阅读说明：本技术 一种金莲花口服液制备工艺 (Preparation process of flos Trollii oral liquid ) 是由 胡林水 王成芳 潘燕 雷蔚雯 吴静之 吴明 于 2020-05-18 设计创作，主要内容包括：本发明公开了一种金莲花口服液制备工艺,具体包括以下步骤：(1)酶解；(2)高速离心；(3)絮凝滤过；(4)微滤；(5)减压浓缩；(6)灌装。本发明优化了金莲花口服液制备工艺,采用酶解-高速离心-絮凝滤过-微滤法联合制备生产金莲花口服液,工艺步骤简单,易于操作,相对于传统的水煎煮工艺,耗水量及能耗大大降低,且生产周期大大缩短,在有效保留了药材中的总黄酮等有效成分的同时,还能有效改善产品的澄清度和稳定性,值得推广应用。(The invention discloses a preparation process of a tropaeolum oral liquid, which specifically comprises the following steps: (1) carrying out enzymolysis; (2) centrifuging at a high speed; (3) flocculation filtration; (4) microfiltration; (5) concentrating under reduced pressure; (6) and (6) filling. The preparation process of the tropaeolum oral liquid is optimized, the preparation and production of the tropaeolum oral liquid are carried out by adopting the enzymolysis-high-speed centrifugation-flocculation filtration-microfiltration method, the steps of the process are simple, the operation is easy, compared with the traditional water decoction process, the water consumption and the energy consumption are greatly reduced, the production period is greatly shortened, the active ingredients such as total flavone in medicinal materials are effectively kept, meanwhile, the clarity and the stability of the product can be effectively improved, and the preparation method is worthy of popularization and application.)

1. The preparation process of the tropaeolum oral liquid is characterized by comprising the following steps of:

(1) enzymolysis: crushing trollius chinensis, adding water, adjusting the pH of a liquid material to 4.5-5.0, adding a complex enzyme, heating to 40-50 ℃ for enzymolysis, and inactivating the enzyme to obtain an enzymatic hydrolysate;

(2) high-speed centrifugation: centrifuging the enzymolysis liquid at high speed, and taking supernatant;

(3) flocculation filtration: heating the supernatant to 40-50 ℃, slowly dripping a chitosan acetic acid solution under a stirring state, adding talcum powder after stirring, uniformly stirring, standing for 20-30 min, and filtering to obtain a filtrate;

(4) and (3) microfiltration: microfiltering the filtrate through a hollow fiber filter membrane, and collecting the filtrate;

(5) and (3) concentrating under reduced pressure: concentrating the filtrate under reduced pressure to relative density of 1.15 + -0.2 (50 deg.C), standing, and filtering to obtain extractive solution;

(6) filling: adding adjuvants into the extractive solution, diluting with purified water, mixing, standing, filtering, bottling, sterilizing, and detecting leakage to obtain flos Trollii oral liquid.

2. The preparation process of the trollius chinensis oral liquid according to claim 1, wherein in the step (1), the grain size of the pulverized trollius chinensis is 10-20 meshes.

3. The preparation process of the tropaeolum oral liquid according to claim 1, wherein in the step (1), the liquid-material ratio is (20-25): 1.

4. the preparation process of the tropaeolum oral liquid according to claim 1, characterized in that in the step (1), the concentration of the complex enzyme in the liquid material is 0.3-0.5 mg/ml, and the complex enzyme comprises the following enzymes in parts by weight: 30-40 parts of cellulase, 20-30 parts of pectinase, 20-30 parts of hemicellulase, 5-10 parts of subtilisin and 3-5 parts of amylase; the enzymolysis time is 80-100 min.

5. The process for preparing an oral liquid of flos Trollii according to claim 1, wherein in step (1), high purity nitrogen or inert gas is introduced into the liquid material for bubbling and stirring during enzymolysis.

6. The process for preparing an oral liquid of flos Trollii according to claim 1, wherein in step (2), the rotation speed of high speed centrifugation is 10000-20000 r/min.

7. The preparation process of the tropaeolum oral liquid according to claim 1, characterized in that in the step (3), the mass concentration of the chitosan acetic acid solution is 1%, the adding amount of the chitosan acetic acid solution is 300-350 mg/L by volume of the supernatant, and the adding amount of the talcum powder is 3-5% by mass of the supernatant.

