CN110215494B - Traditional Chinese medicine granules for regulating sleep and preparation method thereof - Google Patents
Traditional Chinese medicine granules for regulating sleep and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a traditional Chinese medicine granule for adjusting sleep, which comprises the following raw materials: radix rehmanniae, acanthopanax, schisandra chinensis, rhizoma polygonati, caulis polygoni multiflori, mulberry and pearl. The formula of the traditional Chinese medicine granule for adjusting sleep is obtained by combining the dosage of the recommended raw materials in pharmacopoeia, the product development requirement and the related requirement of health food evaluation, and has the effect of improving sleep. The invention also discloses a preparation method of the traditional Chinese medicine granules for adjusting sleep, the preparation method of the traditional Chinese medicine granules for adjusting sleep can extract effective components in raw materials to a large extent, the process is simple, the conditions are mild, the production cost is low, and the prepared product has uniform and stable properties.
Description
Technical Field
The invention relates to a traditional Chinese medicine granule and a preparation method thereof, in particular to a traditional Chinese medicine granule for adjusting sleep and a preparation method thereof.
Background
The sleep is one of the most familiar activities in daily life, about one third of the life of a person spends in sleep, and when the person is in a sleep state, the brain and the body of the person can be rested, rested and recovered, thereby being beneficial to daily work and learning of the person.
Because the modern life rhythm is accelerated, the sleep quality of people is generally reduced, the reduction of the sleep quality can cause the reduction of the immunity of the body, the reduction of the resistance to various diseases, the instability of emotion, the promotion of memory, the dysfunction of the brain, the reduction of the capability of processing and analyzing problems and the reduction of the working efficiency, and therefore, the improvement of the sleep quality is the guarantee of the normal work and study of people.
In the products for regulating sleep in the market, most products cannot achieve the expected effect, and some products have side effects in different degrees. Therefore, the development of a Chinese medicinal preparation having a function of regulating sleep with little side effects is an effort of pharmaceutical workers.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a traditional Chinese medicine granule for regulating sleep and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a traditional Chinese medicine granule for adjusting sleep comprises the following raw materials: radix rehmanniae, acanthopanax, schisandra chinensis, rhizoma polygonati, caulis polygoni multiflori, mulberry and pearl.
Preferably, the traditional Chinese medicine granules for adjusting sleep comprise the following raw materials in parts by weight: comprises the following raw materials in parts by weight: 5-7 parts of radix rehmanniae recen, 5-7 parts of acanthopanax, 3-5 parts of schisandra chinensis, 4-6 parts of rhizoma polygonati, 4-6 parts of caulis polygoni multiflori, 3-5 parts of mulberry and 0.08-0.12 part of pearl.
According to the reports of related documents, the known components contained in the traditional Chinese medicinal materials in the prescription, the pharmacological action and the clinical application research are summarized in a table, and the table is specifically shown in a table 1.
TABLE 1 brief description of the chemical components and pharmacological actions of the materials
The formula of the invention is obtained by combining the dosage of the recommended raw materials of the pharmacopoeia, the development requirement of products and the relevant requirement of the evaluation of health food, and has the effect of improving sleep.
Preferably, the traditional Chinese medicine granules for adjusting sleep comprise the following raw materials in parts by weight: 6 parts of radix rehmanniae recen, 6 parts of acanthopanax, 4 parts of schisandra chinensis, 5 parts of rhizoma polygonati, 5 parts of caulis polygoni multiflori, 4 parts of mulberry and 0.1 part of pearl.
Preferably, the raw materials for preparing the traditional Chinese medicine granules for regulating sleep further comprise 8.5-10.5 parts by weight of maltodextrin and 0.1-0.15 part by weight of stevioside.
The invention also aims to provide a preparation method of the traditional Chinese medicine granules for adjusting sleep, which is characterized by comprising the following steps:
(1) weighing fructus schizandrae, crushing, adding 6-10 times of ethanol with volume concentration of 60-80%, reflux-extracting at 85-95 ℃ for 45-90 min for 1-3 times, filtering to obtain filtrate, and concentrating to relative density of 1.05-1.10 at 60 ℃ to obtain ethanol-extracted concentrated solution;
(2) weighing radix rehmanniae, rhizoma polygonati, mulberry, acanthopanax and caulis polygoni multiflori, adding 8-12 times of water, decocting for 45-90 min, extracting for 1-3 times, filtering to obtain filtrate, and concentrating until the relative density at 60 ℃ is 1.05-1.10 to obtain a water extraction concentrated solution;
(3) mixing the ethanol extract concentrate obtained in the step (1) and the water extract concentrate obtained in the step (2), adding a part of maltodextrin, drying and crushing to obtain dry extract powder; adding the rest maltodextrin, pearl powder and stevioside into the dry extract powder, drying and granulating to obtain the traditional Chinese medicine granules for regulating sleep.
