Preserved calculus bovis coating and preparation method thereof

Abstract

The invention relates to the technical field of film coatings, and discloses a coating for preserving calculus bovis. The coating is prepared from the following components in percentage by weight: 30 to 40 weight percent of acrylic resin IV, 25 to 35 weight percent of hydroxypropyl methylcellulose, 10 to 15 weight percent of beewax, 5 to 10 weight percent of junci medulla extract, 5 to 10 weight percent of antistatic agent, 5 to 10 weight percent of plasticizer and a proper amount of 95 percent ethanol solution. The invention also discloses a preparation method of the coating for preserving calculus bovis. According to the invention, the junci medulla extracting solution is added into the coating component, so that the moisture resistance of the coated bezoar is remarkably improved, and meanwhile, junci medulla has a pharmacological synergistic effect, so that the stability of the coating material and the quality of the preserved bezoar are further improved; the intermittent sinusoidal alternating current is applied in an auxiliary manner when the junci medulla extracting solution is added, so that the integrity, moisture resistance and taste masking effect of the coated bezoar are greatly improved, and the quality of the preserved bezoar is further ensured.

Description

Technical Field

[0001] The invention relates to the technical field of film coatings, in particular to a coating for preserving bezoar and a preparation method thereof. Background Art

[0002] As a precious Chinese medicinal material, bezoar has extremely high medicinal value in the field of traditional Chinese medicine. It has the effects of clearing the heart, removing phlegm, opening the orifices, cooling the liver, calming the wind, and detoxifying, and is widely used in a variety of Chinese medicine preparations. Bezoar is mainly composed of bile pigments, bile acid, cholesterol, fatty acids and various amino acids. This complex chemical composition makes its properties relatively unstable. On the one hand, bezoar has strong hygroscopicity. Under high humidity conditions, bezoar easily absorbs moisture in the air, causing its texture to become soft, sticky, and even moldy and deteriorating, greatly shortening the shelf life of bezoar. On the other hand, bezoar itself has a special smell, which may not only affect the patient's medication experience, but also during storage, the emission of odor may indicate changes in certain components, thereby affecting its quality stability.

[0003] At present, common methods for the preservation of bezoar include conventional means such as dry storage and sealed storage. However, these methods have obvious limitations. Although simple dry storage can reduce the impact of moisture on bezoar to a certain extent, it cannot completely isolate the intrusion of external moisture, especially in an environment with high humidity, and the preservation effect is not good. If the moisture-proof performance of the packaging material is insufficient for sealed storage, it is also difficult to prevent bezoar from getting damp and deteriorating.

[0004] In order to improve the preservation of bezoar, some studies have tried to use coating technology. Traditional coating materials, such as simple sugar coating or general polymer coating, can play a protective role to a certain extent, but the effect in terms of moisture resistance and taste masking is not satisfactory. Sugar coating easily absorbs moisture and dissolves, losing the protection of bezoar; general polymer coating cannot effectively prevent moisture penetration, and has limited effect on masking the odor of bezoar.

[0005] The present invention aims to provide an innovative coating and preparation method for preserving bezoar. By selecting specific coating materials and optimizing the preparation process, the moisture-proof and taste-masking problems of bezoar during the preservation process are effectively solved, the quality stability and medicinal value of bezoar are improved, and the gap in the existing bezoar preservation technology is filled. Summary of the invention

[0006] The object of the present invention is to provide a coating for preserving bezoar and a preparation method thereof, so as to solve the problems raised in the above-mentioned background technology.

[0007] To achieve the above object, the present invention provides the following technical solutions:

[0008] A coating for preserving bezoar, which is composed of the following components by weight percentage: acrylic resin IV: 30–40wt%, hypromellose: 25-35wt%, beeswax: 10-15wt%, rush extract: 5-10wt%, antistatic agent: 5-10wt%, plasticizer: 5-10wt%, and appropriate amount of 95% ethanol solution.

[0009] As a further scheme of the present invention: the coating is composed of the following components by weight percentage: acrylic resin IV: 35wt%, hypromellose: 30wt%, beeswax: 12.5wt%, rush extract: 7.5wt%, antistatic agent: 7.5wt%, plasticizer: 7.5wt%, and appropriate amount of 95% ethanol solution.

