CN114983955B - Slowly-melted tiger plum lozenge and preparation method thereof - Google Patents

Slowly-melted tiger plum lozenge and preparation method thereof Download PDF

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CN114983955B
CN114983955B CN202210525792.9A CN202210525792A CN114983955B CN 114983955 B CN114983955 B CN 114983955B CN 202210525792 A CN202210525792 A CN 202210525792A CN 114983955 B CN114983955 B CN 114983955B
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enzymolysis
plum
premix
tiger
starch
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CN114983955A (en
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王大冲
张恒
黄凤君
罗召丰
金洁
周银锋
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Huiyinbi Group Zhejiang Qiqi Pharmaceutical Co ltd
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Abstract

The invention discloses a slow-melting tiger plum lozenge and a preparation method thereof. The tiger-plum buccal tablet provided by the invention is slow to melt in the oral cavity, long in administration time and good in treatment effect on pharyngitis.

Description

Slowly-melted tiger plum lozenge and preparation method thereof
Technical Field
The invention relates to a tiger plum lozenge, in particular to a slow-melting tiger plum lozenge and a preparation method thereof. Belongs to the technical field of preparation of pharmaceutical preparations.
Background
Pharyngitis is nonspecific inflammation of pharynx, is a common name for inflammation caused by infection of pharynx with various microorganisms, and can be classified into acute pharyngitis and chronic pharyngitis.
Acute pharyngitis is an acute inflammation of pharyngeal mucosa and submucosal tissue, pharyngeal lymphoid tissue is often involved, the early stage of inflammation can be limited, the whole pharyngeal cavity can be often involved along with the progress of the disease, and the treatment is more common in autumn, winter and spring. The main manifestations are dry throat, burning, pain, obvious swallowing pain, congestion and swelling of the throat, etc.
The chronic pharyngitis can be divided into chronic simple pharyngitis, chronic hypertrophic pharyngitis and atrophic pharyngitis, wherein the chronic simple pharyngitis is mainly characterized by chronic congestion of pharyngeal mucosa, hyperplasia of mucosa and submucosal connective tissue, hypertrophy of mucous glands, hypersecretion and increased mucous secretion. Patients often get sticky phlegm in the pharynx or feel foreign body sensation in the pharynx, do not get out, and the pharynx is not depressed. The chronic pharyngitis has the characteristics of complex etiology, intractable symptoms, easy recurrence, difficult cure and the like, and the main etiology comprises: improper treatment of acute pharyngitis; inflammatory stimuli of adjacent organs such as rhinitis, sinusitis, tonsillitis, and the like; often inhalation of noxious, irritating gases; if the spicy and pungent food is frequently eaten in the diet; allergic factors, and the like. The chronic pharyngitis is mostly seen in adults, the disease course is long, the disease is easy to recur, the symptoms are stubborn, and the disease is difficult to cure.
The acute pharyngitis and the chronic pharyngitis can cause great pain to patients, the life quality is seriously affected, particularly the acute pharyngitis and the acute attack stage of the chronic pharyngitis have strong uncomfortable feeling, the medicine is very necessary, but the western medicine has no special effect at present. Some traditional Chinese medicinal materials have obvious curative effects on pharyngitis, but are inconvenient to decoct and take, and the popularization and the use of the traditional Chinese medicinal materials are limited, so that the traditional Chinese medicinal materials are processed into preparations convenient to take, and the traditional Chinese medicinal materials have good clinical application prospects.
The tiger plum preparation is a very common Chinese patent medicine for pharyngitis, and patent application CN109876045A discloses a tiger plum preparation which takes giant knotweed rhizome, dark plum fruit and menthol as main components, sucrose, mannitol, steviosin and starch as auxiliary materials, adopts a controllable spray granulation technology, adopts a sprayer to disperse liquid materials into tiny liquid drops, and adopts generated hot air flow to blow up the powder materials below to evaporate the liquid materials, and bonds the blown powder materials to prepare proper granules. The product obtained by the patent technology can be prepared into preparation forms such as buccal tablets and the like.
