal volume to the above-mentioned pure water was added to the Yingde black tea water extract residue, the mixture was refluxed at 101° C. for 30 min. After cooling to room temperature, the mixture was filtered out with filter paper to obtain the Yingde black tea acid extract residue. A 95 wt % ethanol solution having an equal volume to the above-mentioned pure water was added to the Yingde black tea acid extract residue, the mixture was refluxed at 78.2° C. for 30 min. After cooling to room temperature, the mixture was filtered out with filter paper to obtain the Yingde black tea alcohol extract residue. A 0.1 M hydrochloric acid solution having a volume of 1 / 2 of the above-mentioned pure water was added to the final residue, the mixture was refluxed at 100.3° C. for 10 h. After cooling to room temperature, the mixture was filtered out with a 400-mesh nylon mesh to obtain a filtrate. Sodium hydroxide was added to the filtrate to adjust the pH to 3, and a hydrolyzate composition of the Yingde black tea residue was obtained.

[0071] Example 7

[0072] A composition containing tea extract, the composition of this embodiment is composed of a Nankunshan raw tea extract and a hydrolyzate composition of Platycladus orientalis leaves in a mass ratio of 1:1.

[0073] The preparation method of the Camellia sinensis extract of this embodiment is as follows:

[0074] (1) Grinding Nankunshan raw tea for 18 minutes, introducing oxygen at a rate of 2.5 L / min during the grinding process, and then heating and refluxing at 100° C. under the condition that deionized water is introduced with oxygen at a flow rate of 4 L / min, and the mass ratio of Nankunshan raw tea to deionized water is controlled to be 1:100, and the obtained extract is concentrated to 20% of the volume of the original extract by vacuum distillation to obtain a water extract;

[0075] (2) Grinding raw tea from Nankun Mountain for 15 minutes, introducing oxygen at a flow rate of 2 L / min during the grinding process, and then heating and reflux extraction at 110° C. for 2 hours with acetic acid under the condition of introducing oxygen at a flow rate of 2 L / min, controlling the mass ratio of raw tea from Nankun Mountain to acetic acid to be 1:6, and concentrating the obtained extract to 15% of the volume of the original extract by vacuum distillation to obtain an acetic acid extract;

[0076] (3) Grinding raw tea from Nankun Mountain in the dark for 12 minutes, extracting it with ethanol under reflux at 78.3° C. for 2.5 hours in the dark, controlling the mass ratio of raw tea from Nankun Mountain to ethanol to be 1:80, concentrating the extract to 10% of the volume of the original extract, obtaining extract A and tea residues, extracting the tea residues with ethanol under reflux at 78.3° C. for 3 hours under the condition of passing oxygen at a flow rate of 5 L / min, controlling the mass ratio of tea residue to ethanol to be 1:50, concentrating the extract to 15% of the volume of the original extract, obtaining extract B, combining extract A and extract B to obtain ethanol extract;

[0077] (4) The water extract, the acetic acid extract and the ethanol extract are successively added to the mixture of acetic acid, ethanol and deionized water, and the volume ratio of the water extract, the acetic acid extract, the ethanol extract, the acetic acid, the ethanol and the deionized water is controlled to be 5:1:2:3:7:230 to obtain the Nankunshan raw tea extract.

[0078] The preparation method of the hydrolyzate composition of Platycladus orientalis leaves of this embodiment is as follows:

[0079] The Platycladus orientalis leaf powder and 0.1M hydrochloric acid solution were mixed at a ratio of 1:150 g / mL, refluxed at 100.3°C for 5 hours, cooled to room temperature, and filtered through a 400-mesh nylon mesh. Sodium hydroxide was added to the filtrate to adjust the pH to 7 to obtain a hydrolyzate composition of the Platycladus orientalis leaves.

[0080] Example 8

[0081] A composition containing tea extract, the composition of this embodiment is composed of a Nankunshan raw tea extract and a hydrolyzate composition of wormwood in a mass ratio of 1:1.