[0010] As a further scheme of the present invention: the antistatic agent is talc powder, and the plasticizer is polyethylene glycol 6000.

[0011] Among the above components, the acrylic resin IV serves as the main taste masking ingredient, forming a film on the surface of bezoar to mask its bad smell; the hypromellose can form a continuous coating film, providing moisture-proof performance, and at the same time having good film-forming property and stability; the beeswax can enhance the hydrophobicity of the coating film and further improve the moisture-proof ability; while the rush extract has a certain pharmacological synergistic effect and also has a potential improvement in moisture-proof performance; the talc powder can not only be used as an antistatic agent but also as a glidant, reducing electrostatic adsorption during the coating process, ensuring the uniformity of the coating, and improving the fluidity of the material; and polyethylene glycol 6000 is used as a plasticizer to enhance the flexibility of the coating film and prevent the film coating from cracking during storage and use.

[0012] A preparation method of a coating for preserving bezoar, comprising the following steps:

[0013] S1. Raw material preparation: Weigh the corresponding weights of acrylic resin IV and hypromellose and add them to an appropriate amount of 95% ethanol solution respectively, and stir to fully dissolve the above components to form a uniform and stable acrylic resin IV solution and hypromellose solution.

[0014] S2. Mixing and melting: Mix and stir the dissolved acrylic resin IV solution and hypromellose solution together, and add the melted and filtered beeswax, and continuously stir to make it evenly dispersed in the mixed solution.

[0015] S3. Adding rush extract: Heat up the mixed solution obtained in step S2, and add 0.04-0.08 mL of rush extract to the mixed solution once every 5-7 minutes until the addition of rush extract is completed, and apply a sinusoidal alternating current to the mixed solution each time the rush extract is added.

[0016] S4. Adding adjuvants: Add antistatic agents and plasticizers to the mixed solution obtained in step S3 in sequence, and continuously stir while maintaining the temperature at 60 - 80 °C to ensure that each component is evenly dispersed, forming a stable coating solution.

[0017] As a further solution of the present invention: The preparation method of the Juncus effusus extract includes the following steps:

[0018] 1) Select dry, non-moldy, and high-quality Juncus effusus raw materials, and crush them. Juncus effusus is the dried stem pith of the plant Juncus effusus in the family Juncaceae, and those with long strips, thick and strong, white color, and elasticity are preferred. The particle size after crushing can be controlled to pass through a 20 - 60 mesh sieve, which can not only increase the contact area between the solvent and the raw material in the subsequent extraction process and improve the extraction efficiency, but also prevent excessive impurities from being dissolved due to overly fine particles.

[0019] 2) Select ethyl acetate as the extraction solvent. Ethyl acetate has good solubility and can effectively dissolve various chemical components in Juncus effusus. At the same time, its boiling point is moderate (about 77 °C), which is convenient for subsequent separation and recovery. Using the reflux extraction method, according to the solid-liquid ratio of 1:8 - 1:12 g / mL, place the Juncus effusus powder and ethyl acetate in a round-bottom flask, connect the reflux condenser, and reflux extract at a slightly boiling state of 78 - 80 °C for 2 - 4 times, with each extraction time being 1.5 - 2.5 hours;

[0020] 3) After the extraction is completed, quickly filter the extract through filter paper or filter cloth while it is hot to remove insoluble impurities such as incompletely crushed plant fibers and sediment, obtaining a clear filtrate.

[0021] 4) Transfer the filtered ethyl acetate extract to the distillation flask of a rotary evaporator and perform distillation concentration under reduced pressure to quickly volatilize the ethyl acetate, thereby obtaining a concentrated Juncus effusus ethyl acetate extract. Set the temperature at 40 - 50 °C and the vacuum degree at -0.08 Mpa. This can quickly volatilize the ethyl acetate, thereby obtaining a concentrated Juncus effusus ethyl acetate extract. Distillation under reduced pressure can lower the boiling point of the solvent and reduce the loss of heat-sensitive components.