8. The preparation process of the tropaeolum oral liquid according to claim 1, characterized in that in the step (3), after the chitosan acetic acid solution is dripped, the stirring speed is 40-80 r/min, and the stirring time is 2-4 min.

9. The process for preparing an oral liquid of tropaeolum according to claim 1, wherein in step (4), the aperture of the hollow fiber filter membrane is 0.3-0.5 μm.

10. The preparation process of the tropaeolum oral liquid according to claim 1, characterized in that in step (6), the auxiliary materials comprise at least one of preservative, surfactant, flavoring agent and antioxidant.

Technical Field

The invention relates to a tropaeolum oral liquid, in particular to a preparation process of the tropaeolum oral liquid.

Background

The flos Trollii oral liquid is a Chinese patent medicine potion prepared by taking flos Trollii as a main raw material, has good antibacterial and anti-inflammatory effects, is widely applied to upper respiratory tract infection, tonsillitis, pharyngitis and other diseases caused by internal heat toxin, and is used for daily health care or treatment needs.

The trollius chinensis oral liquid is usually prepared by adopting a traditional water decoction process, the process keeps active ingredients such as total flavonoids in medicinal materials, but consumes a large amount of water, so that the subsequent evaporation concentration time is long, the energy consumption is high, and meanwhile, impurities (protein, tannin and the like) are leached more in the traditional decoction process of the trollius chinensis for a plurality of times and a long time, so that the load is increased for the subsequent filtration and impurity removal of an oral liquid preparation, the impurities cannot be effectively removed, precipitates can be generated, and the appearance quality and the clarity of the product are influenced.

For example, chinese patent application No. 2009100825569 discloses a preparation method of a tropaeolum oral liquid, which specifically discloses: adding water solution 25 times of the weight of the raw materials into flos Trollii, heating the mixture to 95 deg.C under stirring, stirring for 40 min, centrifuging to obtain extractive solution, removing residue, freezing and concentrating the medicinal solution to 10% of the total medicinal solution, centrifuging to remove macromolecular micelle in the medicinal solution, concentrating the medicinal solution to obtain flos Trollii extract, and making into oral liquid by conventional method. The preparation method has the following defects: (1) the extraction temperature is as high as 95 ℃, and the stability of the trollius chinensis total flavonoids can be influenced, so that the loss of the trollius chinensis total flavonoids is caused; (2) the high-speed centrifugation method is used for removing impurities from the liquid medicine (high-speed centrifugation clarification process), but the centrifugation method is too simple, and components such as polysaccharide and mucoid are not easy to completely remove, so that the clarity of the product is poor, secondary precipitates such as wall-sticking substances and sediments are easy to generate, the stability is poor, and the appearance quality of the product is influenced.

Disclosure of Invention

The invention aims to solve the technical problems of the preparation method of the trollius chinensis flower oral liquid in the prior art, and provides the preparation process of the trollius chinensis flower oral liquid, which has the advantages of simple process steps, easiness in operation, reduction in production cost, reduction in loss of effective components of the trollius chinensis flower, and improvement in product clarity and stability.

In order to achieve the purpose, the invention adopts the following technical scheme: a preparation process of a tropaeolum oral liquid comprises the following steps:

(1) enzymolysis: crushing the trollius chinensis bunge, adding water, adjusting the pH of a liquid material to 4.5-5.0, adding a complex enzyme, heating to 40-50 ℃ for enzymolysis, and inactivating the enzyme to obtain an enzymatic hydrolysate. The method has the advantages that the trollius chinensis bunge is crushed and then subjected to enzymolysis, the crushing can increase the specific surface area of the trollius chinensis bunge, the dissolution of active ingredients in the trollius chinensis bunge is accelerated, the full enzymolysis is facilitated, and the production period is shortened; in the invention, the pH of the feed liquid is particularly limited to be 4.5-5.0, and the following purposes are mainly considered: firstly, the pH value is 4.5-5.0, which is the optimum pH value of the complex enzyme; secondly, the pH value is 4.5-5.0, and the total flavonoids as main functional components in the trollius chinensis bunge show better stability; thirdly, the pH value is 4.5-5.0, the flocculation effect of chitosan in the subsequent process is the best, the pH value is too low, most particles in the system have positive charges and can generate electrostatic repulsion with the chitosan with the positive charges, so that colloid particles are difficult to remove, the system is turbid, the pH value is too high, negative electricity particles in the system are increased, the charge of the neutralization effect of the chitosan with the positive charges is increased, the effect of a compressed double electric layer is gradually weakened, and the flocculation effect is influenced; in the invention, the enzymolysis stability is strictly limited to 40-50 ℃, the temperature range is the proper enzymolysis temperature of the complex enzyme, and the temperature is favorable for accelerating the dissolution of effective components in the trollius chinensis; because effective components such as general flavone in the trollius chinensis bunge exist in cells with hard cell walls, the traditional water or organic solvent extraction method has poor effect, so that the complex enzyme is adopted to carry out enzymolysis on the trollius chinensis bunge, the cell walls are loosened, expanded and broken, the permeability of the cell walls is changed, the effective components in the cells can be quickly and fully dissolved out, the extraction time is greatly shortened, and the extraction efficiency is improved.