[0082] The preparation method of the Camellia sinensis extract of this embodiment is as follows:

[0083] (1) Grinding Nankunshan raw tea for 18 minutes, introducing oxygen at a rate of 2.5 L / min during the grinding process, and then heating and refluxing at 100° C. under the condition that deionized water is introduced with oxygen at a flow rate of 4 L / min, and the mass ratio of Nankunshan raw tea to deionized water is controlled to be 1:100, and the obtained extract is concentrated to 20% of the volume of the original extract by vacuum distillation to obtain a water extract;

[0084] (2) Grinding raw tea from Nankun Mountain for 15 minutes, introducing oxygen at a flow rate of 2 L / min during the grinding process, and then heating and reflux extraction at 110° C. for 2 hours with acetic acid under the condition of introducing oxygen at a flow rate of 2 L / min, controlling the mass ratio of raw tea from Nankun Mountain to acetic acid to be 1:6, and concentrating the obtained extract to 15% of the volume of the original extract by vacuum distillation to obtain an acetic acid extract;

[0085] (3) Grinding raw tea from Nankun Mountain in the dark for 12 minutes, extracting it with ethanol under reflux at 78.3° C. for 2.5 hours in the dark, controlling the mass ratio of raw tea from Nankun Mountain to ethanol to be 1:80, concentrating the extract to 10% of the volume of the original extract, obtaining extract A and tea residues, extracting the tea residues with ethanol under reflux at 78.3° C. for 3 hours under the condition of passing oxygen at a flow rate of 5 L / min, controlling the mass ratio of tea residue to ethanol to be 1:50, concentrating the extract to 15% of the volume of the original extract, obtaining extract B, combining extract A and extract B to obtain ethanol extract;

[0086] (4) The water extract, the acetic acid extract and the ethanol extract are successively added to the mixture of acetic acid, ethanol and deionized water, and the volume ratio of the water extract, the acetic acid extract, the ethanol extract, the acetic acid, the ethanol and the deionized water is controlled to be 5:1:2:3:7:230 to obtain the Nankunshan raw tea extract.

[0087] The preparation method of the hydrolyzate composition of the wormwood leaf of the present embodiment is:

[0088] After grinding the mugwort leaves, mix it with 0.1M hydrochloric acid solution at a ratio of 1:150g / mL, reflux it at 100.3°C for 5h, cool it to room temperature, and filter it with a 400-mesh nylon mesh. Add sodium hydroxide to the filtrate to adjust the pH to 7 to obtain a hydrolyzate composition of mugwort leaves.

[0089] Comparative Example 1

[0090] On the basis of Example 2, the 0.1 M sulfuric acid solution was removed and replaced with an equal weight of 0.01 M sulfuric acid solution, and other conditions remained the same as in Example 2.

[0091] Comparative Example 2

[0092] On the basis of Example 2, the 0.1 M sulfuric acid solution was removed and replaced with an equal weight of pure water, and other conditions remained the same as in Example 2.

[0093] Comparative Example 3

[0094] On the basis of Example 2, the 0.1 M sulfuric acid solution was removed and replaced with an equal weight of 5% acetic acid, and other conditions remained the same as in Example 2.

[0095] Comparative Example 4

[0096] On the basis of Example 2, the 0.1 M sulfuric acid solution was removed and replaced with an equal weight of 40% acetic acid, and other conditions remained the same as in Example 2.

[0097] Performance Testing

[0098] 1. Determination of sugar content in the composition

[0099] 1) "Phenol-sulfuric acid" method

[0100] Test method: Refer to relevant literature (M. Rasouli, A. Ostovar-Ravari, H. Shokri-Afra, Eur. Rev. Med. Pharmacol. Sci., vol. 18 (2014), p2020-2024) to prepare several standard samples of glucose aqueous solution with concentration C between 0-100 ppM, and measure the corresponding A value (maximum absorbance wavelength λ max =487nm), with A as the ordinate and concentration C as the abscissa, A and C are linearly related ( Figure 5 ):

[0101] A=1.0302×10 -2 C+1.8626×10 -3 ,

[0102] Or C = (A-1.8626 × 10 -3 ) / (1.0302×10 -2 ).