Patent application CN1091651A discloses a tiger plum preparation and a preparation process thereof, wherein the tiger plum preparation is prepared from traditional Chinese medicinal materials of giant knotweed rhizome and dark plum by adding a proper amount of white sugar, the giant knotweed rhizome and dark plum are decocted with water according to the proportion of 1:0.2-0.8, concentrated, added with ethanol until the ethanol content reaches 60-80%, the filtrate is concentrated into a fluid extract after recovering the ethanol, and added with a proper amount of white sugar powder to be mixed into granules or blocky tiger plum granules, tiger plum lozenges and tiger plum oral liquid. The tiger plum lozenge can be directly taken, is convenient to take and has good efficacy.
The buccal tablet is a common preparation form which is convenient to carry and take, so the tiger plum buccal tablet is an ideal tiger plum preparation product. In the two patent technologies, starch is used as a disintegrating agent when the tiger plum lozenge is prepared. The melting process of the buccal tablet in the oral cavity is not only influenced by the temperature of the oral cavity, but also is corroded by saliva and abraded by tongue fur, so that the melting time is not long. The tiger plum lozenge in the current market is frequent in taking times and complicated in taking process, and the tiger plum lozenge is inconvenient to take and take again very frequently, and cannot meet the existing fast-paced life completely, so that the tiger plum lozenge is beneficial to alleviating the discomfort of the pharynx and achieving a better treatment effect on the pharyngitis by slowing down the melting process and prolonging the taking time.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a slow-melting tiger plum lozenge and a preparation method thereof, which have the advantages of slow melting in an oral cavity, long administration time and good treatment effect on pharyngitis.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the slow-melting tiger plum lozenge comprises the following specific steps in parts by weight:
(1) Drying and crushing giant knotweed and dark plum, mixing to obtain mixed powder with the particle size of 30-50 meshes, then dispersing the mixed powder in water by ultrasonic, carrying out enzymolysis, concentrating, and extracting by supercritical carbon dioxide to obtain an extract;
(2) Mixing rhamnolipid, polyethylene glycol and peppermint oil to obtain a premix, then dispersing the extract in water by ultrasonic to prepare a dispersion, slowly dripping the dispersion into the premix at a constant speed while stirring, continuing stirring for 30-40 minutes after dripping, spray drying to obtain a premix, preparing the premix into a soft material, and granulating to obtain particles;
(3) Then carrying out double-screw extrusion treatment and superfine grinding on corn starch to obtain pretreated starch, then dispersing the pretreated starch in water by ultrasonic, heating and gelatinizing to prepare starch milk, continuously adding cyclodextrin glucosyltransferase and seleno carrageenan into the starch milk, carrying out enzymolysis treatment, carrying out high-speed jet treatment, and drying to obtain modified starch;
(4) And finally, uniformly mixing 1-2 parts of particles with 10-12 parts of modified starch, 10-12 parts of sodium carboxymethyl cellulose, 80-90 parts of sucrose and 8-10 parts of essence, and tabletting to obtain the tiger plum lozenge.
Preferably, in the step (1), the mass ratio of the giant knotweed, the dark plum and the water is 100:30-40:300-350.
Preferably, in the step (1), enzymes used in enzymolysis are cellulase and pectase, and the dosages of the cellulase and pectase are respectively 0.1-0.2% and 0.08-0.12% of the mass of the giant knotweed; the enzymolysis conditions are as follows: pH=5-6, enzymolysis temperature 45-55 deg.c and enzymolysis time 2-3 hr.
Preferably, in the step (1), the mixture is concentrated to 35 to 45 percent of the original volume after enzymolysis.
Preferably, in the step (1), the process conditions of supercritical carbon dioxide extraction are as follows: the temperature is 45-50 ℃, the pressure is 35-45 MPa, and the extraction time is 5-7 hours.