(2) High-speed centrifugation: and (4) carrying out high-speed centrifugation on the enzymolysis liquid, and taking supernatant. The high-speed centrifugation is a physical separation method, and has the advantages of convenient operation, short working hours, low production cost, less loss of effective components and the like.

(3) Flocculation filtration: heating the supernatant to 40-50 ℃, slowly dripping a chitosan acetic acid solution under a stirring state, adding talcum powder after stirring, uniformly stirring, standing for 20-30 min, and filtering to obtain a filtrate. After high-speed centrifugation, a small amount of components such as polysaccharide, mucilage and the like are contained in the supernatant, so that the supernatant needs to be further subjected to impurity removal, chitosan can effectively retain effective components, the safety is good, and the cost is low.

(4) And (3) microfiltration: and (4) performing microfiltration on the filtrate through a hollow fiber filter membrane, and collecting and filtering out clear liquid. According to the invention, the hollow fiber filter membrane is adopted to carry out microfiltration on the filtrate, so that the treatment is convenient, the working hours are short, the treatment cost is low, the treatment capacity is large, the regeneration of the hollow fiber filter membrane is convenient, and the clarification is further improved by carrying out microfiltration to further remove impurities.

(5) And (3) concentrating under reduced pressure: concentrating the filtrate under reduced pressure to relative density of 1.15 + -0.2 (50 deg.C), standing, and filtering to obtain extractive solution.

(6) Filling: adding adjuvants into the extractive solution, diluting with purified water, mixing, standing, filtering, bottling, sterilizing, and detecting leakage to obtain flos Trollii oral liquid. The addition of auxiliary materials and the dilution with purified water are conventional means in the field for preparing the tropaeolum oral liquid, and are not repeated; the sterilization can adopt high-pressure steam sterilization, and the specific steps are as follows: sterilizing the filled flos Trollii oral liquid in a high pressure steam sterilizing pot at 121 deg.C for 30min, and taking out.

Preferably, in the step (1), the particle size of the pulverized trollius chinensis bunge is 10-20 meshes. The flos Trollii is crushed mainly for increasing the specific surface area of the medicine to improve the bioavailability and accelerate the leaching of effective components in the flos Trollii, but the smaller the crushing, the better the particle size, the too small particle size, the more fine impurities, the adverse effect on the subsequent removal of impurities, and the too large particle size, which influences the enzymolysis efficiency and the dissolution of index components, so the crushed particle size of the flos Trollii is controlled to be 10-20 meshes.

Preferably, in the step (1), the liquid-material ratio is (20-25): 1.

preferably, in the step (1), the concentration of the complex enzyme in the liquid material is 0.3-0.5 mg/ml, and the complex enzyme comprises the following enzymes in parts by weight: 30-40 parts of cellulase, 20-30 parts of pectinase, 20-30 parts of hemicellulase, 5-10 parts of subtilisin and 3-5 parts of amylase; the enzymolysis time is 80-100 min. The trollius chinensis bunge cell wall has high cellulose, pectin and hemicellulose content and low starch and protein content, and a single enzyme preparation only acts on certain specific components in the cell wall, so that a plurality of enzyme preparations are compounded, and the compound enzyme is finally determined to consist of the following enzymes in parts by weight after screening: 30-40 parts of cellulase, 20-30 parts of pectinase, 20-30 parts of hemicellulase, 5-10 parts of subtilisin and 3-5 parts of amylase. By utilizing the synergistic effect of the various enzyme preparations, the effects of quickly decomposing and destroying macromolecular substances such as fibers, pectin and the like are achieved, and the cell wall is completely broken as much as possible, so that the effective components in the cell are quickly and fully dissolved out, the solution can be clarified, the production period is favorably shortened, and the stability of the oral liquid is favorably improved; the cell wall is completely destroyed in a certain time, the continuous enzymolysis loses significance, the resource waste is caused, the cost is increased, and the control of a certain time is a key factor of the enzymolysis reaction.