As shown in Table 1, rehmannia root, acanthopanax root, siberian solomonseal rhizome, mulberry and vine of multiflower knotweed mainly contain glycosides, polysaccharides and other components with good water solubility, so that the extraction solvent is water. The schisandra chinensis is mainly lignans, wherein schizandrin A, schizandrin B and the like have strong activity of improving sleep, but mainly comprise alcohol-soluble components, so the schisandra chinensis adopts ethanol as an extraction solvent. The pearl powder has less formula dosage, higher price, more inorganic calcium salt components and poorer water solubility, so the process adopts a method of directly adding full powder. The method can be used for extracting the effective components in the traditional Chinese medicine raw materials with high efficiency.
Preferably, in the step (1), the extraction times are 2 times, 10 times of ethanol is added in each time, the volume concentration is 70%, and the time of each reflux extraction is 60 min. The inventor finds that the concentration, the addition amount, the extraction time and the extraction frequency of the extracting solution have great influence on the extraction of the effective components, and the extraction rate of the schizandrol A is up to 89% when the schisandra chinensis adopts the extraction conditions, and the production cost can be controlled.
Preferably, in step (2), the number of extraction times is 2, the amount of water added in the first extraction is 10 times, the amount of water added in the second extraction is 8 times, the first extraction time is 90min, and the second extraction time is 60 min. The inventor finds that the polysaccharide extraction efficiency is higher and the production cost can be controlled when the extraction conditions are adopted.
Preferably, in step (1) and step (2), the concentration is carried out at 80. + -. 5 ℃ under reduced pressure. The transfer rate of the effective components is high by vacuum concentration under the above conditions.
Preferably, in the step (3), the ethanol extract concentrated solution obtained in the step (1) and the water extract concentrated solution obtained in the step (2) are combined and then uniformly mixed, heated to 70-90 ℃, dissolved by adding 20-30% of maltodextrin in total weight which is 30-50% of dry solid content, spray-dried and crushed to obtain dry extract powder; and then uniformly mixing the pearl powder and stevioside, adding the rest maltodextrin by an equivalent increment method, adding the dry extract powder, uniformly mixing, adding 50% ethanol for granulation, and drying at 75-80 ℃. A certain amount of maltodextrin is added in the preparation of the dry extract powder, so that the wall sticking of the extract powder is greatly reduced. After the dry extract powder is prepared, the dry extract powder is crushed and sieved by a 80-mesh sieve, and the obtained dry extract powder is fine, uniform and consistent in color and luster.
Preferably, in the step (1), the size of the crushed traditional Chinese medicine particles is 24 meshes. The inventor finds that the size of the traditional Chinese medicine granules has great influence on the extraction rate, and the extraction of the effective components in the schisandra chinensis can be improved by adopting 24 meshes.
Preferably, the air inlet temperature of the spray drying is 185 +/-5 ℃, and the air outlet temperature is 100-105 ℃.
The invention has the beneficial effects that: the invention provides a traditional Chinese medicine granule for regulating sleep, and the traditional Chinese medicine granule for regulating sleep is obtained by combining the dosage of recommended raw materials in pharmacopeia, the product development requirement and the related requirement of health food evaluation, and has the effect of improving sleep. The invention also provides a preparation method of the traditional Chinese medicine granules for adjusting sleep, the preparation method of the traditional Chinese medicine granules for adjusting sleep can extract effective components in raw materials to a large extent, the process is simple, the conditions are mild, the production cost is low, and the prepared product has uniform and stable properties.
Drawings
FIG. 1 shows the identification of Acanthopanax senticosus;
FIG. 2 is a diagram of the identification of Polygonatum sibiricum Red;
FIG. 3 is a photograph of identification of rehmannia;
FIG. 4 is a drawing showing identification of caulis Polygoni Multiflori;
FIG. 5 System adaptive chromatogram; wherein, (A) is a chromatogram of a reference substance, and (B) is a chromatogram of a sample;
FIG. 6 is a graph of the results of a linear test; wherein, the graph of A is the graph of schizandrin A, the graph of B is the graph of schizandrin A, and the graph of C is the graph of Schizandrin B.
Detailed Description
The sources of the raw materials used in the examples are shown in Table 2.
TABLE 2 raw material sources and lot numbers
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
In an embodiment of the traditional Chinese medicine granule for regulating sleep of the present invention, the traditional Chinese medicine granule for regulating sleep of the present embodiment comprises the following raw materials in parts by weight: 6 parts of radix rehmanniae recen, 6 parts of acanthopanax, 4 parts of schisandra chinensis, 5 parts of rhizoma polygonati, 5 parts of caulis polygoni multiflori, 4 parts of mulberry, 0.1 part of pearl, 9.44 parts of maltodextrin and 0.128 part of stevioside.
