Microcapsule as well as preparation method and application thereof

Abstract

The invention discloses a microcapsule as well as a preparation method and application thereof. The microcapsule comprises a core material and a wall material, the wall material comprises pericarpium citri reticulatae polysaccharide, and the core material comprises tea polyphenol. The microcapsule disclosed by the invention can be effectively used for resisting oxidation and regulating intestinal flora, meanwhile, the microcapsule enriches the function development of the dried orange peel, enlarges the effect of the dried orange peel, and provides a new choice for the development of the dried orange peel. The microcapsule can be matched with other flavor substances to be further prepared into products such as solid beverages and the like, so that the microcapsule has a wide application prospect.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of nanometer microcapsules, in particular to a microcapsule and a preparation method and application thereof. BACKGROUND

[0002] Pericarpium Citri Reticulatae has the functions of promoting digestion, relieving abdominal distension and abdominal pain, expelling phlegm, and relieving cough. After extracting polysaccharide substances from Pericarpium Citri Reticulatae, it is found that Pericarpium Citri Reticulatae polysaccharide has the function of regulating human intestinal flora, but Pericarpium Citri Reticulatae polysaccharide is highly soluble and is quickly digested and absorbed, so the efficacy is not long-lasting.

[0003] Therefore, there is an urgent need to provide a product that can enhance the efficacy of Pericarpium Citri Reticulatae polysaccharide and delay the solubility of Pericarpium Citri Reticulatae polysaccharide. SUMMARY

[0004] The present application aims to at least solve one of the technical problems existing in the prior art. To this end, the present application proposes a microcapsule.

[0005] The present application also proposes a preparation method of the microcapsule.

[0006] The present application also proposes an application of the above-mentioned microcapsule.

[0007] The present application also proposes a product.

[0008] According to one aspect of the present application, a microcapsule is proposed, comprising a core material and a wall material:

[0009] The wall material comprises Pericarpium Citri Reticulatae polysaccharide, and the core material comprises tea polyphenol.

[0010] In some embodiments of the present application, the mass ratio of the core material to the wall material is 1:(4-7).

[0011] In some embodiments of the present application, the mass ratio of the core material to the wall material is 1:(4-6).

[0012] In some embodiments of the present application, the mass ratio of the core material to the wall material is 1:(5-6).

[0013] In some embodiments of the present application, the mass ratio of the core material to the wall material is 1:5.57.

[0014] In some embodiments of the present application, the wall material further comprises beta-cyclodextrin.

[0015] In some embodiments of the present application, the mass addition ratio of beta-cyclodextrin to Pericarpium Citri Reticulatae polysaccharide in the wall material is (1-3):1.

[0016] In some embodiments of the present application, the microcapsule further comprises an emulsifier and a stabilizer.

[0017] In some embodiments of the present application, the emulsifier comprises monoglyceride.

[0018] In some embodiments of the present application, the mass of the emulsifier accounts for 7-9% of the mass of the microcapsule.

[0019] In some embodiments of the present application, the mass of the emulsifier accounts for 8.61% of the mass of the microcapsule.

[0020] In some embodiments of the present application, the stabilizer comprises carboxymethyl cellulose.

[0021] In some embodiments of the present application, the mass ratio of the addition of the β-cyclodextrin to the carboxymethyl cellulose is 1:(3-5).

[0022] In some embodiments of the present application, the mass ratio of the addition of the β-cyclodextrin to the carboxymethyl cellulose is 1:(3-4).

[0023] In some embodiments of the present application, the mass ratio of the addition of the β-cyclodextrin to the carboxymethyl cellulose is 1:3.63.

[0024] In some embodiments of the present application, the particle size of the microcapsule is 16-22 μm; for example, it can be 16 μm, 17 μm, 18 μm, 19 μm, 20 μm, 21 μm, 22 μm.

[0025] According to a second aspect of the present application, a preparation method of the above-mentioned microcapsule is provided, and the method comprises the following steps:

[0026] S1, preparing a wall material containing pericarpium citri reticulatae polysaccharide;

[0027] S2, adding tea polyphenol as core material into the wall material, mixing uniformly to obtain a mixture;

[0028] S3, sequentially adding an emulsifier and a stabilizer into the mixture, and drying to obtain the microcapsule.