[0103] The working curve of glucose standard ( Figure 5 ) Calculate the corresponding sugar content (concentration) from the absorbance A; this value multiplied by the dilution factor of the sample is the actual sugar content of the original sample (if the sample is not diluted, the dilution factor is 1).

[0104] 2) HPLC method

[0105] Since most sugar compounds have no absorption in the "UV-visible" band, evaporative light detector (ELSD) or differential detector is often used when detecting sugar compounds by high performance liquid chromatography. Therefore, an HPLC system is used, including a Shimadzu 2030 high performance liquid chromatograph equipped with a dual-band UV detector and an ELSD detector and an Agilent 1100 high performance liquid chromatograph equipped with an array diode (DAD) detector. The corresponding peak areas under different injection volumes are measured to make a standard curve, and then the sugar content of the unknown sample is calculated from the peak area of ​​the unknown sample through the calibration curve. The test results are shown in Figure 6 , Figure 6This is the working curve of the sugar contained in the hydrolyzate composition of Nankunshan raw tea residue using an ELSD detector, wherein the injection amount of sugar M (μg) and the peak area S are in a quadratic function relationship:

[0106] M=-8.6862×10 -12 S 2 +1.6122×10 -4 S+56.891.

[0107] 2. DPPH method to determine free radical scavenging rate

[0108] Test materials: The compositions of Examples 1-8 and Comparative Examples 1-4 were used as test samples.

[0109] Test method: Take 0.5% concentration of each sample and put it into a 96-well plate respectively, add DPPH prepared with 100 μM methanol solution until the total volume of the solution reaches 200 μl, place it at 37°C for 30 minutes, and then measure it at a wavelength of 560 nm. The calculation formula of free radical scavenging rate is: Free radical scavenging rate (%) = (100-A1 / A0) × 100, wherein A0 is the absorbance of the control group well without adding the sample; A1 is the absorbance of the experimental group well with adding the sample; the test results are shown in Table 1 below.

[0110] Table 1

[0111] Free radical scavenging rate / % Example 1 57.3 Example 2 23.2 Example 3 24.9 Example 4 29.5 Example 5 58.4 Example 6 18.9 Example 7 68.5 Example 8 51.2 Comparative Example 1 10.5 Comparative Example 2 2.4 Comparative Example 3 4.6 Comparative Example 4 9.3

[0112] As shown in Table 1, the compositions prepared in Examples 1-8 of the present invention can effectively extract insoluble matter in tea residues, roots, old leaves and other parts, and synergistically exert good free radical scavenging effects. Comparative Example 1, on the basis of Example 2, replaces the 0.1M sulfuric acid solution with a 0.01M sulfuric acid solution, and uses the "phenol-sulfuric acid" method to determine the sugar yield in the hydrolyzate composition of the Nankunshan raw tea residue treated with 0.1M sulfuric acid solution and 0.01M sulfuric acid solution, and the hydrolysis time is calculated from the moment the liquid starts to boil to the moment the heating is stopped, as shown in the attached figure. Figure 7 As shown, it can be seen that the yield of sugar increases with time and with the concentration of sulfuric acid solution, so the free radical scavenging effect of comparative example 1 is weaker than that of example 2; comparative examples 2-4 are based on example 2, and the 0.1M sulfuric acid solution is replaced by pure water, 5% acetic acid and 40% acetic acid. In order to more intuitively characterize the data, the polysaccharide content obtained when the above-mentioned solvents are used, the sugar yield is determined by the "phenol-sulfuric acid" method, and 0.1M hydrochloric acid solution, 10% acetic acid and 20% acetic acid are added to compare the differences in the hydrolysis curves of Nankunshan raw tea residues catalyzed by different types and concentrations of acids ( Figure 8), the results show that the yield of sugar in the hydrolysis reaction increases with the increase of reaction time and the increase of acid concentration. Compared with hydrochloric acid and sulfuric acid, the efficiency of acetic acid in catalyzing the hydrolysis reaction of tea residues is lower. When the acetic acid concentration is 0 (i.e. pure water), the hydrolysis reaction is so slow that it can be basically ignored. That is, hydrochloric acid has the strongest catalytic efficiency, sulfuric acid is second, and acetic acid is the weakest. Therefore, the effective components extracted by Comparative Examples 2-4 are less than that of Example 2, and the free radical scavenging ability is also weaker than that of Example 2.