The preparation method of the traditional Chinese medicine granules for regulating sleep comprises the following steps:
(1) weighing fructus schizandrae, crushing and sieving with a 24-mesh sieve, adding 10 times of ethanol with the volume concentration of 70%, performing reflux extraction for 60min for 2 times, filtering to obtain filtrate, combining the extracts under the same extraction conditions for each time, and concentrating to obtain an ethanol extraction concentrate with the relative density of 1.05-1.10 at 60 ℃;
(2) weighing radix rehmanniae, rhizoma polygonati, mulberry, acanthopanax and caulis polygoni multiflori, adding water for extraction for 2 times, adding 10 times of water for decoction for 90min for the first time, filtering to obtain filtrate, adding 8 times of water for decoction for 60min for the second time, filtering to obtain filtrate, combining the extracts, and concentrating until the relative density at 60 ℃ is 1.05-1.10 to obtain a water extraction concentrated solution;
(3) mixing the ethanol extract concentrated solution obtained in the step (1) and the water extract concentrated solution obtained in the step (2), uniformly mixing, heating to 80 ℃, adding 20% of the total weight of maltodextrin to dissolve, spray-drying, crushing at the air inlet temperature of 185 +/-5 ℃ and the air outlet temperature of 100-105 ℃, and sieving with a 80-mesh sieve to obtain dry extract powder; and then uniformly mixing the pearl powder and stevioside, adding the rest maltodextrin by an equivalent increment method, adding the dry extract powder, uniformly mixing, granulating by using 50% ethanol, and drying at 75 ℃ to obtain the traditional Chinese medicine granules for regulating sleep.
Example 2
In an embodiment of the traditional Chinese medicine granule for regulating sleep of the present invention, the traditional Chinese medicine granule for regulating sleep of the present embodiment comprises the following raw materials in parts by weight: 5 parts of radix rehmanniae recen, 5 parts of acanthopanax, 3 parts of schisandra chinensis, 4 parts of rhizoma polygonati, 4 parts of caulis polygoni multiflori, 3 parts of mulberry, 0.08 part of pearl, 8.5 parts of maltodextrin and 0.1 part of stevioside.
The preparation method of the traditional Chinese medicine granules for regulating sleep in the embodiment is the same as that in the embodiment 1.
Example 3
In an embodiment of the traditional Chinese medicine granule for regulating sleep of the present invention, the traditional Chinese medicine granule for regulating sleep of the present embodiment comprises the following raw materials in parts by weight: 7 parts of radix rehmanniae recen, 7 parts of acanthopanax, 5 parts of schisandra chinensis, 6 parts of rhizoma polygonati, 6 parts of caulis polygoni multiflori, 5 parts of mulberry, 0.12 part of pearl, 10.5 parts of maltodextrin and 0.15 part of stevioside.
The preparation method of the traditional Chinese medicine granules for regulating sleep in the embodiment is the same as that in the embodiment 1.
Example 4
To investigate the effect of extraction conditions on the extraction effect, the following experiments were performed:
extraction of first and second Chinese magnoliavine fruit
1. Single factor investigation
Pulverizing fructus Schisandrae decoction pieces into 20-mesh and 40-mesh coarse powders, respectively, extracting under reflux with 10 times of 50%, 60%, 70% and 80% solvent for 60min, and calculating the extraction rate of main active ingredients including schisandrin, deoxyschizandrin and schisandrin B, the results are shown in Table 3.
TABLE 3 Table for examining single factor of extraction of schisandra chinensis
From the results in table 3, it can be seen that after 24-mesh crushing of schisandra chinensis, extraction with 70% ethanol is performed, the extraction rates of the main components of schizandrol A, schizandrin A and schizandrin B are respectively 6.58 times, 6.65 times and 8.80 times higher than that of the original medicinal materials, however, the extraction rate of the 40-mesh powder is still 24-mesh powder, which may be related to the influence of too much fine powder on the extraction of medicinal components, and it can be seen that crushing of schisandra chinensis into 24-mesh is beneficial to the extraction of the components. From the extracts with different alcohol concentrations, the extraction efficiency of 50%, 60%, 70% and 80% ethanol has a certain tendency to increase, but the extraction rate of different components is close.