Preferably, in the step (1), high-purity nitrogen gas or inert gas is introduced into the liquid material during the enzymolysis, and the liquid material is stirred by bubbling. When the enzymolysis is carried out, high-purity nitrogen or inert gas is introduced into the feed liquid for bubbling and stirring, so that firstly, heat can be dissipated, and the phenomenon that the temperature is increased due to heat accumulation in the feed liquid to influence the enzymolysis process is avoided; secondly, the feed liquid is fully stirred, so that the insufficient enzymolysis is avoided, and the wall pasting phenomenon caused by the adhesion of the trollius chinensis in the feed liquid on the wall of the container is avoided.

Preferably, in the step (2), the rotation speed of the high-speed centrifugation is 10000-20000 r/min.

Preferably, in the step (3), the chitosan acetic acid solution has a mass concentration of 1%, the chitosan acetic acid solution is added in an amount of 300-350 mg/L by volume of the supernatant, the talc powder is added in an amount of 3-5% by volume of the supernatant, the chitosan acetic acid solution is obtained by dissolving chitosan in the acetic acid solution, the chitosan is too little to completely destabilize and flocculate the particles, the chitosan is too much to surround the generated colloidal particles with chitosan, and the flocculation is affected, so that the chitosan acetic acid solution is strictly limited to have a mass concentration of 1% by volume of the supernatant, and the chitosan acetic acid solution is added in an amount of 300-350 mg/L by volume of the supernatant, and the talc powder is too much to cause turbidity and viscosity of the liquid medicine, so that the filtration is not facilitated, the talc powder is too little to cause a poor precipitation effect, and the talc powder is comprehensively considered, and the addition amount of the talc powder is controlled to be 3-5% in the invention.

Preferably, in the step (3), after the chitosan acetic acid solution is dripped, the stirring speed is 40-80 r/min, and the stirring time is 2-4 min. In the invention, after the chitosan acetic acid solution is dripped, the stirring speed is not too high, the stirring time is not too long, and if the stirring speed is too high and the stirring time is too long, relatively large suspended particles formed can be broken into small particles due to larger shearing force, so that the particles are difficult to settle, and the flocculation effect is reduced; if the stirring speed is too slow and the stirring time is too short, the chitosan and the colloidal particles can not be fully contacted, the chitosan trapping colloidal particles are influenced, and the chitosan is unevenly distributed, can not fully play a role and can also influence the flocculation effect. Therefore, the stirring speed is limited to be 40-80 r/min, and the stirring time is 2-4 min.

Preferably, in the step (4), the pore diameter of the hollow fiber filter membrane or the micro-filtration membrane is 0.3 to 0.5 μm.

Preferably, in the step (6), the auxiliary material includes at least one of a preservative, a surfactant, a flavoring agent and an antioxidant. The antiseptic can be methyl p-hydroxybenzoate, sodium benzoate, ethylparaben, etc., the surfactant can be polysorbate 80, polyoxyethylene (35) castor oil, poloxamer, etc., the correctant can be Mel, sucrose, simple syrup, sodium cyclamate, stevioside, xylitol, maltitol, aspartame, glycyrrhizin, etc., the antioxidant can be gallic acid, vitamin C, sodium bisulfite, sodium metabisulfite, etc., and the above adjuvants can be selected according to the actual needs of the product.

Therefore, the invention has the following beneficial effects: the preparation process of the tropaeolum oral liquid is optimized, the preparation and production of the tropaeolum oral liquid are carried out by adopting the enzymolysis-high-speed centrifugation-flocculation filtration-microfiltration method, the steps of the process are simple, the operation is easy, compared with the traditional water decoction process, the water consumption and the energy consumption are greatly reduced, the production period is greatly shortened, the clarity and the stability of the product can be effectively improved while the effective components such as total flavonoids in the medicinal materials are effectively reserved, and the preparation method is worthy of popularization and application.

Detailed Description

The following detailed description further describes the invention.