[0113] The SH1011 sugar column produced by Shodex was used to analyze and compare the sugar composition in the hydrolysis product composition of Nankunshan raw tea residue catalyzed by 0.1M hydrochloric acid solution (1) and 5% acetic acid (2). The results are as follows: Fig. 9 As shown in the figure, the analysis results show that the chemical composition of the product obtained by catalytic hydrolysis with inorganic acids (such as hydrochloric acid and sulfuric acid) is very different from that of the product obtained by catalytic hydrolysis with organic acids (acetic acid). Hydrochloric acid catalytic hydrolysis not only has a higher yield of sugars, but also has a simpler composition of sugars (better homogeneity), indicating that the selectivity of the hydrolysis reaction is better ( Fig. 9 (1)); however, the acetic acid-catalyzed hydrolysis not only results in a low sugar yield, but also a more complex sugar composition and poor selectivity ( Fig. 9 (2)). Fig. 9 As shown, the HPLC spectrum of the hydrolysis product catalyzed by hydrochloric acid has only one strong peak (retention time Rt≈9.0min) and two very weak peaks (Rt≈8.6min, Rt≈9.5min); while the HPLC spectrum of the hydrolysis product catalyzed by acetic acid contains four peaks with similar intensities and retention times of Rt=8.4min, 9.0min, 9.6min, and 11.15min, respectively, indicating that the hydrolysis reaction catalyzed by acetic acid has poor selectivity.

[0114] On this basis, the SH1011 sugar column was also used to replace the above hydrochloric acid with sulfuric acid for analysis. Compared with hydrochloric acid, the sulfuric acid-catalyzed hydrolysis product under the same conditions has a slightly lower sugar content and a sugar composition similar to that of hydrochloric acid. The HPLC spectrum shows a main peak at Rt≈9.0min and two weak peaks at Rt≈8.6min and Rt≈9.5min, indicating that sulfuric acid also has similar selectivity to hydrochloric acid. The main components contained in the hydrolysis products of Nankunshan Maocha old leaves and Nankunshan Maocha tree stems under hydrochloric acid catalysis are similar to those of Nankunshan Maocha residue hydrolysis products, both of which are main peaks at Rt≈9.0min. Compared with the standard, the retention time of the main peak is consistent with D-galactose.

[0115] 3. Tyrosinase Activity Inhibition Test

[0116] Test materials: The compositions prepared in Example 2 and Comparative Examples 1-4 were used as test samples.

[0117] Test method: Referring to the relevant literature (Liu Qi, Liu Yang, Wu Jinhao, et al. Study on the inhibition of tyrosinase activity by several whitening agents [J]. Daily Chemicals Science, 2015, 38(11): 22-26), 0.05% L-tyrosine solution, 0.5% sample solution and pH=6.8, 0.1 mol / L PBS buffer were prepared and added to the tubes of groups A1, A2, B1 and B2 in turn and mixed. The test tube rack was placed in a 37°C water bath for 15 min and the enzyme activity was 100 U. / mL tyrosinase solution was added to each tube of group A1 and group B1 in turn, shaken and spotted on 96-well plates after 15 minutes. The absorbance was measured with a microplate reader and the inhibition rate was calculated. The inhibition rate was calculated as follows: Inhibition rate = [(A1-A2)-(B1-B2) / (A1-A2)] × 100%, wherein A1 is the absorbance of the blank sample with enzyme system; A2 is the absorbance of the blank sample without enzyme system; B1 is the absorbance of the sample group with enzyme system; B2 is the absorbance of the sample group without enzyme system. The test results are shown in Table 2 below.