2. Orthogonal experimental investigation
Weighing 9 parts of decoction pieces of five medicinal materials, 5g each, according to an orthogonal test table L9(34) Arranging an experiment, extracting, filtering by a 300-mesh screen, and performing extraction process investigation by taking the extraction rate evaluation index of the schizandrol A and the solvent multiples of A (alcohol concentration), B (extraction time), C (extraction frequency) and D as investigation factors. The factor levels are shown in Table 4.
TABLE 4 extraction of levels of orthogonal test factors
TABLE 5 fructus Schisandrae chinensis alcohol extraction orthogonal test results
From the experimental results in table 5, it can be seen that the extraction frequency has the greatest influence on the schizandrol A content, and the other sequences are the ethanol concentration, the solvent multiple and the extraction time, and from the orthogonal experimental results, the process with the best extraction effect is A3B2C2D3 by taking the extraction rate of the schizandrol A as an evaluation index, that is, the extraction is performed for 2 times with 10 times of 80% ethanol, and each time is 60 min. However, the extraction rate of the schizandrol A by 70% ethanol is up to 89%, and is only about 3% lower than that of the extraction rate of 80% ethanol, and considering the factors of production cost, safety risk brought by high-concentration ethanol and the like, the process A2B2C2D3 is determined, namely 10 times of 70% ethanol is used for 2 times, and each time is 60 min.
Extracting radix rehmanniae, rhizoma Polygonati, Mori fructus, radix Acanthopanacis Senticosi and caulis Polygoni Multiflori with water
Preparing 9 parts of medicinal decoction pieces according to the formulated amount, weighing 6g of radix rehmanniae, 6g of radix Acanthopanacis Senticosi, 5g of rhizoma Polygonati, 5g of Mori fructus and 5g of caulis Polygoni Multiflori in each part, and performing orthogonal test according to the orthogonal test table L9(34) Arranging experiments, adding water for decoction, filtering by 300 meshes, taking the extraction rate of crude polysaccharide as an extraction rate evaluation index, and taking the water adding times, the decoction time and the decoction times as investigation factors to perform extraction process investigation. The factor levels are shown in Table 6.
TABLE 6 Water extraction orthogonal test factor levels
TABLE 7 Water extraction orthogonal test results
From the experimental results in table 7, it can be seen that the number of extractions has a large influence on the polysaccharide extraction rate, and the other sequences are extraction time and solvent times, and from the orthogonal experimental results, the process with the best extraction effect is A2B3C3, i.e., 10 times of water extraction for 3 times, each time for 90min, using the crude polysaccharide extraction rate as an evaluation index. Wherein, the extraction times have larger influence on the extraction rate of the crude polysaccharide, the extraction rate is increased by 50.22 percent compared with 1 time of extraction when 2 times of extraction are carried out, the extraction rate is only increased by 17.72 percent compared with 2 times of extraction when 3 times of extraction are carried out, and the extraction time is selected to be 2 times in consideration of the factors such as the extraction cost and the like. The extraction time is 60min and 90min, the extraction rate of polysaccharide is above 2.2%, and the extraction time can be determined as 90min for the first extraction and 60min for the second extraction. Therefore, by combining factors such as production practice, production cost and the like, the water extraction process of the medicine is to add 10 times of water and extract twice, and the time is 90min and 60min respectively.
Third, investigation of concentration process
Pulverizing fructus Schisandrae into coarse powder, adding 10 times of 70% ethanol for 2 times, each for 60min, mixing extractive solutions, recovering ethanol, and concentrating under reduced pressure at 80 deg.C to a certain concentration. Extracting decoction pieces of other medicinal materials by extraction process, concentrating under reduced pressure at 80 deg.C to a certain concentration, mixing with fructus Schisandrae concentrated solution, mixing well, concentrating to relative density of 1.10(60 deg.C), and inspecting fructus Schisandrae component content.
TABLE 8 sample concentration investigation
As can be seen from the results in Table 8, the transfer rates of schizandrol A, schizandrin A and schizandrin B after the concentration of the schisandra chinensis are more than 88%, and the transfer rates are high.
Fourthly, drying process
1. Selection of drying process
The conventional drying process for the traditional Chinese medicine extract mainly comprises a reduced pressure drying method, a spray drying method and the like, wherein the concentrated fluid extract is dried by the reduced pressure drying method and the spray drying method (adding 25% of maltodextrin) at 80 ℃ respectively, and the results are shown in table 9.
TABLE 9 examination results of drying methods
From the results of the two drying methods, it can be known that the reduced pressure drying method has long drying time, high requirements on relative density of fluid extract, darker sample property color, short time and lighter product property color, and the drying method is determined to be the spray drying method from the aspects of production efficiency and the like.