Preferably, in the step (2), the mass ratio of the extract to the water to the premix is 20-30:80-90:90-100, and the mass ratio of the rhamnolipid to the polyethylene glycol to the peppermint oil in the premix is 1:2-3:0.8-1.
Preferably, in step (2), the dispersion is added dropwise for 30 to 40 minutes.
Preferably, in the step (3), the mass ratio of the corn starch, the water, the cyclodextrin glucosyltransferase and the selenized carrageenan is 10-15:40-50:0.1-0.2:4-5.
Preferably, in the step (3), the process conditions of the twin-screw extrusion treatment are as follows: the rotating speed is 60-80 r/min, and the temperature is 70-80 ℃; the process conditions of the superfine grinding are as follows: the pressure is 10-12 MPa, the feeding speed is 150-200 r/min, and the powder is crushed to the particle size below 10 mu m.
Preferably, in step (3), the process conditions for the thermal gelatinization are: treating at 85-95 deg.c for 20-30 min.
Preferably, in the step (3), the enzymolysis treatment process conditions are as follows: pH=5-6, enzymolysis temperature 50-60 deg.c and enzymolysis time 3-4 hr.
Preferably, in the step (3), the process conditions of the high-speed jet treatment are as follows: 300-400 MPa for 2-3 times.
Preferably, in the step (4), the tablet weight of the lozenge is 0.6g.
A slow thawing tiger plum buccal tablet is prepared by the above preparation method.
The invention has the beneficial effects that:
the invention firstly prepares the giant knotweed and the dark plum into particles, then uniformly mixes the particles with modified starch, sodium carboxymethyl cellulose, sucrose and essence, and tabletting to prepare the giant knotweed lozenge. The tiger-plum buccal tablet provided by the invention is slow to melt in the oral cavity, long in administration time and good in treatment effect on pharyngitis.
1. In the preparation of the granules, the giant knotweed and the dark plum are firstly dried and crushed, mixed to obtain mixed powder, then the mixed powder is ultrasonically dispersed in water, and the mixture is subjected to enzymolysis, concentration and supercritical carbon dioxide extraction to obtain the extract. The giant knotweed and dark plum are crushed and then subjected to enzymolysis treatment, so that the active ingredients in the giant knotweed and dark plum are fully released, and the content of the active ingredients in the buccal tablet is improved by combining supercritical carbon dioxide extraction, so that the curative effect is improved.
The preparation method comprises the steps of mixing rhamnolipid, polyethylene glycol and peppermint oil to obtain a premix, then dispersing the extract in water by ultrasonic to obtain a dispersion, slowly dripping the dispersion into the premix at a constant speed while stirring, continuously stirring for 30-40 minutes after dripping, spray drying to obtain a premix, preparing the premix into a soft material, and granulating to obtain particles. In other words, the invention utilizes the premix to carry out inclusion on the active ingredients obtained after the extraction of the giant knotweed and the dark plum, and plays a role of similar slow release, thereby slowing down the melting speed of the lozenge and prolonging the administration time, and further obtaining better curative effect.
2. The modified starch is prepared by the following steps: performing double-screw extrusion treatment and superfine grinding on corn starch to obtain pretreated starch, then performing ultrasonic dispersion on the pretreated starch in water, heating and gelatinizing to obtain starch milk, continuously adding cyclodextrin glucosyltransferase and seleno carrageenan into the starch milk, performing enzymolysis treatment, performing high-speed jet treatment, and drying to obtain the corn starch. Corn starch is subjected to double-screw extrusion treatment and superfine grinding, so that the starch structure is fully unfolded, the subsequent gelatinization is promoted, starch particles are highly expanded, cyclodextrin and amylopectin are generated along with enzymolysis of cyclodextrin glucosyltransferase, and the selenized carrageenan and starch are crosslinked to form a three-dimensional network structure, so that the water solubility is reduced, the melting speed of a lozenge is delayed, and the taking time is prolonged.
