阅读说明：本技术 一种桃拓酚微囊及其制备方法 (Peach tocol microcapsule and preparation method thereof ) 是由 陆海亮 刘冠静 郭懿 王玉 钟玉容 于 2021-04-23 设计创作，主要内容包括：本发明涉及日化品领域,更具体地,本发明涉及一种桃拓酚微囊及其制备方法,所述桃拓酚微囊,从内至外依次包括内核层、缓冲层、外壳层；所述内层的原料包括桃拓酚和醇类。本申请通过将桃拓酚制备微囊,在水相中通过悬浮剂可以很好地悬浮,而不产生沉淀,不影响体系透明度,不产生泡沫、黏腻感；在乳液体系中,可直接加入,分散于体系中,不产生沉淀,不影响体系透明度,不产生泡沫、黏腻感；而且在包裹形态下,本申请中微囊形成柔软的皮肤触感,在使用时,微囊破裂,释放微小的桃拓酚粉末。(The invention relates to the field of daily chemicals, in particular to a totarol microcapsule and a preparation method thereof, wherein the totarol microcapsule sequentially comprises an inner core layer, a buffer layer and an outer shell layer from inside to outside; the raw materials of the inner layer comprise totarol and alcohols. According to the application, the totarol is prepared into the micro-capsules, and can be well suspended in a water phase through the suspending agent, so that no precipitate is generated, the transparency of a system is not influenced, and no foam or sticky feeling is generated; the emulsion can be directly added into an emulsion system, is dispersed in the system, does not generate precipitate, does not influence the transparency of the system, and does not generate foam and sticky feeling; in addition, in the encapsulated form, the microcapsules form a soft skin feel, and in use, the microcapsules rupture and release tiny totarol powder.)

1. The totarol microcapsule is characterized by comprising an inner core layer, a buffer layer and an outer shell layer from inside to outside in sequence; the raw materials of the inner layer comprise totarol and alcohols.

2. The totarol microcapsule according to claim 1, wherein the alcohol is selected from one or more of sorbitol, erythritol, glucitol, xylitol, mannitol, steviol and maltitol.

3. The totarol microcapsule according to claim 2, wherein the buffer layer is made of one or more materials selected from the group consisting of hydrophilic colloid, cellulose, and starch.

4. The totarol microcapsule according to claim 3, wherein the hydrophilic colloid is xanthan gum and/or carrageenan gum.

5. The totarol microcapsule of claim 3, wherein the cellulose comprises one or more of hydroxyethylcellulose, carboxymethylcellulose, and microcrystalline cellulose.

6. The totarol microcapsule according to any one of claims 1 to 5, wherein the raw material of the outer shell layer comprises one or more of a binder, a plant extract, and a colorant.

7. The totarol microcapsule according to claim 6, wherein the plant extract is selected from one or more of lavender extract, lithospermum extract, haematococcus pluvialis extract, turmeric extract, crabapple fruit extract, prinsepia utilis royle extract, camellia extract, dendrobium nobile extract, honeysuckle flower extract, and cacao bean extract.

8. A method for preparing totarol microcapsules according to any of claims 1 to 7, comprising the steps of:

(1) grinding the totarol and then placing the ground totarol in a fluidized bed;

(2) preparing alcohols and the totarol powder obtained in the step (1) to obtain an inner core layer;

(3) adhering the raw material of the buffer layer to the surface of the inner core layer to obtain the buffer layer;

(4) adhering the raw material of the shell layer to the surface of the buffer layer;

(5) and (5) granulating to obtain the finished product.

9. The method for preparing the totarol microcapsule according to claim 8, wherein the step (1) comprises: grinding totarol to 800-.

10. The method for preparing totarol microcapsules of claim 8, wherein the step (2) comprises: adopting 450-550m for alcohol and totarol powder obtained in the step (1)³The wind speed is 600-700rpm, and high-speed jet flow is carried out for 8-15min to prepare the inner core layer.

Technical Field

The invention relates to the field of daily chemicals, in particular to a totarol microcapsule and a preparation method thereof.

Background

The main component of the Mycoplasma persimmons phenol having the functions of sterilization, antimicrobial, antioxidant and anti-inflammatory is aromatic diterpene, which can inhibit peroxidation of oil and fat and remove active oxygen. The totarol is light yellow powder in appearance, is tasteless and has slight aromatic odor. The molecular formula of totarol is C₂₀H₃₀O has a structure of

The basic physicochemical properties of totarol are as follows: the solubility in water was 0.37mg/L (20 ℃ C.), the melting point was 68 ℃ and thermal decomposition was carried out at 96 ℃. Because of the lower solubility and higher melting point of totarol in water, and because of more aqueous phase systems, personal care products can form granular precipitates, and the problems of influence on daily use such as foam, stickiness and the like can be caused by the use of a surfactant for solubilization; by solubilization with alcohols, after addition to the aqueous phase, a suspension can form, affecting the apparent clarity of the system. Therefore, the application of totarol in personal care products is limited at present. In addition, the totarol is light yellow in appearance, so that the requirement of various appearances in the field of personal care products cannot be met.