[0029] In some embodiments of the present application, the preparation method of the pericarpium citri reticulatae polysaccharide is as follows: pericarpium citri reticulatae is mixed with water at a solid-liquid ratio of 15-50 g / mL, and sequentially subjected to ultrasonic-assisted extraction and hot water extraction to obtain a crude extract; the crude extract is subjected to alcohol precipitation to obtain the pericarpium citri reticulatae polysaccharide.

[0030] In some embodiments of the present application, before the ultrasonic-assisted extraction, a step of performing defatting and decoloring treatment on the pericarpium citri reticulatae is further included.

[0031] In some embodiments of the present application, the defatting and decoloring treatment is performed by using ethanol.

[0032] In some embodiments of the present application, the ultrasonic power of the ultrasonic-assisted extraction is 40-60 W.

[0033] In some embodiments of the present application, the ultrasonic power of the ultrasonic-assisted extraction is 45-55 W.

[0034] In some embodiments of the present application, the ultrasonic power of the ultrasonic-assisted extraction is 48-52 W.

[0035] In some embodiments of the present application, the temperature of the ultrasonic-assisted extraction is 22-28℃.

[0036] In some embodiments of the present application, the temperature of the ultrasonic-assisted extraction is 24-26℃.

[0037] In some embodiments of the present application, the time of the ultrasonic-assisted extraction is 20-40 min.

[0038] In some embodiments of the present application, the time of the ultrasonic-assisted extraction is 25-38 min.

[0039] In some embodiments of the present application, the time of the ultrasonic-assisted extraction is 30-35 min.

[0040] In some embodiments of the present application, the solid-liquid ratio is 25-35 g / mL.

[0041] In some embodiments of the present application, the solid-liquid ratio is 28-32 g / mL.

[0042] In some embodiments of the present application, the hot water extraction comprises the following steps: placing the reaction solution obtained by ultrasonic-assisted extraction in 65-75℃ hot water for extraction for 0.5-2 h.

[0043] In some embodiments of the present application, the alcohol precipitation is further preceded by a centrifugation step, which comprises centrifugation at 6000-8000 rpm for 7-9 min.

[0044] In some embodiments of the present application, the alcohol precipitation treatment specifically comprises the following steps:

[0045] Mixing the crude extract with ethanol at a volume ratio of 1:3-5, followed by standing treatment; solid-liquid separation to obtain a solid phase.

[0046] In some embodiments of the present application, the standing treatment temperature is 0-6℃. Preferably, it is 4℃.

[0047] In some embodiments of the present application, the standing treatment time is 8-20 h.

[0048] In some embodiments of the present application, the volume concentration of ethanol in the ethanol solution is 90%-100%, preferably 90%.

[0049] In some embodiments of the present application, the step of purifying the alcohol-precipitated pericarpium citri reticulatae polysaccharide is further included.

[0050] In some embodiments of the present application, the purifying treatment includes at least one of washing treatment, decoloring treatment, protein removal treatment, and dialysis treatment.

[0051] In some embodiments of the present application, the purifying treatment includes washing treatment.

[0052] In some embodiments of the present application, the washing treatment includes centrifuging the alcohol-precipitated pericarpium citri reticulatae polysaccharide, collecting the solid phase, and sequentially washing the solid phase with ethanol, diethyl ether, and acetone.

[0053] In some embodiments of the present application, the step of adding β-cyclodextrin to the wall material is further included.

[0054] In some embodiments of the present application, the mass addition ratio of β-cyclodextrin to pericarpium citri reticulatae polysaccharide in the wall material is (1-3):1.

[0055] In some embodiments of the present application, the mass ratio of the core material to the wall material is 1:(4-7).

[0056] In some embodiments of the present application, the mass ratio of the core material to the wall material is 1:(4-6).

[0057] In some embodiments of the present application, the mass ratio of the core material to the wall material is 1:(5-6).

[0058] In some embodiments of the present application, the mass ratio of the core material to the wall material is 1:5.57.

[0059] In some embodiments of the present application, the emulsifier includes monoglyceride.

[0060] In some embodiments of the present application, the mass of the emulsifier accounts for 7-9% of the mass of the microcapsule.