[0022] 5) Transfer the concentrated extract to a dryer and dry it to a constant weight at a temperature of 40 - 50 °C under a vacuum condition with a vacuum degree of -0.09 Mpa to remove the remaining small amount of solvent, finally obtaining the solid structure of the Juncus effusus extract.

[0023] As a further solution of the present invention: In step S3, the application time of the sinusoidal alternating current starts from 1 - 2 minutes before the addition of the Juncus effusus extract to 1 - 2 minutes after the addition of the Juncus effusus extract.

[0024] As a further solution of the present invention: in step S3, the frequency of the sinusoidal alternating current is 40 - 50 Hz, and the period is 0.02 - 0.025 s.

[0025] As a further solution of the present invention: in step S3, the heating temperature is controlled at 120 - 130 °C.

[0026] As a further solution of the present invention: the total stirring time is controlled at 2 - 3 hours, and the stirring speed is controlled at 300 - 500 rpm.

[0027] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0028] 1. By adding the extract of Juncus effusus L. to the coating components, the present invention significantly improves the moisture-proof performance of the coated calculus bovis. At the same time, Juncus effusus L. itself also has a pharmacological synergistic effect, further improving the stability of the coating material and the quality of calculus bovis after storage.

[0029] 2. By applying intermittent sinusoidal alternating current when adding the extract of Juncus effusus L., the present invention greatly improves the integrity, moisture-proof property and taste-masking effect of the coated calculus bovis, further ensuring the quality of calculus bovis after storage. Specific Embodiments

[0030] Next, the technical solutions in the present invention will be clearly and completely described in conjunction with multiple embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0031] Example 1

[0032] In an embodiment of the present invention, a coating for preserving calculus bovis is composed of the following components in weight percentage: acrylic resin IV: 30 g, hypromellose: 25 g, beeswax: 10 g, extract of Juncus effusus L.: 5 g, talc powder: 5 g, polyethylene glycol 6000: 5 g.

[0033] The preparation method of the above coating is as follows:

[0034] S1. Raw material preparation: Weigh the corresponding weights of acrylic resin IV and hypromellose and add them to appropriate 95% ethanol solutions respectively, and stir to fully dissolve the above components to form a uniform and stable acrylic resin IV solution and hypromellose solution.

[0035] S2. Mixing and melting: Mix the dissolved acrylic resin Ⅳ solution and hydroxypropyl methylcellulose solution together by stirring, and add the melted and filtered beeswax, then continue stirring to make it evenly dispersed in the mixed solution;

[0036] S3. Adding Juncus effusus extract: Heat up the mixed solution obtained in step S2, control the heating temperature at 125 °C, add 0.06 mL of Juncus effusus extract to the mixed solution every 6 minutes until the addition of Juncus effusus extract is completed. And apply a sinusoidal alternating current to the mixed solution each time when adding Juncus effusus extract. The application time of the sinusoidal alternating current starts from 1.5 minutes before the addition of Juncus effusus extract to 1.5 minutes after the addition of Juncus effusus extract. The frequency of the sinusoidal alternating current is 45 Hz, and the period is 0.0225 s;

[0037] The preparation method of the above Juncus effusus extract solution includes the following steps:

[0038] 1) Select dry, non-mildewed and high-quality Juncus effusus raw materials, crush them, and the particle size after crushing can be controlled to pass through a 40-mesh sieve;

[0039] 2) Select ethyl acetate as the extraction solvent, adopt the reflux extraction method, according to the material-liquid ratio of 1:10 g / mL, put the Juncus effusus powder and ethyl acetate into a round-bottom flask, connect the reflux condensation device, and reflux and extract 3 times at a slightly boiling state of 79 °C, with each extraction time being 2 hours;

[0040] 3) After the extraction is completed, quickly filter the extract through filter paper or filter cloth while it is hot to remove the insoluble impurities therein;

[0041] 4) Transfer the filtered ethyl acetate extract to the distillation flask of a rotary evaporator, and carry out distillation and concentration under reduced pressure to quickly volatilize the ethyl acetate, so as to obtain a concentrated Juncus effusus ethyl acetate extract, with the temperature set at 45 °C and the vacuum degree set at -0.08 Mpa;

[0042] 5) Transfer the concentrated extract to a dryer, and dry it to constant weight at a temperature of 45 °C under a vacuum condition with a vacuum degree of -0.09 Mpa to remove the remaining small amount of solvent, and finally obtain the solid structure of the Juncus effusus extract.