3. The peppermint oil in the premix and the selenium in the selenized carrageenan have synergistic effect on the giant knotweed and the dark plum, and can further improve the curative effect.
Detailed Description
The present invention will be further illustrated by the following examples, which are given by way of illustration only and are not intended to be limiting.
Example 1:
a preparation method of a slow thawing tiger plum lozenge comprises the following specific steps:
(1) Firstly, 100g of giant knotweed and 30g of dark plum are dried and crushed, mixed powder with the particle size of 30 meshes is obtained, then the mixed powder is dispersed in 300g of water by ultrasonic, cellulase and pectase are added for enzymolysis, the enzymolysis is carried out, the concentration is carried out until the volume of enzymolysis liquid obtained by the enzymolysis is 35%, and supercritical carbon dioxide extraction is carried out, thus obtaining an extract;
(2) Mixing rhamnolipid, polyethylene glycol and peppermint oil according to the mass ratio of 1:2:0.8 to obtain a premix, then taking 20g of extract, ultrasonically dispersing the extract in 80g of water to prepare a dispersion, slowly dripping the dispersion into 90g of the premix at a constant speed while stirring for 30 minutes, continuing stirring for 30 minutes after the dripping is finished, spray-drying to obtain a premix, preparing the premix into a soft material, and granulating to obtain particles;
(3) Then carrying out double screw extrusion treatment and superfine grinding on 10g of corn starch to obtain pretreated starch, then dispersing the pretreated starch in 40g of water by ultrasonic, heating and gelatinizing for 20 minutes at 85 ℃ to prepare starch milk, continuously adding 0.1g of cyclodextrin glucosyltransferase and 4g of selenized carrageenan into the starch milk, carrying out enzymolysis treatment, carrying out high-speed jet treatment, and drying to obtain modified starch;
(4) Finally, 1g of particles, 10g of modified starch, 10g of sodium carboxymethyl cellulose, 80g of sucrose and 8g of essence are uniformly mixed, and tabletting is carried out to obtain the tiger plum buccal tablet, wherein the tablet weight is 0.6g.
In the step (1), the dosage of cellulase and pectase is respectively 0.1% and 0.08% of the mass of the giant knotweed; the enzymolysis conditions are as follows: ph=5, enzymatic hydrolysis temperature 45 ℃, enzymatic hydrolysis time 2 hours.
In the step (1), the supercritical carbon dioxide extraction process conditions are as follows: the temperature is 45 ℃, the pressure is 35MPa, and the extraction time is 5 hours.
In the step (3), the process conditions of the twin-screw extrusion treatment are as follows: the rotating speed is 60r/min, and the temperature is 70 ℃; the process conditions of the superfine grinding are as follows: the pressure is 10MPa, the feeding speed is 150r/min, and the powder is crushed to the particle size of less than 10 mu m.
In the step (3), the enzymolysis treatment process conditions are as follows: ph=5, enzymatic hydrolysis temperature 50 ℃, enzymatic hydrolysis time 3 hours.
In the step (3), the process conditions of the high-speed jet treatment are as follows: 300MPa for 2 times.
Example 2:
a preparation method of a slow thawing tiger plum lozenge comprises the following specific steps:
(1) Firstly, 100g of giant knotweed and 40g of dark plum are dried and crushed, mixed powder with the particle size of 50 meshes is obtained, then the mixed powder is ultrasonically dispersed in 350g of water, cellulase and pectase are added for enzymolysis, the enzymolysis is carried out, the concentration is carried out until the volume of enzymolysis liquid obtained by the enzymolysis is 45%, and supercritical carbon dioxide extraction is carried out, thus obtaining an extract;
(2) Mixing rhamnolipid, polyethylene glycol and peppermint oil according to the mass ratio of 1:3:1 to obtain a premix, then taking 30g of extract, ultrasonically dispersing in 90g of water to prepare a dispersion, slowly dripping the dispersion into 100g of the premix at a constant speed while stirring for 40 minutes, continuing stirring for 40 minutes after dripping, spray-drying to obtain a premix, preparing the premix into a soft material, and granulating to obtain particles;
(3) Then carrying out double-screw extrusion treatment and superfine grinding on 15g of corn starch to obtain pretreated starch, then dispersing the pretreated starch in 50g of water by ultrasonic, heating and gelatinizing for 30 minutes at 95 ℃ to prepare starch milk, continuously adding 0.2g of cyclodextrin glucosyltransferase and 5g of selenized carrageenan into the starch milk, carrying out enzymolysis treatment, carrying out high-speed jet treatment, and drying to obtain modified starch;
(4) And finally, uniformly mixing 2g of particles with 12g of modified starch, 12g of sodium carboxymethyl cellulose, 90g of sucrose and 10g of essence, and tabletting to obtain the tiger plum buccal tablet, wherein the tablet weight is 0.6g.