[0061] In some embodiments of the present application, the mass of the emulsifier accounts for 8.61% of the mass of the microcapsule.

[0062] In some embodiments of the present application, the emulsifier is added and uniformly mixed, and then the stabilizer is added after standing for 25-35 min.

[0063] In some embodiments of the present application, the stabilizer includes carboxymethyl cellulose.

[0064] In some embodiments of the present application, the mass ratio of the beta-cyclodextrin to the carboxymethyl cellulose is 1:(3-5).

[0065] In some embodiments of the present application, the mass ratio of the beta-cyclodextrin to the carboxymethyl cellulose is 1:(3-4).

[0066] In some embodiments of the present application, the mass ratio of the beta-cyclodextrin to the carboxymethyl cellulose is 1:3.63.

[0067] In some embodiments of the present application, the drying comprises freeze-drying.

[0068] According to a third aspect of the present application, the above-mentioned microcapsules are used in any one of the following:

[0069] (1) antioxidant;

[0070] (2) regulating intestinal flora;

[0071] (3) preparing a product for regulating intestinal flora.

[0072] In some embodiments of the present application, the regulating intestinal flora comprises increasing the abundance of Bifidobacteriaceae flora;

[0073] and / or, reducing the abundance of Enterobacteriaceae, Helicobacteriaceae and / or Rikenellaceae flora.

[0074] According to a fourth aspect of the present application, a product is provided, which comprises the above-mentioned microcapsules.

[0075] In some embodiments of the present application, the product comprises a pharmaceutical product or a beverage product.

[0076] According to some embodiments of the present application, at least the following beneficial effects are achieved: the present application provides a microcapsule which can be effectively used for antioxidant, regulating intestinal flora, at the same time, the microcapsule enriches the functional development of pericarpium citri reticulatae and amplifies its efficacy, providing a new choice for the development of pericarpium citri reticulatae. The microcapsule can also be combined with other flavoring substances to further prepare a solid beverage product, etc., which has a broad application prospect. BRIEF DESCRIPTION OF DRAWINGS

[0077] The present application will be further described below in conjunction with the drawings and examples, in which:

[0078] Figure 1 is a graph of the antioxidant detection results in the embodiments of the present application;

[0079] Figure 2 is a graph of the antioxidant detection results in the embodiments of the present application;

[0080] Figure 3 Figure for the influence of the pericarpium citri reticulatae polysaccharide microcapsules in the embodiments of the present application on the abundance of different bacterial families of the intestinal flora of mice. DETAILED DESCRIPTION

[0081] The concept and technical effects of the present application will be described below in conjunction with the embodiments so as to fully understand the objects, features and effects of the present application. Obviously, the described embodiments are only some of the embodiments of the present application, but not all the embodiments. Based on the embodiments of the present application, other embodiments obtained by those skilled in the art without creative effort fall within the scope of the present application.

[0082] The specific conditions not mentioned in the embodiments are carried out according to the conventional conditions or the conditions recommended by the manufacturers. The reagents or instruments used are all conventional products that can be purchased on the market.

[0083] When a numerical range is disclosed herein, the above range is considered to be continuous and includes the minimum value and the maximum value of the range, and every value between the minimum value and the maximum value. Further, when the range refers to an integer, every integer between the minimum value and the maximum value of the range is included. In addition, when multiple ranges are provided to describe a feature or a characteristic, the ranges can be combined. In other words, unless otherwise indicated, all the ranges disclosed herein should be understood to include any and all sub-ranges falling within the range.

[0084] “and / or” is used to indicate that one or both of the described conditions can occur, for example, A and / or B includes (A and B) and (A or B).

[0085] Example 1

[0086] In this embodiment, a microcapsule containing pericarpium citri reticulatae polysaccharide extract (particle size 20 μm) is prepared, which comprises the following raw materials in weight parts: pericarpium citri reticulatae 422 parts, β-cyclodextrin 100 parts, carboxymethyl cellulose (CMC) 363 parts, monoglyceride 15 parts, tea polyphenol 27 parts. The preparation steps are as follows:

[0087] 1. Extraction of pericarpium citri reticulatae polysaccharide

[0088] (1) Drying of pericarpium citri reticulatae: pericarpium citri reticulatae (specifically Xinhui pericarpium citri reticulatae purchased from Jiangmen Liguang International Food Co., Ltd.) is weighed and dried in a 40℃ oven to constant weight.