Disclosure of Invention

In order to solve the problems in the prior art, the invention provides a totarol microcapsule, which comprises an inner core layer, a buffer layer and an outer shell layer from inside to outside in sequence; the raw materials of the inner layer comprise totarol and alcohols.

In a preferred embodiment of the present invention, the alcohol is one or more selected from sorbitol, erythritol, glucitol, xylitol, mannitol, steviol and maltitol.

In a preferred embodiment of the present invention, the raw material of the buffer layer is selected from one or more of hydrophilic colloid, cellulose, and starch.

As a preferred technical solution of the present invention, the hydrophilic colloid is xanthan gum and/or carrageenan.

In a preferred embodiment of the present invention, the cellulose includes one or more of hydroxyethyl cellulose, carboxymethyl cellulose, and microcrystalline cellulose.

In a preferred embodiment of the present invention, the raw material of the outer shell layer includes one or more of a binder, a plant extract, and a colorant.

As a preferred technical solution of the present invention, the plant extract is selected from one or more of lavender extract, lithospermum extract, haematococcus pluvialis extract, turmeric extract, crabapple fruit extract, prinsepia utilis royle extract, camellia extract, dendrobium nobile extract, honeysuckle flower extract, and cacao bean extract.

The second aspect of the invention provides a preparation method of the totarol micro-capsule, which comprises the following steps:

(1) grinding the totarol and then placing the ground totarol in a fluidized bed;

(2) preparing alcohols and the totarol powder obtained in the step (1) to obtain an inner core layer;

(3) adhering the raw material of the buffer layer to the surface of the inner core layer to obtain the buffer layer;

(4) adhering the raw material of the shell layer to the surface of the buffer layer;

(5) and (5) granulating to obtain the finished product.

As a preferred embodiment of the present invention, the step (1) includes: grinding totarol to 800-.

As a preferred embodiment of the present invention, the step (2) includes: adopting 450-550m for alcohol and totarol powder obtained in the step (1)³The wind speed is 600-700rpm, and high-speed jet flow is carried out for 8-15min to prepare the inner core layer.

Compared with the prior art, the invention has the following beneficial effects:

(1) according to the application, the totarol is prepared into the micro-capsules, and can be well suspended in a water phase through the suspending agent, so that no precipitate is generated, the transparency of a system is not influenced, and no foam or sticky feeling is generated; the emulsion can be directly added into an emulsion system, is dispersed in the system, does not generate precipitate, does not influence the transparency of the system, and does not generate foam and sticky feeling; in addition, in the encapsulated form, the microcapsules form a soft skin feel, and in use, the microcapsules rupture and release tiny totarol powder.

(2) The present application can create different color appearances through the selection of different plant extracts and colorants.

(3) The specific alcohols and totarol in the application make the jet nucleation stable and uniform in nucleation shape.

(4) The weight ratio in the application is (2-2.5): (1-1.5): cellulose, hydrophilic colloid and starch, and can maintain the adhesion stability of the buffering layer and the inner core layer and has high dissolving and releasing performance.

(5) The xanthan gum and the dendrobium extract are used as raw materials of the outer shell layer, so that the skin-friendly and soft skin feeling is good.

Detailed Description

The present invention is illustrated by the following specific embodiments, but is not limited to the specific examples given below.

The invention provides a totarol microcapsule, which sequentially comprises an inner core layer, a buffer layer and an outer shell layer from inside to outside.

Inner core layer

In one embodiment, the raw material of the inner layer comprises totarol and alcohols.

In one embodiment, the totarol and alcohol are present in a weight ratio of 1: (1-2).

Preferably, the weight ratio of totarol to alcohols is 1: 1.5.

preferably, the alcohol is selected from one or more of sorbitol, erythritol, glucitol, xylitol, mannitol, steviol and maltitol; more preferably, the alcohols include erythritol and mannitol.