2. Investigation of spray drying Process
Taking the mixed concentrated solution concentrated to the relative density of 1.05(60 ℃), dividing the mixed concentrated solution into 4 parts with the dry solid content of 20.37 percent, dividing each part into 500mL, heating the parts to 80 ℃, performing spray drying according to the method in the table 10 to observe the wall sticking degree of the dry extract powder in the spray drying process, and measuring the moisture content of the dry extract powder by using a rapid moisture meter, wherein the results are shown in the table 10.
TABLE 10 spray drying review
As can be seen from the results in Table 10, when dextrin was added to the concentrated extract in an amount of 20% to 30% of the dry solids content during the spray drying process, the powder was less sticky and the process was suitable, especially when 20% was used, the sticky wall was the least.
3. Pulverizing, sieving and mixing
From the state of dry paste collected after spray drying, partial small blocky dry paste exists, the color is darker, and the problems of inconsistent color and luster of dry extract powder, non-uniform system and the like are easily caused due to the fact that powder is formed in the collecting process. In order to ensure the uniformity of the prepared dry paste, after the dry paste is collected, the dry paste is crushed, sieved by a 80-mesh sieve and uniformly mixed, and the obtained dry paste is fine and uniform and has consistent color.
Example 5
In order to verify the stability of the traditional Chinese medicine granules for regulating sleep in the process, 1 batch of scale-up production is carried out, and the data are summarized in a table 11.
TABLE 11 production records summary sheet
From the experimental results, the production process of the three batches of products is stable and feasible.
Example 6
In order to verify the quality of the traditional Chinese medicine granules for regulating sleep prepared by the preparation method of the invention, the following researches are carried out by taking the raw materials and the preparation method of the traditional Chinese medicine granules for regulating sleep described in example 1 as an example:
first, research on sensory requirements
Sensory requirements were determined based on the characteristics of the three batches of samples, as detailed in Table 12.
TABLE 12 sensory index recording sheet
According to the research result, the sensory requirements in the product standard are formulated.
Second, research of identification method
1. Identification of Acanthopanax senticosus
Taking 25g of the product particles, grinding into fine powder, taking 25g of the powder, adding 50mL of 75% ethanol, heating and refluxing for 1h, filtering, evaporating the filtrate to dryness, adding 10mL of water into the residue to dissolve, shaking and extracting for 2 times by using trichloromethane, 5mL each time, combining trichloromethane solutions, evaporating to dryness, and adding 1mL of methanol into the residue to dissolve to obtain a sample solution. Preparing another 5g of radix Acanthopanacis Senticosi reference material, and making into reference medicinal solution in the same way. According to thin layer chromatography (Pharmacopeia of the people's republic of China 2015 edition, the fourth general rule 0502), sucking 10 μ L of the two solutions, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol (19:1) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (365 mn). The results are shown in fig. 1, wherein the original image of fig. 1 is in color, 1 and 2 in fig. 1 are acanthopanax root reference medicinal materials, and 3 and 4 are traditional Chinese medicine granule samples for regulating sleep. As can be seen from FIG. 1, the test chromatogram shows fluorescence spots of the same color at the corresponding positions of the control chromatogram.
2. Identification of rhizoma Polygonati
(1) Sample processing
Taking 6g of the product particles, grinding into fine powder, taking 6g of the powder, adding 20mL of 70% ethanol, heating and refluxing for 1h, filtering, evaporating the filtrate to dryness, adding 10mL of water into the residue to dissolve, adding n-butanol, shaking and extracting for 2 times, 20mL each time, combining n-butanol solutions, evaporating to dryness, adding 1mL of methanol into the residue to dissolve to obtain a sample solution. Taking 1g of rhizoma Polygonati as reference material, and making into reference material solution by the same method. Performing thin layer chromatography (0502 of the fourth guideline of the pharmacopoeia of the people's republic of China 2015), sucking 10 μ L of each of the two solutions, respectively dropping the two solutions on the same silica gel G thin layer plate, developing by using petroleum ether (60-90 ℃) -ethyl acetate-formic acid (5:2:0.1) as a developing agent, taking out, drying in the air, spraying a 5% vanillin sulfuric acid solution, and heating at 105 ℃ until spots are clearly developed. The result is shown in fig. 2, wherein the original picture in fig. 2 is in color, 1 and 2 in fig. 2 are rhizoma polygonati reference medicinal materials, and 3 and 4 are traditional Chinese medicine granule samples for regulating sleep. As can be seen from FIG. 2, the test chromatogram shows spots of the same color at the positions corresponding to those of the control chromatogram.