In the step (1), the dosage of cellulase and pectase is 0.2% and 0.12% of the mass of the giant knotweed respectively; the enzymolysis conditions are as follows: ph=6, enzymatic hydrolysis temperature 55 ℃, enzymatic hydrolysis time 3 hours.
In the step (1), the supercritical carbon dioxide extraction process conditions are as follows: the temperature is 50 ℃, the pressure is 45MPa, and the extraction time is 7 hours.
In the step (3), the process conditions of the twin-screw extrusion treatment are as follows: the rotating speed is 80r/min, and the temperature is 80 ℃; the process conditions of the superfine grinding are as follows: the pressure is 12MPa, the feeding speed is 200r/min, and the powder is crushed to the particle size of less than 10 mu m.
In the step (3), the enzymolysis treatment process conditions are as follows: ph=6, enzymatic hydrolysis temperature 60 ℃, enzymatic hydrolysis time 4 hours.
In the step (3), the process conditions of the high-speed jet treatment are as follows: 400MPa for 3 times.
Example 3:
a preparation method of a slow thawing tiger plum lozenge comprises the following specific steps:
(1) Firstly, 100g of giant knotweed and 35g of dark plum are dried and crushed, mixed powder with the particle size of 40 meshes is obtained, then the mixed powder is dispersed in 330g of water by ultrasonic, cellulase and pectase are added for enzymolysis, the enzymolysis is carried out, the concentration is carried out until the volume of enzymolysis liquid obtained by the enzymolysis is 40%, and supercritical carbon dioxide extraction is carried out, thus obtaining an extract;
(2) Mixing rhamnolipid, polyethylene glycol and peppermint oil according to the mass ratio of 1:2.5:0.9 to obtain a premix, then taking 25g of extract, ultrasonically dispersing the extract in 85g of water to prepare a dispersion, slowly dripping the dispersion into 95g of the premix at a constant speed while stirring for 35 minutes, continuing stirring for 35 minutes after the dripping is finished, spray-drying to obtain a premix, preparing the premix into a soft material, and granulating to obtain granules;
(3) Then carrying out double-screw extrusion treatment and superfine grinding on 12g of corn starch to obtain pretreated starch, then dispersing the pretreated starch in 45g of water by ultrasonic, heating and gelatinizing for 25 minutes at 90 ℃ to prepare starch milk, continuously adding 0.15g of cyclodextrin glucosyltransferase and 4.5g of selenized carrageenan into the starch milk, carrying out enzymolysis treatment, carrying out high-speed jet treatment, and drying to obtain modified starch;
(4) Finally, 1.5g of particles, 11g of modified starch, 11g of sodium carboxymethyl cellulose, 85g of sucrose and 9g of essence are uniformly mixed, and tabletting is carried out to obtain the tiger plum buccal tablet, wherein the tablet weight is 0.6g.
In the step (1), the dosage of cellulase and pectase is 0.15% and 0.1% of the mass of the giant knotweed respectively; the enzymolysis conditions are as follows: ph=5, enzymatic hydrolysis temperature 50 ℃, enzymatic hydrolysis time 2.5 hours.