[0118] Table 2

[0119] Inhibition rate / % Example 2 21.8 Comparative Example 1 8.7 Comparative Example 2 0.8 Comparative Example 3 3.2 Comparative Example 4 7.4

[0120] As shown in Table 2, in Comparative Examples 1-4, the solvent used was replaced on the basis of Example 2, and the tyrosinase activity inhibition rate of the obtained tea composition was significantly reduced.

[0121] In addition, further extraction of the old leaves, tea residues and stems of the Nankunshan tea tree through the scheme of the present invention is helpful to extract the effective ingredients contained in the insoluble substances with larger molecular weight. Not only is the sugar yield higher, but the sugar composition is also simpler, and the selectivity of the hydrolysis reaction is also better. When the components extracted through this scheme are used for other extracts, for example, the compound use of the Nankunshan tea extract and the old leaves, tea residues and stems of the Nankunshan tea tree in Example 1 can greatly reduce the production cost of functional skin care products, or cooperate with the application of Platycladus orientalis leaves in hair growth products, etc., and has great application prospects.

[0122] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment as above, it is not used to limit the present invention. Any technical personnel in this field can make some changes or modify the technical contents disclosed above into equivalent embodiments without departing from the scope of the technical solution of the present invention. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. A composition containing tea extract, characterized in that: The composition is selected from one or more of Nankunshan raw tea extract, a hydrolysate composition of Nankunshan raw tea old leaves, a hydrolysate composition of Nankunshan raw tea stems, a hydrolysate composition of Nankunshan raw tea residues, a hydrolysate composition of Yingde black tea, a hydrolysate composition of Yingde black tea residues, a hydrolysate composition of Platycladus orientalis leaves and a hydrolysate composition of Artemisia argyi.

2. A composition containing tea extract according to claim 1, characterized in that: The preparation method of the hydrolyzate composition of the Nankunshan raw tea old leaves is as follows: The old leaves of the Nankunshan raw tea tree are ground into powder, mixed with 0.1M hydrochloric acid solution at a ratio of 1:70-80g / mL, refluxed at 100-101°C for 8-12h, cooled to room temperature, and filtered with a 400-mesh nylon mesh. Sodium carbonate is added to the filtrate to adjust the pH to 2.5-3.5 to obtain a hydrolyzate composition of the old leaves of the Nankunshan raw tea.

3. A composition containing tea extract according to claim 1, characterized in that: The preparation method of the hydrolyzate composition of Nankunshan raw tea stems is as follows: The stems of the air-dried Nankunshan tea tree are chopped and ground, mixed with 1.0M hydrochloric acid solution at a ratio of 1:70-80g / mL, refluxed at 100-101°C for 8-12h, cooled to room temperature, and filtered with a 400-mesh nylon mesh. Sodium carbonate is added to the filtrate to adjust the pH to 2.5-3.5 to obtain a hydrolyzate composition of the Nankunshan tea stems.