[0089] (2) Crushing and sieving: pericarpium citri reticulatae is put into a crusher and crushed, and the pericarpium citri reticulatae powder is sieved with a 100-mesh sieve. The unsieved pericarpium citri reticulatae residue is crushed and sieved again, and sealed for use.

[0090] (3) Ethanol degreasing, decolorization: Put the dried pericarpium citri reticulatae powder into a round bottom flask, add anhydrous ethanol at a ratio of 1:10 (W / V), and heat in a water bath at 80°C for 2 times, each time for 1.5 h.

[0091] (4) Ultrasonic treatment: After degreasing and decolorization, mix the dried pericarpium citri reticulatae powder with distilled water at a ratio of 31 g / mL, and then perform ultrasonic treatment in an ultrasonic cleaning machine for 33 min, with a power of 50 W and a temperature of 25°C.

[0092] (5) Hot water extraction: After ultrasonic treatment, place the pericarpium citri reticulatae powder in a water bath at 71°C for 1 h.

[0093] (6) Centrifugal concentration: Centrifuge the extraction liquid at 7000 rpm for 8 min, collect the supernatant, and concentrate it.

[0094] (7) Ethanol precipitation: Mix the pericarpium citri reticulatae polysaccharide concentrate with 90% anhydrous ethanol at a ratio of 1:4 by volume, and then place it in a 4°C refrigerator for 12 h to precipitate the pericarpium citri reticulatae polysaccharide.

[0095] (8) Washing: Centrifuge the precipitated pericarpium citri reticulatae polysaccharide at 7000 rpm for 4 min, collect the precipitate, and then wash it with anhydrous ethanol, diethyl ether, and acetone twice.

[0096] (9) Drying: Pour the washed pericarpium citri reticulatae polysaccharide into a blank culture dish, and then place it in a 45°C oven to dry to a constant weight, which is the finished product of pericarpium citri reticulatae polysaccharide (yield of 11.78%).

[0097] The finished product of pericarpium citri reticulatae polysaccharide is used to determine the content and yield of polysaccharide by the anthrone-sulfuric acid method, and the specific steps are as follows:

[0098] Take 0.1 g of the finished product of pericarpium citri reticulatae polysaccharide, dissolve it in 100 mL of distilled water. Take 1 mL of the dissolved liquid, add 4 mL of anthrone reagent (weigh 1 g of anthrone, dissolve it in 1000 mL of 80% (V / V) sulfuric acid. The preparation method of sulfuric acid is as follows: slowly add 760 mL of concentrated sulfuric acid (specific gravity 1.84) to water, and dilute to 1000 mL.), heat in a boiling water bath for 10 min, quickly cool to room temperature, place in the dark for 10 min, and measure the absorbance at 620 nm. Under the same experimental conditions and steps, prepare a standard curve with glucose as the standard, and calculate the content of polysaccharide.

[0099] The yield of pericarpium citri reticulatae polysaccharide is calculated according to the following formula.

[0100] Pericarpium citri reticulatae polysaccharide extraction rate (%) = m1 / m2 x 100%

[0101] In the formula, m1 is the mass of pericarpium citri reticulatae polysaccharide powder, g; m2 is the mass of pericarpium citri reticulatae powder, g.

[0102] 2. Preparation of microcapsules containing extract of pericarpium citri reticulatae polysaccharide

[0103] (1) Wall material: prepare saturated β-cyclodextrin solution, add the prepared pericarpium citri reticulatae polysaccharide (the mass ratio of β-cyclodextrin and pericarpium citri reticulatae polysaccharide is 2 / 1) to form a uniform paste.

[0104] (2) Core material: add the core material tea polyphenol dissolved in distilled water to the paste obtained in the above (1), control the core / wall mass ratio to be 1:5.57, and stir uniformly.

[0105] (3) Emulsifier: add emulsifier monoglyceride (8.61% of the total mass of the microcapsules), and stir uniformly.