In the step (1), the supercritical carbon dioxide extraction process conditions are as follows: the temperature is 48 ℃, the pressure is 40MPa, and the extraction time is 6 hours.
In the step (3), the process conditions of the twin-screw extrusion treatment are as follows: the rotating speed is 70r/min, and the temperature is 75 ℃; the process conditions of the superfine grinding are as follows: the pressure is 12MPa, the feeding speed is 180r/min, and the powder is crushed to the particle size of less than 10 mu m.
In the step (3), the enzymolysis treatment process conditions are as follows: ph=6, enzymatic hydrolysis temperature 55 ℃, enzymatic hydrolysis time 3.5 hours.
In the step (3), the process conditions of the high-speed jet treatment are as follows: 400MPa for 3 times.
Comparative example 1
A preparation method of tiger plum lozenge comprises the following specific steps:
(1) Firstly, 100g of giant knotweed and 30g of dark plum are dried and crushed, mixed powder with the particle size of 30 meshes is obtained, then the mixed powder is dispersed in 300g of water by ultrasonic, cellulase and pectase are added for enzymolysis, the enzymolysis is carried out, the concentration is carried out until the volume of enzymolysis liquid obtained by the enzymolysis is 35%, supercritical carbon dioxide extraction is carried out, an extract is obtained, the extract is made into soft materials, and particles are obtained by granulating;
(2) Then carrying out double screw extrusion treatment and superfine grinding on 10g of corn starch to obtain pretreated starch, then dispersing the pretreated starch in 40g of water by ultrasonic, heating and gelatinizing for 20 minutes at 85 ℃ to prepare starch milk, continuously adding 0.1g of cyclodextrin glucosyltransferase and 4g of selenized carrageenan into the starch milk, carrying out enzymolysis treatment, carrying out high-speed jet treatment, and drying to obtain modified starch;
(3) Finally, 1g of particles, 10g of modified starch, 10g of sodium carboxymethyl cellulose, 80g of sucrose and 8g of essence are uniformly mixed, and tabletting is carried out to obtain the tiger plum buccal tablet, wherein the tablet weight is 0.6g.
In the step (1), the dosage of cellulase and pectase is respectively 0.1% and 0.08% of the mass of the giant knotweed; the enzymolysis conditions are as follows: ph=5, enzymatic hydrolysis temperature 45 ℃, enzymatic hydrolysis time 2 hours.
In the step (1), the supercritical carbon dioxide extraction process conditions are as follows: the temperature is 45 ℃, the pressure is 35MPa, and the extraction time is 5 hours.
In the step (2), the process conditions of the twin-screw extrusion treatment are as follows: the rotating speed is 60r/min, and the temperature is 70 ℃; the process conditions of the superfine grinding are as follows: the pressure is 10MPa, the feeding speed is 150r/min, and the powder is crushed to the particle size of less than 10 mu m.
In the step (2), the enzymolysis treatment process conditions are as follows: ph=5, enzymatic hydrolysis temperature 50 ℃, enzymatic hydrolysis time 3 hours.
In the step (2), the process conditions of the high-speed jet treatment are as follows: 300MPa for 2 times.
Comparative example 2
A preparation method of tiger plum lozenge comprises the following specific steps:
(1) Firstly, 100g of giant knotweed and 30g of dark plum are dried and crushed, mixed powder with the particle size of 30 meshes is obtained, then the mixed powder is dispersed in 300g of water by ultrasonic, cellulase and pectase are added for enzymolysis, the enzymolysis is carried out, the concentration is carried out until the volume of enzymolysis liquid obtained by the enzymolysis is 35%, and supercritical carbon dioxide extraction is carried out, thus obtaining an extract;
(2) Mixing rhamnolipid, polyethylene glycol and peppermint oil according to the mass ratio of 1:2:0.8 to obtain a premix, then taking 20g of extract, ultrasonically dispersing the extract in 80g of water to prepare a dispersion, slowly dripping the dispersion into 90g of the premix at a constant speed while stirring for 30 minutes, continuing stirring for 30 minutes after the dripping is finished, spray-drying to obtain a premix, preparing the premix into a soft material, and granulating to obtain particles;
(3) Then carrying out double screw extrusion treatment and superfine grinding on 10g of corn starch to obtain pretreated starch, then dispersing the pretreated starch in 40g of water by ultrasonic, heating and gelatinizing for 20 minutes at 85 ℃ to prepare starch milk, carrying out high-speed jet treatment, and drying to obtain modified starch;
(4) Finally, 1g of particles, 10g of modified starch, 10g of sodium carboxymethyl cellulose, 80g of sucrose and 8g of essence are uniformly mixed, and tabletting is carried out to obtain the tiger plum buccal tablet, wherein the tablet weight is 0.6g.