Preferably, the weight ratio of erythritol to mannitol is 1: (1-2); more preferably, the weight ratio of erythritol to mannitol is 1: 1.5.

totarol has low solubility in aqueous phase, while personal care products have more aqueous phase systems and are easy to form granular precipitates. At present, a surfactant is adopted for solubilization, however, the surfactant is easy to generate foam, the viscosity of the surfactant influences the use, and after the surfactant is dissolved by alcohols and added into a water phase, a suspension can be formed, and the appearance transparency of a system is influenced. Applicants have unexpectedly discovered that the use of totarol in personal care products can be improved by microencapsulating totarol. However, during the formation of totarol into the inner core layer, the applicant found that totarol is not easy to nucleate and has poor stability, affecting the adhesion of the subsequent buffer layer, and the applicant surprisingly found that when the alcohol is selected from one or more of sorbitol, erythritol, glucitol, xylitol, mannitol, steviol and maltitol, in particular, the alcohol is present in a weight ratio of 1: when erythritol and mannitol of (1-2) are used, the formation of the inner core layer is stable and the nucleation shape is uniform, and the applicant believes that the possible reason is that under the action of the specific alcohol, on the one hand, the influence of water molecules in air on nucleation in the jet nucleation process is avoided, and on the other hand, the flexible chain segment of the alcohol maintains the nucleation shape stability.

Buffer layer

In one embodiment, the raw material of the buffer layer is selected from one or more of hydrophilic colloid, cellulose and starch.

Preferably, the hydrophilic colloid is xanthan gum and/or carrageenan; more preferably, the hydrocolloid is xanthan gum.

Preferably, the cellulose comprises one or more of hydroxyethyl cellulose, carboxymethyl cellulose and microcrystalline cellulose; more preferably, the cellulose is microcrystalline cellulose.

Microcrystalline cellulose (MCC) is a straight-chain polysaccharide substance combined by beta-1, 4-glucoside bonds as a main component, and is white, odorless and tasteless crystalline powder which is formed by superfine, short rod-shaped or powdery porous particles capable of freely flowing and hydrolyzed to the limit degree of polymerization (LOOP) by dilute acid of natural cellulose.

In one embodiment, the starch is amylopectin.

The source of the amylopectin starch according to the present invention is not particularly limited, and those skilled in the art can select it routinely.

In one embodiment, the source of amylopectin is glutinous rice.

In one embodiment, the buffer layer is prepared from cellulose, hydrophilic colloid and starch, and the weight ratio of the cellulose to the hydrophilic colloid is (2-2.5): (1-1.5): 1.

preferably, the buffer layer is prepared from cellulose, hydrophilic colloid and starch in a weight ratio of 2.2: 1.3: 1.

the weight ratio in the application is (2-2.5): (1-1.5): cellulose, hydrophilic colloid and starch, and can maintain the adhesion stability of the buffering layer and the inner core layer and has high dissolving and releasing performance.

Outer shell layer

In one embodiment, the raw material of the outer shell layer comprises one or more of a binder, a plant extract, and a colorant.

Preferably, the plant extract is selected from one or more of lavender extract, lithospermum extract, haematococcus pluvialis extract, turmeric extract, crabapple fruit extract, prinsepia utilis royle extract, camellia extract, dendrobium extract, honeysuckle flower extract and cacao bean extract; more preferably, the plant extract comprises a dendrobium extract.

Preferably, the adhesive is selected from one or more of xanthan gum, carrageenan, hydroxyethyl cellulose, carboxymethyl cellulose, corn starch and rice starch; more preferably, the binder is xanthan gum.

The coloring agent described in the present application is not particularly limited and may be conventionally selected by those skilled in the art.

Preferably, the colorant is selected from one or more of caramel color, carmine and sunset yellow.

The xanthan gum and the dendrobium extract are used as raw materials of the outer shell layer, so that the skin-friendly and soft skin feeling is good.

In one embodiment, the weight ratio of the binder, the plant extract and the colorant is (5-8): (25-35): 1.

preferably, the weight ratio of the adhesive to the plant extract to the colorant is 6.7: 30: 1.

in one embodiment, the weight ratio of the inner core layer, the buffer layer and the outer shell layer is (7-10): (7-10): 1.

preferably, the weight ratio of the inner core layer, the buffer layer and the outer shell layer is 8.8: 8: 1.

the weight ratio of the inner core layer, the buffer layer and the outer shell layer in the application is (7-10): (7-10): 1, the product is soft and skin friendly.

The second aspect of the invention provides a preparation method of the totarol micro-capsule, which comprises the following steps:

(1) grinding the totarol and then placing the ground totarol in a fluidized bed;

(2) preparing alcohols and the totarol powder obtained in the step (1) to obtain an inner core layer;

(3) adhering the raw material of the buffer layer to the surface of the inner core layer to obtain the buffer layer;

(4) adhering the raw material of the shell layer to the surface of the buffer layer;

(5) and (5) granulating to obtain the finished product.