[0106] (4) Stabilizer: after standing for 30 min, slowly add carboxymethyl cellulose (dissolved in anhydrous ethanol), and the mass ratio of β-cyclodextrin and CMC is 1:3.63.

[0107] (5) Drying: after freeze-drying, the microcapsule product is obtained.

[0108] Comparative Example 1

[0109] In this example, a microcapsule containing extract of pericarpium citri reticulatae polysaccharide is prepared, which is different from Example 1 only in that no pericarpium citri reticulatae polysaccharide is added.

[0110] Test Example

[0111] In this test example, the performance of the microcapsules prepared in Example 1 and Comparative Example 1 is tested.

[0112] 1. Antioxidant capacity analysis

[0113] The antioxidant activity of the microcapsules prepared in Example 1 and Comparative Example 1 is analyzed by ABTS free radical scavenging experiment and DPPH free radical scavenging experiment.

[0114] (1) ABTS free radical scavenging experiment

[0115] Equal volumes of 7 mmol / L ABTS solution were mixed with 2.45 mmol / L potassium persulfate and reacted in the dark for 12–16 h to prepare ABTS+. The ABTS+ solution was diluted with methanol until its absorbance at 734 nm was 0.70 ± 0.02. 25 μL of samples (a solution of microcapsules prepared in Example 1 with a concentration of 1 mg / mL, a solution of microcapsules prepared in Comparative Example 1 with a concentration of 1 mg / mL, a 0.77 mg / mL solution of tangerine peel polysaccharide, a 0.14 mg / mL solution of tea polyphenols, and a solution of a combination of tangerine peel polysaccharide and tea polyphenols containing 0.77 mg / mL of tangerine peel polysaccharide and 0.14 mg / mL of tea polyphenols) were added to 2 mL of ABTS+ solution, and the absorbance (A) at 734 nm was measured after 6 min. The absorbance (A0) of a mixture of 2 mL ABTS+ solution and 25 μL methanol solution was measured at 517 nm; the absorbance (Aj) of a mixture of 2 mL methanol solution and 25 μL sample was measured at 517 nm. The free radical scavenging rate was calculated using the following formula: Scavenging rate (%) = 1 - (A - Aj) / A0 × 100%.

[0116] (2) DPPH free radical scavenging experiment

[0117] Add 1 mL of sample solutions of different concentrations to a 0.2 mmol / L DPPH ethanol solution (the solutions of microcapsules prepared in Example 1 with a concentration of 1 mg / mL, the solutions of microcapsules prepared in Comparative Example 1 with a concentration of 1 mg / mL, a 0.77 mg / mL solution of tangerine peel polysaccharide, a 0.14 mg / mL solution of tea polyphenols, and a solution of a combination of tangerine peel polysaccharide and tea polyphenols (containing 0.77 mg / mL tangerine peel polysaccharide and 0.14 mg / mL tea polyphenols)). Mix well and react at room temperature for 60 min. The blank sample solution was replaced with distilled water. The absorbance was measured at 517 nm, and the free radical scavenging rate was calculated using the following formula: Free radical scavenging rate (%) = 1 - (sample absorbance / blank absorbance) × 100%.

[0118] The results obtained are as follows Figures 1-2 As shown, from Figure 1 As can be seen, the addition of tangerine peel polysaccharide enhanced the antioxidant capacity of traditional polyphenol microcapsules, indicating that the antioxidant properties of tangerine peel polysaccharide were maintained and functioned within the microcapsules.

[0119] from Figure 2 It can be seen that after being made into microcapsules, the antioxidant capacity of tangerine peel polysaccharides and polyphenols can be superimposed compared to single tangerine peel polysaccharides and polyphenols. At the same time, microcapsules delay the release of the antioxidant capacity of each component.