In the step (1), the dosage of cellulase and pectase is respectively 0.1% and 0.08% of the mass of the giant knotweed; the enzymolysis conditions are as follows: ph=5, enzymatic hydrolysis temperature 45 ℃, enzymatic hydrolysis time 2 hours.
In the step (1), the supercritical carbon dioxide extraction process conditions are as follows: the temperature is 45 ℃, the pressure is 35MPa, and the extraction time is 5 hours.
In the step (3), the process conditions of the twin-screw extrusion treatment are as follows: the rotating speed is 60r/min, and the temperature is 70 ℃; the process conditions of the superfine grinding are as follows: the pressure is 10MPa, the feeding speed is 150r/min, and the powder is crushed to the particle size of less than 10 mu m.
In the step (3), the process conditions of the high-speed jet treatment are as follows: 300MPa for 2 times.
Test examples
Clinical studies are carried out on the tiger plum lozenges obtained in the examples 1 to 3 and the comparative examples 1 and 2 respectively, and the specific method is as follows:
a total of 120 patients with acute pharyngitis aged 18-50 years are selected, the average of the patients is divided into 6 groups at random, 20 patients in each group, the first 5 groups are respectively taken with the tiger plum lozenges obtained in the examples 1-3 and the comparative examples 1 and 2, and the last 1 group is taken with the throat lozenge as a control group. The tiger plum lozenge is taken one piece at a time, 2 times a day, and the gold throat lozenge is taken one piece at a time, 2 times a day for one week. The time of complete buccal tablet containing tiger plum in oral cavity was recorded, and the average value of each group was taken.
And (3) judging curative effect:
and (3) curing: the pharyngeal symptoms disappear and the examination is normal;
improvement: the pharyngeal symptoms are obviously relieved;
invalidation: the symptoms have no obvious change.
The results of the investigation are shown in tables 1 and 2.
TABLE 1 time to complete incubation
Complete time of incubation (min)
Example 1 20.2
Example 2 20.5
Example 3 21.2
Comparative example 1 16.4
Comparative example 2 15.6
TABLE 2 curative effect on acute pharyngitis
Cure (example) Improvement (example) Invalidation (example) Cure rate (%)
Control group 5 8 7 25
Example 1 19 1 0 95
Example 2 19 1 0 95
Example 3 20 0 0 100
Comparative example 1 15 5 0 75
Comparative example 2 14 6 0 70
As is clear from tables 1 and 2, the buccal tablets obtained in examples 1 to 3 have long complete dissolution time, which indicates that the buccal tablets of the invention have slow melting and longer administration time, one tablet at a time and 2 times a day, and have high cure rate and good curative effect on acute pharyngitis.
Comparative example 1 omits the premix when preparing granules, comparative example 2 omits the enzymolysis treatment steps of cyclodextrin glucosyltransferase and seleno carrageenan when preparing modified starch, the melting speed of the obtained tiger plum lozenge is obviously increased, the curative effect is poor, and the inclusion of the premix, the subsequent enzymolysis treatment, the addition of seleno carrageenan and the like are used for synergistically slowing down the melting speed, and the curative effect is improved.