In one embodiment, the step (1) comprises: grinding totarol to 800-.

Preferably, the step (1) comprises: the totarol is ground to 1000 mesh and placed in a fluidized bed.

In one embodiment, the step (2) comprises: adopting 450-550m for alcohol and totarol powder obtained in the step (1)³The wind speed is 600-700rpm, and high-speed jet flow is carried out for 8-15min to prepare the inner core layer.

Preferably, the step (2) includes: adopting 500m of alcohol and the totarol powder obtained in the step (1)³And/h wind speed, 650rpm rotating speed, and performing high-speed jet flow for 10min to prepare the inner core layer.

In one embodiment, the step (3) comprises: the raw material of the buffer layer adopts 900-1000m³The wind speed is 700 and 800rpm, and high-speed jet flow is carried out for 8-14min to obtain the buffer layer.

Preferably, the step (3) includes: the raw material of the buffer layer is 970m³And (4) carrying out high-speed jet flow for 10min at the speed of 750rpm at the speed of/h to obtain the buffer layer.

In one embodiment, the step (4) comprises: the raw material of the outer shell layer adopts 800-850m³The wind speed is 800-.

Preferably, the step (4) includes: the raw material of the outer shell layer is 820m³And/h wind speed, 880rpm, and performing high-speed jet for 10min to make the raw material of the outer shell layer adhere to the surface of the buffer layer.

In one embodiment, the step (5) comprises: top spray drying, 55 deg.C hot air, 1050m³Drying for 35min, and performing rounding granulation to prepare particles with uniform particle size.

Examples

Hereinafter, the present invention will be described in more detail by way of examples, but it should be understood that these examples are merely illustrative and not restrictive. The starting materials used in the examples which follow are all commercially available unless otherwise stated.

Example 1

Embodiment 1 of the present invention provides a totarol microcapsule, which is specifically prepared by the following steps:

(1) grinding totarol to 1000-mesh fine particles, quantitatively pouring 20kg of totarol into a fluidized bed;

(2) mixing 12kg erythritol, 18kg mannitol and totarol powder at a ratio of 500m³Performing high-speed jet flow for 10min at the wind speed of 650rpm per hour to prepare an inner core layer;

(3) the buffer layer raw materials of 22kg of microcrystalline cellulose, 13kg of xanthan gum and 10kg of glutinous rice starch are 970m³Performing high-speed jet flow for 10min at the wind speed of 750rpm per hour to obtain a buffer layer;

(4) mixing 1kg xanthan gum, 4.5kg herba Dendrobii extract, and 0.15kg caramel pigment at 820m³The wind speed is/h, the rotating speed is 880rpm, and high-speed jet flow is carried out for 10min, so that the raw material of the outer shell layer is adhered to the surface of the buffer layer;

(5) top spray drying, 55 deg.C hot air, 1050m³Drying for 35min, and performing rounding granulation to prepare particles with uniform particle size.

The microcrystalline cellulose is purchased from Hebei hongtao bioengineering limited, the xanthan gum is purchased from Zhonghong bioengineering limited in Anhui, the sticky rice starch is purchased from Xingwang food limited in Foshan city, and the dendrobium extract is purchased from Xianhhang Yue biotechnology limited with the specification of 5: 1.

Example 2

Embodiment 2 of the present invention provides a totarol microcapsule, which is specifically prepared by the following steps:

(1) grinding totarol to 800-mesh fine particles, quantitatively pouring 20kg of totarol into a fluidized bed;

(2) mixing 12kg erythritol, 12kg mannitol and totarol powder at a ratio of 500m³Performing high-speed jet flow for 10min at the wind speed of 650rpm per hour to prepare an inner core layer;

(3) the buffer layer raw materials of 20kg of microcrystalline cellulose, 10kg of xanthan gum and 10kg of glutinous rice starch are 970m³Performing high-speed jet flow for 10min at the wind speed of 750rpm per hour to obtain a buffer layer;

(4) mixing xanthan gum 0.75kg, herba Dendrobii extract 3.75kg, and coke 0.15kgOuter shell material of sugar pigment at 820m³The wind speed is/h, the rotating speed is 880rpm, and high-speed jet flow is carried out for 10min, so that the raw material of the outer shell layer is adhered to the surface of the buffer layer;

(5) top spray drying, 55 deg.C hot air, 1050m³Drying for 35min, and performing rounding granulation to prepare particles with uniform particle size.