3. Identification of rehmannia
(1) Sample processing
Taking 10g of the product particles, grinding into fine powder, taking 10g of the powder, adding 20mL of methanol, heating and refluxing for 1h, cooling, filtering, and concentrating the filtrate to 5mL to be used as a test solution. Preparing 2g of radix rehmanniae reference material, and making into reference material solution by the same method. Performing thin layer chromatography (general rule 0502) test, sucking the above two solutions 5 μ L, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol-water (14:6:1) as developing agent, taking out, air drying, spraying anisaldehyde solution, and heating at 105 deg.C to spot color development . The results are shown in fig. 3, wherein the original image in fig. 3 is in color, in fig. 3, 1 and 2 are rehmanniae radix reference medicinal materials, and 3 and 4 are Chinese medicinal granule samples for regulating sleep. As is clear from FIG. 3, the test chromatogram showed a spot of the same pigment color at the position corresponding to the control chromatogram.
4. Identification of caulis Polygoni Multiflori
Taking 1.5g of the product particles, grinding into fine powder, taking 1.5g of the powder, adding 50mL of ethanol, heating and refluxing for 1h, filtering, and concentrating the filtrate to 1mL to be used as a test solution. Another control medicinal material of caulis Polygoni Multiflori 0.25g is prepared by the same method as above. Performing thin layer chromatography (general rule 0502) test, sucking 2 μ L of the above three solutions, respectively dropping on the same silica gel H thin layer plate, developing with petroleum ether (30-60 deg.C) -ethyl formate-formic acid (15:5:1) upper layer solution as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (365 nm). The result is shown in fig. 4, the original drawing of fig. 4 is in color, in fig. 4, 1 and 2 are caulis polygoni multiflori reference medicinal materials, and 3 and 4 are Chinese medicinal granule samples for adjusting sleep, and as can be seen from fig. 4, in the chromatogram of the test sample, fluorescent spots with the same color are displayed at the positions corresponding to the chromatogram of the reference medicinal material.
5. Description of other Components identification
The formula of the invention is mainly prepared by taking rehmannia root, acanthopanax root, rhizoma polygonati, mulberry, vine of multiflower knotweed, schisandra fruit, pearl powder and the like as raw materials, wherein the schisandra fruit is taken as an important raw material in the formula, has obvious functions of promoting sleep and the like, is drawn out as an effective component in a standard, and has no definite identification method for corresponding standards of mulberry pearl powder and the like.
Third, research on physical and chemical indexes
The physical and chemical index formulation basis and the inspection method are shown in Table 13.
TABLE 13 formulation basis and inspection method for physicochemical indexes
According to the physicochemical indexes in table 13, the product was studied and verified with three samples, small sample 1, small sample 2 and 180520, and the results are shown in table 14.
TABLE 14 results of physical and chemical indexes
The results in Table 14 show that the physical and chemical indexes of the 3 batches of the traditional Chinese medicine granules for regulating sleep all meet the standard regulations and have stable quality.
Fourth, research on indexes of functional components or marker components
1. Selection of Schisandrin
The Chinese medicinal granules for regulating sleep take schisandra chinensis and the like as main raw materials, and the schisandra chinensis in the formula has a remarkable sleep improvement effect. Schisandrin is a lignan contained in schisandra, mainly contains schisandrin A, deoxyschizandrin and schisandrin B, wherein the schisandrin A is the component with the strongest hypnotic effect in the schisandrin A, and the deoxyschizandrin and the schisandrin B also have certain effects. The main components of other medicinal ingredients are not reported in clear researches on sedation and hypnosis. Meanwhile, the determination of the schisandra chinensis components is also clearly recorded in the national technical Specification for health food inspection and evaluation (2003 edition), and the method is mature and feasible. Therefore, the functional components of the product are schizandrin (the sum of schizandrin A, schizandrin A and schizandrin B).
2. Research on method for determining schizandrin
The method refers to the method of high performance liquid chromatography determination of schisandrin, deoxyschizandrin and deoxyschizandrin in health food in 2003 edition "health food detection and evaluation Specification".
(1) Principle of
Extracting lignan from the sample, separating by isocratic elution reversed phase high performance liquid chromatography, detecting with ultraviolet detector (UV), and quantifying according to retention time of chromatographic peak and external standard method.
(2) Instruments and reagents
(i) Instrument for measuring the position of a moving object
An LC-15C type Shimadzu high performance liquid chromatograph equipped with an SPD-15C type ultraviolet detector, an SIL-10AF type automatic sample injector and an LCsolution 15C chromatographic workstation;
XB-Phenyl column (250 mm. times.4.6 mm, 5 μm); SQP type electronic balance (sidoris); electronic balance model FA2004N (pet electronics ltd, city, chang); SB-5200D ultrasoundWave washer (Ningbo Xinzhi Biotechnology GmbH).