[0043] S4. Adding auxiliary agents: Add an antistatic agent and a plasticizer to the mixed solution obtained in step S3 in sequence, and keep stirring at a temperature of 70 °C. The total stirring time is controlled at 2.5 hours, and the stirring speed is controlled at 400 rpm to ensure that each component is evenly dispersed to form a stable coating solution.

[0044] Example 2

[0045] The difference between the embodiment of the present invention and Embodiment 1 is that the coating is composed of the following components by weight percentage: acrylic resin IV: 40 g, hydroxypropyl methylcellulose: 35 g, beeswax: 15 g, rush extract: 10 g, talcum powder: 10 g, polyethylene glycol 6000: 10 g.

[0046] Example 3

[0047] The difference between the embodiment of the present invention and Embodiment 1 is that the coating is composed of the following components by weight percentage: acrylic resin IV: 35 wt%, hydroxypropyl methylcellulose: 30 g, beeswax: 12.5 g, rush extract: 7.5 g, talcum powder: 7.5 g, polyethylene glycol 6000: 7.5 g.

[0048] Example 4

[0049] The difference between the embodiment of the present invention and Embodiment 3 is that the temperature of the mixed solution is raised to 120 °C, and 0.04 mL of rush extract is added to the mixed solution every 5 min, with a total of 4 additions.

[0050] Example 5

[0051] The difference between the embodiment of the present invention and Embodiment 3 is that the temperature of the mixed solution is raised to 130 °C, and 0.08 mL of rush extract is added to the mixed solution every 7 min, with a total of 6 additions.

[0052] Example 6

[0053] The difference between the embodiment of the present invention and Embodiment 3 is that a sinusoidal alternating current is applied to the mixed solution each time the rush extract is added, and the application time of the sinusoidal alternating current starts from 1 min before the addition of the rush extract to 1 min after the addition of the rush extract.

[0054] Example 7

[0055] The difference between the embodiment of the present invention and Embodiment 3 is that a sinusoidal alternating current is applied to the mixed solution each time the rush extract is added, and the application time of the sinusoidal alternating current starts from 2 min before the addition of the rush extract to 2 min after the addition of the rush extract.

[0056] Example 8

[0057] The difference between the embodiment of the present invention and Embodiment 3 is that the frequency of the sinusoidal alternating current is 40 Hz and the period is 0.025 s.

[0058] Example 9

[0059] The difference between the embodiment of the present invention and Embodiment 3 is that the frequency of the sinusoidal alternating current is 50 Hz and the period is 0.02 s.

[0060] Comparative Example 1

[0061] The difference between the embodiment of the present invention and Embodiment 3 is that the weight percentage components of the coating do not contain the extract of Juncus effusus.

[0062] Comparative Example 2

[0063] The difference between the embodiment of the present invention and Embodiment 3 is that a sinusoidal alternating current is not applied to the mixed solution each time the extract of Juncus effusus is added.

[0064] The coating solutions prepared in the above embodiments and comparative examples are used to coat bezoar. After that, quality inspection is carried out on the coated bezoar, including the detection of indicators such as appearance, coating integrity, moisture-proof performance, and taste masking effect. The specific process of the coating operation is as follows:

[0065] 1) Place the bezoar in a coating pan and rotate the coating pan at a speed of 20 - 30 rpm;

[0066] 2) Uniformly spray the prepared coating solution on the surface of the bezoar through a spray gun, control the spray gun pressure at 0.2 - 0.4 MPa, and the liquid spraying speed at 5 - 10 mL / min, so that the coating solution can uniformly cover the bezoar particles;

[0067] 3) During the coating process, control the temperature at 30 - 40 °C, keep the air in the pan flowing through a blowing device, accelerate the volatilization of ethanol, and make the coating film dry and solidify quickly;

[0068] 4) After the coating is completed, continue to dry the coated bezoar at 30 - 40 °C for 1 - 2 hours to further solidify the coating film and improve its stability.