The microcrystalline cellulose is purchased from Hebei hongtao bioengineering limited, the xanthan gum is purchased from Zhonghong bioengineering limited in Anhui, the sticky rice starch is purchased from Xingwang food limited in Foshan city, and the dendrobium extract is purchased from Xianhhang Yue biotechnology limited with the specification of 5: 1.

Example 3

Embodiment 3 of the present invention provides a totarol microcapsule, which is specifically prepared by the following steps:

(1) grinding totarol to 1200-mesh fine particles, quantitatively pouring 20kg of totarol into a fluidized bed;

(2) mixing 10kg erythritol, 20kg mannitol and totarol powder at 500m³Performing high-speed jet flow for 10min at the wind speed of 650rpm per hour to prepare an inner core layer;

(3) the buffer layer raw materials of 25kg of microcrystalline cellulose, 15kg of xanthan gum and 10kg of glutinous rice starch are 970m³Performing high-speed jet flow for 10min at the wind speed of 750rpm per hour to obtain a buffer layer;

(4) mixing 1.2kg xanthan gum, 5.25kg herba Dendrobii extract, and 0.15kg caramel pigment at 820m³The wind speed is/h, the rotating speed is 880rpm, and high-speed jet flow is carried out for 10min, so that the raw material of the outer shell layer is adhered to the surface of the buffer layer;

(5) top spray drying, 55 deg.C hot air, 1050m³Drying for 35min, and performing rounding granulation to prepare particles with uniform particle size.

The microcrystalline cellulose is purchased from Hebei hongtao bioengineering limited, the xanthan gum is purchased from Zhonghong bioengineering limited in Anhui, the sticky rice starch is purchased from Xingwang food limited in Foshan city, and the dendrobium extract is purchased from Xianhhang Yue biotechnology limited with the specification of 5: 1.

Example 4

The embodiment 4 of the present invention provides a totarol microcapsule, and the specific implementation manner of the specific preparation method is the same as that in embodiment 1, except that the step (2) is: mixing 30kg erythritol and totarol powder with a weight of 500m³The inner core layer is prepared by jetting at high speed for 10min at the wind speed of 650rpm per hour.

Example 5

The embodiment 5 of the present invention provides a totarol microcapsule, and the specific implementation manner of the specific preparation method is the same as that in embodiment 1, except that the step (2) is: mixing mannitol 30kg and totarol powder 500m³The inner core layer is prepared by jetting at high speed for 10min at the wind speed of 650rpm per hour.

Example 6

Embodiment 6 of the present invention provides a totarol microcapsule, and the specific preparation method is as follows:

(1) grinding totarol to 1000-mesh fine particles, quantitatively pouring 20kg of totarol into a fluidized bed;

(2) mixing 12kg erythritol, 18kg mannitol and totarol powder at a ratio of 500m³Performing high-speed jet flow for 10min at the wind speed of 650rpm per hour to prepare an inner core layer;

(3) the buffer layer raw materials of 22kg of microcrystalline cellulose, 13kg of xanthan gum and 10kg of glutinous rice starch are 970m³Performing high-speed jet flow for 10min at the wind speed of 750rpm per hour to obtain a buffer layer;

(4) mixing 1kg xanthan gum, 4.5kg Curcuma rhizome extract, and 0.15kg caramel pigment at 820m³The wind speed is/h, the rotating speed is 880rpm, and high-speed jet flow is carried out for 10min, so that the raw material of the outer shell layer is adhered to the surface of the buffer layer;

(5) top spray drying, 55 deg.C hot air, 1050m³Drying for 35min, and performing rounding granulation to prepare particles with uniform particle size.

The microcrystalline cellulose is purchased from Hebei hongtao bioengineering limited, the xanthan gum is purchased from Zhonghong bioengineering limited in Anhui, the sticky rice starch is purchased from Xingwang food limited in Foshan city, the turmeric extract is purchased from West Anchang Yue biotechnology limited, and the product specification is as follows: 95% curcumin, 10: 1.

Performance evaluation

1. Nucleation stability: 10 parts of the inner core layer formed in the step (2) of each of examples 1 to 6 were taken, the particle diameters thereof were measured, and the relative standard deviation of the particle diameters of each example was calculated, and if it was not more than 5%, it was regarded as being acceptable, otherwise it was regarded as being unacceptable.

2. Sensory evaluation: the handfeel of the totarol microcapsules obtained in examples 1 to 6 was evaluated, respectively, and the handfeel was found to be excellent, soft, slightly rough, and good; the harsh hand was marked as poor.

TABLE 1

The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.