(ii) Reagent
The methanol is chromatographically pure;
schisandrin, deoxyschizandrin and schisandrin B are purchased from China food and drug testing research institute: schizandrol A: 110857 and 201714 with the purity of 99.9 percent;
schizandrin A: 110764 and 201714 with 99.3% purity;
and schisandrin b: 110765-201512 with purity 99.0%.
(3) Detection solution preparation
(i) Preparation of control solution
Accurately weighing appropriate amount of schizandrol A, schizandrin A and schizandrin B reference substances, and preparing into mixed reference solution containing schizandrol A15 μ g/mL, schizandrin A3 μ g/mL and schizandrin B3 μ g/mL.
(ii) Preparation of test sample solutions
Taking a proper amount of sample, grinding into fine powder, sampling 0.5g, accurately weighing, placing in a 25mL measuring flask, adding about 20mL of methanol, carrying out ultrasonic treatment for 20min, taking out, placing to room temperature, adding methanol to scale, shaking uniformly, filtering with a 0.45 mu m filter membrane, and taking a subsequent filtrate as a sample solution.
(4) Detection method verification
(i) System suitability test
Taking traditional Chinese medicine particles (batch number: 180520) for regulating sleep to prepare a test sample solution according to a preparation method of the test sample solution, taking a mixed reference sample solution and the test sample solution, carrying out high performance liquid chromatography determination on schisandrin, deoxyschizandrin and deoxyschizandrin in health food according to 2003 edition of detection and evaluation standards of health food, and injecting 10 mu L:
a chromatographic column:
wondasil series C18 chromatography column (250 mm. times.4.6 mm, 5 μm);
an ultraviolet detector: the detection wavelength is 254 nm;
mobile phase: methanol-water (77: 23);
flow rate: 1.0 ml/min;
sample introduction amount: 10 μ l.
Samples were injected separately and chromatograms were recorded, see figure 5.
As can be seen from the results in FIG. 5, under the above chromatographic conditions, the reference solution and the sample solution have good schizandrin A, schizandrin A and schizandrin B peak shapes, no interference occurs before and after the component peaks, and the chromatographic conditions are good.
(ii) Drawing of standard curve
The mixed reference solution is placed on an automatic sample injector sample rack, 2, 5, 10, 15 and 20 mu L of series standard solutions are injected respectively, and the absorption peak area is determined. The results of linear regression were plotted using the absorption peak area as the ordinate and the concentration of the control solution (. mu.g/mL) as the abscissa, and are shown in Table 15 and FIG. 6.
TABLE 15 results of the Linear test
From the results of table 15 and fig. 6, the sample regression equation is: schizandrol methyl (R) 21207x-1336.7 (R)20.9995), schizandrin y 17933x-71.4 (R)20.99935), schizandrin y 16855x-533.0 (R)2Results show that the linear relation of the schizandrol A in the range of 2.94-29.4 mu g/ml is good, the linear relation of the schizandrin A in the range of 0.672-6.72 mu g/ml is good, and the linear relation of the schizandrin B in the range of 0.734-7.34 mu g/ml is good.
(iii) Precision test
Taking the mixed reference substance solution, continuously processing 3 parts, carrying out sample injection measurement according to the chromatographic conditions, recording the peak area of each sample, and calculating the result RSD of 3 parts of samples, wherein the result is shown in Table 16.
TABLE 16 results of precision test
As can be seen from the results in Table 16, the RSD of the content detection results of schizandrin A, schizandrin A and schizandrin B are respectively 0.61%, 0.62% and 0.61%, which indicates that the method and the component determination precision are good.
(iv) Recovery test
Taking 180520 batches of samples to be tested, wherein the contents of schizandrol A, schizandrin A and schizandrin B are respectively 50mg/100g, 21.59mg/100g and 17.62mg/100g, taking 3 parts, precisely weighing, respectively adding 249.9 mu g of schizandrol A, 101.0 mu g of schizandrin A and 110.2 mu g of schizandrin B, simultaneously processing 3 parts, preparing a solution according to the sample solution processing method, and determining, calculating and recovering the components according to the method. The results are shown in Table 17.
TABLE 17 results of component recovery test
As can be seen from the results in Table 17, the average recovery rates of schizandrol A, deoxyschizandrin and schisandrin B are 105.3%, 98.31% and 96.96%, respectively, which indicates that the component recovery rate is good and the method accuracy is good.
(v) Sample assay
Taking 3 parts of the traditional Chinese medicine granule sample for regulating sleep, and determining the result by the method, the result is shown in table 18.