4. A composition containing tea extract according to claim 1, characterized in that: The preparation method of the hydrolyzate composition of Nankunshan raw tea residue is as follows: The Nankunshan raw tea made from normal tender buds and leaves was ground into powder, mixed with pure water at a ratio of 1:70-80 g / mL, refluxed at 100° C. for 20-40 min, cooled to room temperature, and filtered out the liquid with filter paper to obtain Nankunshan raw tea water extract residue, and an equal volume of 15-25wt% acetic acid aqueous solution and the above-mentioned pure water were added to the Nankunshan raw tea water extract residue, refluxed at 100-102° C. for 20-40 min, cooled to room temperature, and filtered out the liquid with filter paper to obtain Nankunshan raw tea acid extract residue, and an equal volume of 92-98wt% ethanol solution and the above-mentioned pure water were added to the Nankunshan raw tea acid extract residue. , reflux at 78-79°C for 20-40min, cool to room temperature, and filter out the liquid with filter paper to obtain Nankunshan raw tea alcohol extraction residue, add 1 / 2 of the above-mentioned pure water volume of 0.1M sulfuric acid solution to the final residue, reflux at 100-101°C for 8-12h, cool to room temperature, and filter with a 400-mesh nylon mesh to obtain a filtrate, add calcium oxide to the above filtrate to adjust the pH to 6.5-7.5, let it stand overnight, filter out the precipitate with filter paper to obtain a filtrate, add acetic acid to the filtrate to adjust the pH to 2.5-3.5, and obtain a hydrolyzate composition of Nankunshan raw tea residue.

5. The composition containing tea extract according to claim 1, characterized in that: The preparation method of the hydrolyzate composition of Yingde black tea is as follows: The Yingde black tea was ground into powder, mixed with 0.1M hydrochloric acid solution at a ratio of 1:70-80g / mL, refluxed at 100-101°C for 8-12h, cooled to room temperature, and filtered with a 400-mesh nylon mesh. Sodium hydroxide was added to the filtrate to adjust the pH to 2.5-3.5 to obtain a hydrolyzate composition of the Yingde black tea.

6. A composition containing tea extract according to claim 1, characterized in that: The preparation method of the hydrolyzate composition of Yingde black tea residue is as follows: After grinding Yingde black tea, mix it with pure water at a ratio of 1:70-80g / mL, reflux at 100°C for 20-40min, cool to room temperature, filter out the liquid with filter paper to obtain Yingde black tea water extract residue, add 15-25wt% acetic acid aqueous solution with the same volume as the above pure water to the Yingde black tea water extract residue, reflux at 100-102°C for 20-40min, cool to room temperature, filter out the liquid with filter paper to obtain Yingde black tea acid extract residue, add 15-25wt% acetic acid aqueous solution with the same volume as the above pure water to the Yingde black tea acid extract residue A 92-98wt% ethanol solution is prepared, refluxed at 78-79°C for 20-40min, cooled to room temperature, and filtered with filter paper to obtain the Yingde black tea alcohol extraction residue, to the final residue is added 1 / 2 of the volume of the above pure water 0.1M hydrochloric acid solution, refluxed at 100-101°C for 8-12h, cooled to room temperature, and filtered with a 400-mesh nylon mesh to obtain a filtrate, sodium hydroxide is added to the above filtrate to adjust the pH to 2.5-3.5 to obtain a hydrolyzate composition of Yingde black tea residue.

7. A composition containing tea extract according to claim 1, characterized in that: The preparation method of the hydrolyzate composition of Platycladus orientalis leaves is as follows: The Platycladus orientalis leaf powder and 0.1M hydrochloric acid solution are mixed at a ratio of 1:140-160g / mL, refluxed at 100-101°C for 3-7h, cooled to room temperature, and filtered through a 400-mesh nylon mesh. Sodium hydroxide is added to the filtrate to adjust the pH to 6.5-7.5 to obtain a hydrolyzate composition of the Platycladus orientalis leaves.

8. The composition containing tea extract according to claim 1, characterized in that: The preparation method of the hydrolyzate composition of wormwood is as follows: After grinding the mugwort leaves, mix it with 0.1M hydrochloric acid solution at a ratio of 1:140-160g / mL, reflux it at 100-101°C for 3-7h, cool it to room temperature, filter it with a 400-mesh nylon mesh, add sodium hydroxide to the filtrate to adjust the pH to 6.5-7.5, and obtain a hydrolyzate composition of mugwort leaves.

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