[0120] 2. Analysis of microcapsule regulating intestinal flora function

[0121] Experimental method: Inbred mice were used as experimental animals, 18-22g, all male, 10-15 in each group. In the experiment, in order to detect the effect of pericarpium citri reticulatae polysaccharide in microcapsules, single dose 2 groups were set, which were microcapsules prepared by example 1 and microcapsules prepared by comparative example 1 respectively. The mice were tested for 14 days by giving microcapsules (5g at a time, twice a day). 24 hours after the last administration, 0.1g of mouse feces was taken aseptically, diluted 10 times continuously, and inoculated into culture medium. The identification and counting of reaction colonies were carried out, and the number of bacteria per gram of wet feces was calculated, and the logarithm was taken for statistical processing. Intestinal flora was detected. Detection index: intestinal flora such as bifidobacterium, enterobacterium, helicobacterium, etc. The regulating effect of pericarpium citri reticulatae polysaccharide microcapsules on intestinal flora of mice was analyzed.

[0122] The results are shown in Figure 3 As can be seen from the figure, the pericarpium citri reticulatae polysaccharide microcapsules prepared by the embodiment of the application can increase the abundance of bifidobacterium family flora, while reducing the abundance of enterobacterium family, helicobacterium family and rikenella family flora. Compared with microcapsules without pericarpium citri reticulatae polysaccharide, it has obvious regulating ability, and also reveals the regulating ability of pericarpium citri reticulatae polysaccharide on intestinal flora and adds it to the microcapsules.

[0123] The above embodiments of the application are described in detail in combination with the drawings, but the application is not limited to the above embodiments. Within the scope of knowledge possessed by those skilled in the art, various changes can be made without departing from the purpose of the application. In addition, the embodiments of the application and the features in the embodiments can be combined with each other without conflict.

Claims

1. A microcapsule, characterized in that, Includes core and wall materials: The wall material includes tangerine peel polysaccharide, and the core material includes tea polyphenols.

2. The microcapsule according to claim 1, characterized in that, The mass ratio of the core material to the wall material is 1:(4-7).

3. The microcapsule according to claim 1, characterized in that, The wall material also includes β-cyclodextrin; Preferably, the mass ratio of β-cyclodextrin to tangerine peel polysaccharide in the wall material is (1-3):

1.

4. The microcapsule according to claim 1, characterized in that, The microcapsules also include emulsifiers and stabilizers; Preferably, the emulsifier comprises monoglycerides; More preferably, the emulsifier accounts for 7-9% of the mass of the microcapsule; Preferably, the stabilizer comprises carboxymethyl cellulose.

5. A method for preparing microcapsules as described in any one of claims 1-4, characterized in that, The preparation method includes the following steps: S1. Preparation of wall material containing tangerine peel polysaccharide; S2. Add tea polyphenols as a core material to the wall material and mix them evenly to obtain a mixture. S3. Add emulsifier and stabilizer to the mixture in sequence, and then dry to prepare microcapsules.

6. The preparation method according to claim 5, characterized in that, The preparation method of the tangerine peel polysaccharide is as follows: Tangerine peel is mixed with water at a solid-liquid ratio of 15-50 g / mL, and then subjected to ultrasonic-assisted extraction and hot water extraction to obtain a crude extract; the crude extract is subjected to alcohol precipitation to obtain tangerine peel polysaccharide; Preferably, the ultrasonic power for the ultrasound-assisted extraction is 40-60W; Preferably, the ultrasound-assisted extraction time is 20-40 minutes; Preferably, the hot water extraction includes the following steps: placing the reaction solution obtained by ultrasonic-assisted extraction in hot water at 65-75℃ for 0.5-2 hours.

7. The preparation method according to claim 5, characterized in that, It also includes the step of adding β-cyclodextrin to the wall material; Preferably, the mass ratio of β-cyclodextrin to tangerine peel polysaccharide in the wall material is (1-3):

1. Preferably, the mass ratio of the core material to the wall material is 1:(4-7). And / or, the emulsifier includes monoglycerides; And / or, the stabilizer includes carboxymethyl cellulose.

8. The use of the microcapsules according to any one of claims 1-4 in any of the following: (1) Antioxidant; (2) Regulates the gut microbiota; (3) Prepare products for regulating gut microbiota.

9. The application according to claim 8, characterized in that, The regulation of gut microbiota includes increasing the abundance of Bifidobacteriaceae. And / or, reduce the abundance of Enterobacteriaceae, Helicobacteraceae and / or Riken Bacteriaceae flora.

10. A product characterized in that, The product includes the microcapsules as described in any one of claims 1-4.

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