Table 18 test results
The results in Table 18 show that the content of schizandrin A, schizandrin A and schizandrin B in the traditional Chinese medicine granules for regulating sleep is 49.72mg/100g, 21.80mg/kg and 17.80mg/100g respectively, and the content of schizandrin (calculated by schizandrin A, schizandrin A and schizandrin B) in the product is 89.32mg/100 g. Therefore, the content of schizandrin (calculated by schizandrin A, schizandrin A and schizandrin B) in the proposed product is not less than 72mg/100 g.
(5) Summary of effective component detection method
By combining the research results, the traditional Chinese medicine granules for regulating sleep select schizandrin (calculated by schizandrin A, schizandrin A and schizandrin B) as an effective component, and refer to a detection method formulated by a method of high performance liquid chromatography determination of the schizandrin A, the schizandrin A and the schizandrin B in health food in 2003 edition, the detection method has high precision and better reproducibility, and can be used as a product quality control method and written into product standards.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. A preparation method of traditional Chinese medicine granules for adjusting sleep is characterized by comprising the following steps:
(1) weighing fructus schizandrae, crushing, adding 6-10 times of ethanol with volume concentration of 60-80%, reflux-extracting at 85-95 ℃ for 45-90 min for 1-3 times, filtering to obtain filtrate, and concentrating to relative density of 1.05-1.10 at 60 ℃ to obtain ethanol-extracted concentrated solution;
(2) weighing radix rehmanniae, rhizoma polygonati, mulberry, acanthopanax and caulis polygoni multiflori, adding 8-12 times of water, decocting for 45-90 min, extracting for 1-3 times, filtering to obtain filtrate, and concentrating until the relative density at 60 ℃ is 1.05-1.10 to obtain a water extraction concentrated solution;
(3) mixing the ethanol extract concentrate obtained in the step (1) and the water extract concentrate obtained in the step (2), adding a part of maltodextrin, spray-drying, and crushing to obtain dry extract powder; adding the rest maltodextrin, pearl powder and stevioside into the dry extract powder, granulating, and drying to obtain the traditional Chinese medicine granules for regulating sleep;
the traditional Chinese medicine granules for adjusting sleep comprise the following raw materials in parts by weight: 5-7 parts of radix rehmanniae recen, 5-7 parts of acanthopanax, 3-5 parts of schisandra chinensis, 4-6 parts of rhizoma polygonati, 4-6 parts of caulis polygoni multiflori, 3-5 parts of mulberry and 0.08-0.12 part of pearl; the traditional Chinese medicine granule for adjusting sleep is prepared from 8.5-10.5 parts by weight of maltodextrin and 0.1-0.15 part by weight of stevioside.
2. The preparation method of the traditional Chinese medicine granule for adjusting sleep as claimed in claim 1, wherein the traditional Chinese medicine granule for adjusting sleep is composed of the following raw materials in parts by weight: 6 parts of radix rehmanniae recen, 6 parts of acanthopanax, 4 parts of schisandra chinensis, 5 parts of rhizoma polygonati, 5 parts of caulis polygoni multiflori, 4 parts of mulberry and 0.1 part of pearl.
3. The method for preparing traditional Chinese medicine granules for sleep regulation as claimed in claim 1, wherein in step (1), the number of extraction times is 2, 10 times of ethanol is added each time, the volume concentration is 70%, and the time of each reflux extraction is 60 min.
4. The method for preparing traditional Chinese medicine granules for sleep regulation as claimed in claim 1, wherein in step (2), the number of extraction times is 2, the amount of water added for the first extraction is 10 times, the amount of water added for the second extraction is 8 times, the first extraction time is 90min, and the second extraction time is 60 min.
5. The method for preparing traditional Chinese medicine granules for regulating sleep as claimed in claim 1, wherein in the step (1) and the step (2), the concentration is carried out under reduced pressure at 80 ± 5 ℃.
6. The preparation method of the traditional Chinese medicine granules for adjusting sleep according to claim 1, wherein in the step (3), the ethanol extract concentrated solution obtained in the step (1) and the water extract concentrated solution obtained in the step (2) are combined and uniformly mixed, heated to 70-90 ℃, added with 20% of the total weight of maltodextrin to be dissolved, spray-dried and crushed to obtain dry extract powder; and then uniformly mixing the pearl powder and stevioside, adding the rest maltodextrin by an equivalent increment method, adding the dry extract powder, uniformly mixing, adding 50% ethanol for granulation, and drying at 75-80 ℃.
7. The method for preparing traditional Chinese medicine granules for regulating sleep as claimed in claim 1, wherein in the step (1), the size of the crushed traditional Chinese medicine granules is 24 meshes.
8. The method for preparing traditional Chinese medicine granules for adjusting sleep as claimed in claim 1, wherein in the step (3), the air inlet temperature of the spray drying is 185 ± 5 ℃, and the air outlet temperature is 100-105 ℃.
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