[0069] Appearance detection: Under natural light or bright white light, directly observe the appearance of the coated bezoar with the naked eye. The observation content includes color, luster, shape, etc.

[0070] Coating integrity detection: Place a certain number of coated bezoars on an oscillator and vibrate them at a certain frequency (such as 100 - 200 times / minute) and amplitude (such as 5 - 10 mm) for 5 - 10 minutes, and then observe whether there are any cracks or peeling off phenomena on the coating.

[0071] Moisture-proof performance detection: Take a certain weight (accurate to 0.0001 g) of coated bezoar, place it in a desiccator containing saturated sodium chloride solution (relative humidity about 75%), control the temperature at 25°C ± 1°C, and place it for a certain period of time (such as 72 hours). Immediately weigh it after taking it out and calculate the weight gain rate.

[0072] Taste masking effect detection: Select 10 - 20 trained evaluators, let them taste a small amount of coated bezoar respectively (simulating the actual taking situation), and score the taste masking effect according to the pre-established sensory evaluation criteria. The evaluation criteria can be divided into 5 levels, 5 points for completely no strange smell, 4 points for slight strange smell, 3 points for acceptable strange smell, 2 points for obvious strange smell, and 1 point for strong and unacceptable strange smell.

[0073] The results of the above various quality inspections are shown in Table 1 below:

[0074]

[0075]

[0076] Table 1

[0077] Conclusion 1: Taking Examples 1 - 3 and Comparative Example 1 as experimental controls, it can be seen that different ratios in the coating components will have a certain impact on the integrity and moisture-proof property of coated bezoar. The indicators in Example 3 are the best. Without adding the extract of Juncus effusus L., the moisture-proof performance and taste masking effect of coated bezoar will be significantly reduced, and the integrity of coated bezoar will also be affected.

[0078] Conclusion 2: Taking Examples 3 - 5 as experimental controls, it can be seen that the addition amount, addition time, and addition temperature of the extract of Juncus effusus L. will all have a certain impact on the quality of coated bezoar, and the indicators in Example 5 are the best. However, the amount of the extract of Juncus effusus L. consumed in Example 5 is also the largest, and the required temperature power consumption is also high. And the overall improvement of these indicators compared to Example 3 is not too large. Therefore, from the perspective of cost, the indicator parameters of Example 3 are obviously still the best.

[0079] Conclusion 3: Taking Example 3, Examples 6 - 7, and Comparative Example 2 as experimental controls, it can be seen that the application time of sinusoidal alternating current has a certain impact on the quality of coated bezoar. Through comparison with Comparative Example 2, it can be known that without the auxiliary effect of sinusoidal alternating current, the improvement effect of the extract of Juncus effusus L. on the quality of coated bezoar is lower than that of Examples 3, 6 - 7. And if the application time of sinusoidal alternating current is too long or too short, the integrity, moisture-proof property, and taste masking effect of coated bezoar will all decline compared to Example 3. Therefore, through comparison, it can be seen that the quality indicators of Example 3 are still the best.

[0080] Conclusion 4: Taking Examples 3, 8 - 9 as experimental controls, it can be concluded that the parameters of sinusoidal alternating current have a certain impact on the quality of coated bezoar, and through comparison, it can be seen that the quality indicators of Example 3 are the best.

[0081] Conclusion 5: Through experimental comparison of Examples 1 - 9, Comparative Examples 1 - 2 and the blank control group, it is obtained that there is a huge improvement in the integrity and moisture-proof property of bezoar after coating. Obviously, the coated bezoar will have a longer storage time without affecting its medicinal efficacy.

[0082] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and without departing from the spirit or basic characteristics of the present invention, the present invention can be implemented in other specific forms. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present invention.