While the foregoing describes the embodiments of the present invention, it is not intended to limit the scope of the present invention, and various modifications or variations may be made by those skilled in the art without the need for inventive effort on the basis of the technical solutions of the present invention.

Claims (10)

1. The preparation method of the slow-melting tiger plum lozenge is characterized by comprising the following specific steps of, by weight:
(1) Drying and crushing giant knotweed and dark plum, mixing to obtain mixed powder with the particle size of 30-50 meshes, then dispersing the mixed powder in water by ultrasonic, carrying out enzymolysis, concentrating, and extracting by supercritical carbon dioxide to obtain an extract;
(2) Mixing rhamnolipid, polyethylene glycol and peppermint oil to obtain a premix, then dispersing the extract in water by ultrasonic to prepare a dispersion, slowly dripping the dispersion into the premix at a constant speed while stirring, continuing stirring for 30-40 minutes after dripping, spray drying to obtain a premix, preparing the premix into a soft material, and granulating to obtain particles;
(3) Then carrying out double-screw extrusion treatment and superfine grinding on corn starch to obtain pretreated starch, then dispersing the pretreated starch in water by ultrasonic, heating and gelatinizing to prepare starch milk, continuously adding cyclodextrin glucosyltransferase and seleno carrageenan into the starch milk, carrying out enzymolysis treatment, carrying out high-speed jet treatment, and drying to obtain modified starch;
(4) And finally, uniformly mixing 1-2 parts of particles with 10-12 parts of modified starch, 10-12 parts of sodium carboxymethyl cellulose, 80-90 parts of sucrose and 8-10 parts of essence, and tabletting to obtain the tiger plum lozenge.
2. The preparation method according to claim 1, wherein in the step (1), the mass ratio of the giant knotweed, the dark plum and the water is 100:30-40:300-350.
3. The preparation method of claim 1, wherein in the step (1), enzymes used in the enzymolysis are cellulase and pectase, and the dosages of the cellulase and pectase are respectively 0.1-0.2% and 0.08-0.12% of the mass of the giant knotweed; the enzymolysis conditions are as follows: pH=5-6, enzymolysis temperature 45-55 deg.c and enzymolysis time 2-3 hr.
4. The method according to claim 1, wherein in the step (1), the supercritical carbon dioxide extraction is performed under the following process conditions: the temperature is 45-50 ℃, the pressure is 35-45 MPa, and the extraction time is 5-7 hours.
5. The preparation method according to claim 1, wherein in the step (2), the mass ratio of the extract, water and the premix is 20-30:80-90:90-100, and the mass ratio of the rhamnolipid, polyethylene glycol and peppermint oil in the premix is 1:2-3:0.8-1.
6. The process according to claim 1, wherein in the step (2), the dispersion is added dropwise for 30 to 40 minutes.
7. The preparation method according to claim 1, wherein in the step (3), the mass ratio of the corn starch, the water, the cyclodextrin glucosyltransferase and the selenized carrageenan is 10-15:40-50:0.1-0.2:4-5.
8. The method according to claim 1, wherein in the step (3), the twin-screw extrusion treatment is performed under the following process conditions: the rotating speed is 60-80 r/min, and the temperature is 70-80 ℃; the process conditions of the superfine grinding are as follows: the pressure is 10-12 MPa, the feeding speed is 150-200 r/min, and the powder is crushed to the particle size below 10 mu m.
9. The method according to claim 1, wherein in the step (3), the process conditions for the thermal gelatinization are: treating at 85-95 deg.c for 20-30 min;
the enzymolysis treatment process conditions are as follows: pH=5-6, enzymolysis temperature 50-60 deg.c, enzymolysis time 3-4 hr;
the technological conditions of the high-speed jet treatment are as follows: 300-400 MPa for 2-3 times.
10. A slow thawing tiger plum lozenge obtainable by the process of any one of claims 1 to 9.
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CN106387654A (en) * 2016-09-09 2017-02-15 吉林农业大学 Preparation method of aging-resistant modified corn flour
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