[0083] In addition, it should be understood that although this specification is described according to embodiments, not each embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A coating for preserving bezoar, characterized in that: The coating consists of the following components in percentage by weight: Composition: acrylic resin IV: 30-40wt%, hydroxypropyl methylcellulose: 25-35wt%, beeswax: 10-15wt%, rush extract: 5-10wt%, antistatic agent: 5-10wt%, plasticizer: 5-10wt%, 95% ethanol solution in appropriate amount.

2. A coating for preserving bezoar according to claim 1, characterized in that, The coating consists of the following components in percentage by weight: Composition: acrylic resin IV: 35wt%, hydroxypropyl methylcellulose: 30wt%, beeswax: 12.5wt%, rush extract: 7.5wt%, antistatic agent: 7.5wt%, plasticizer: 7.5wt%, 95% ethanol solution in appropriate amount.

3. A coating for preserving bezoar according to claim 1, characterized in that, The antistatic agent is talcum powder, and the plasticizer is polyethylene glycol 6000.

4. A method for preparing a coating for preserving bezoar according to any one of claims 1 to 3, characterized in that: The steps include: S1. Raw material preparation: Weigh corresponding weights of acrylic resin IV and hydroxypropyl methylcellulose, add them into an appropriate amount of 95% ethanol solution, stir to fully dissolve the above components, and form a uniform and stable acrylic resin IV solution and hydroxypropyl methylcellulose solution; S2, mixing and melting: the dissolved acrylic resin IV solution and the hydroxypropyl methylcellulose solution are mixed and stirred together, and the melted and filtered beeswax is added, and the mixture is stirred continuously to be evenly dispersed in the mixed solution; S3, adding rush extract: heating the mixed solution obtained in step S2, adding 0.04-0.08 mL of rush extract to the mixed solution every 5-7 minutes until the rush extract is added, and applying sinusoidal alternating current to the mixed solution each time the rush extract is added; S4, adding auxiliary agents: adding antistatic agent and plasticizer to the mixed solution obtained in step S3 in sequence, and maintaining the temperature at 60-80° C. and continuously stirring to ensure that all ingredients are evenly dispersed to form a stable coating solution.

5. The method for preparing a coating for preserving bezoar according to claim 4, characterized in that: The preparation method of the Juncus effusus extract comprises the following steps: 1) Select dry, mildew-free, high-quality rush materials and crush them to a particle size that can pass through a 20-60 mesh sieve; 2) ethyl acetate is selected as the extraction solvent, and a reflux extraction method is adopted. According to a solid-liquid ratio of 1:8-1:12 g / mL, rush powder and ethyl acetate are placed in a round-bottom flask, and a reflux condenser is connected. Reflux extraction is performed 2-4 times at a slightly boiling state of 78-80° C., and each extraction time is 1.5-2.5 hours; 3) After the extraction is completed, filter the extract through filter paper or filter cloth while it is hot to remove insoluble impurities; 4) transferring the filtered ethyl acetate extract to a distillation bottle of a rotary evaporator, distilling and concentrating under reduced pressure to volatilize the ethyl acetate quickly, thereby obtaining a concentrated ethyl acetate extract of Juncus effusus, the temperature being set at 40-50° C. and the vacuum degree being set at -0.08 Mpa; 5) The concentrated extract is transferred to a dryer and dried to constant weight at a vacuum degree of -0.09 MPa and a temperature of 40-50° C. to remove a small amount of residual solvent, thereby finally obtaining a solid structure of the Juncus effusus extract.

6. The method for preparing a coating for preserving bezoar according to claim 4, characterized in that: In step S3, the sinusoidal alternating current is applied from 1 to 2 minutes before the addition of the Juncus effusus extract to 1 to 2 minutes after the addition of the Juncus effusus extract.

7. The method for preparing a coating for preserving bezoar according to claim 4, characterized in that: In step S3, the frequency of the sinusoidal alternating current is 40-50 Hz, and the period is 0.02-0.025 s.

8. The method for preparing a coating for preserving bezoar according to claim 4, characterized in that: In step S3, the heating temperature is controlled at 120-130°C.

9. The method for preparing a coating for preserving bezoar according to claim 4, characterized in that: The total stirring time is controlled at 2-3 hours, and the stirring speed is controlled at 300-500rpm.

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