CN115120567A - Method for improving content of effective ingredients in radix puerariae and rhizoma polygonati hypoglycemic chewable tablets - Google Patents
Method for improving content of effective ingredients in radix puerariae and rhizoma polygonati hypoglycemic chewable tablets Download PDFInfo
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Abstract
The invention provides a method for improving the content of active ingredients in a kudzuvine root and polygonatum sibiricum blood sugar reducing chewable tablet, which comprises the following steps: s1, mixing the kudzu vine root powder with an ethanol solution according to the material-liquid ratio of 1 g: 14-18 mL, then carrying out ultrasonic extraction, concentrating the filtrate into an extract, and drying to obtain a kudzu vine root extract; s2, mixing the polygonatum sibiricum powder with water, and adding complex enzyme for enzymolysis; s3, mixing the mixed solution obtained after the enzymolysis of the S2 with water, then carrying out ultrasonic extraction, concentrating the filtrate into an extract, and drying to obtain a sealwort extract; s4, mixing the kudzu root extract and the rhizoma polygonati extract according to the mass ratio of 1: 2-3, adding auxiliary materials, and then preparing the chewable tablet by a wet granulation and tabletting method. The method can achieve the purposes of saving energy and retaining the effective components of puerarin and polygonatum polysaccharide to the maximum extent, and provides a health-care food with good taste and convenient use for diabetics.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine extraction and chewable tablet preparation, in particular to a method for improving the content of effective ingredients in kudzu root and rhizoma polygonati hypoglycemic chewable tablets.
Background
The kudzu root is the dry root of the leguminous plant kudzu, is known as kudzu, has brown surface, has longitudinal wrinkles, solid quality, rough section, strong fiber property, slightly powdery property, sweet and pungent taste and cool property, is an important medicinal and edible plant, has extremely high nutritional value, has the reputation of longevity powder and Asian ginseng, and is a good raw material for preparing health-care food. The kudzu root contains various effective components such as flavonoid, polysaccharide, triterpenoid saponins, alkaloid, amino acid and the like, and researches show that the pueraria root flavone is the most main effective component and has definite functions of reducing blood sugar and blood fat. The pueraria flavone is also called puerarin, mainly takes alcoholic solution as solvent, and is extracted by a heating and leaching way, but the extraction rate is lower in the extraction process, and the industrialized production is not facilitated.
Rhizoma Polygonati is dried rhizome of Polygonatum kingianum, Polygonatum sibiricum or Polygonatum cyrtonema of Liliaceae, and is called "rheum officinale essence", "Polygonatum sibiricum Rehd" or "Polygonatum cyrtonema Hua" according to different shapes. The sealwort polysaccharide is one of the main active ingredients of sealwort, and has a plurality of functions of resisting aging and oxidation, regulating immunity, reducing blood sugar, reducing blood fat, resisting bacteria, diminishing inflammation and the like. The polygonatum polysaccharide is usually extracted by adopting a water extraction method, but the extraction rate is relatively low.
The chewable tablet is convenient to take and is suitable for diabetics to carry and take. However, no report is found on the preparation of sugar-reducing chewable tablets by mixing pueraria flavone and polygonatum polysaccharide at present. Therefore, in order to improve the curative effect of the sugar-reducing chewable tablets, a method for improving the content of the effective ingredients in the sugar-reducing chewable tablets containing radix puerariae and rhizoma polygonati is needed.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for improving the content of effective ingredients in pueraria and polygonatum hypoglycemic chewable tablets. The method can achieve the purposes of saving energy and retaining the effective components of puerarin and polygonatum polysaccharide to the maximum extent, and provides a health-care food with good taste and convenient use for diabetics.
In order to achieve the above object, the technical scheme of the invention is as follows.
A method for improving the content of active ingredients in radix puerariae and rhizoma polygonati hypoglycemic chewable tablets comprises the following steps:
s1, mixing the kudzu vine root powder with an ethanol solution according to the material-liquid ratio of 1 g: 14-18 mL, then carrying out ultrasonic extraction, concentrating the filtrate into an extract, and drying to obtain a kudzu vine root extract;
s2, mixing the polygonatum sibiricum powder with water, and adding complex enzyme for enzymolysis;
s3, mixing the mixed solution obtained after the enzymolysis of the S2 with water, then carrying out ultrasonic extraction, concentrating the filtrate into an extract, and drying to obtain a polygonatum sibiricum extract;
s4, mixing the kudzu root extract and the polygonatum extract according to the mass ratio of 1: 2-3, adding auxiliary materials, and then preparing the chewable tablet by a wet granulation and tabletting method.
Further, in the S1, the mass percentage concentration of the ethanol solution is 40-60%.
Further, in S1, the ultrasonic extraction conditions were as follows: the ultrasonic temperature is 50-60 ℃; the ultrasonic time is 30-50 min.
Further, in S1 and S3, the relative density of the extract was 1.10(60 ℃).
Further, in S2, the mass ratio of rhizoma Polygonati powder to water is 10 g: 20-40 mL.
Further, in S2, the complex enzyme is cellulase and/or pectinase.
Furthermore, in S2, the complex enzyme is a mixture of cellulase and pectinase in a mass ratio of 2: 2-4.
Furthermore, in S2, the addition amount of the complex enzyme is 0.2-0.5% of the mass of the rhizoma polygonati powder.
Further, in S2, the conditions for enzymatic hydrolysis are as follows: the pH value of enzymolysis is 6.5-6.8; the enzymolysis time is 20-40 min; the temperature of enzymolysis is 50-70 ℃.
Further, in S4, the adjuvants include aspartame, citric acid, isomalt, and peppermint oil; the mass ratio of the kudzu root dry paste powder to the aspartame, the citric acid, the isomaltitol and the peppermint oil is 1: 4-5: 0.03: 0.1: 0.01;
the specific process for preparing the chewable tablet by the wet granulation and tabletting method comprises the following steps:
mixing radix Puerariae extract and rhizoma Polygonati extract, adding aspartame, citric acid and isomalt, mixing, adding 90% ethanol solution as wetting agent, making soft mass, granulating, drying, adding 0.3% magnesium stearate, mixing, spraying appropriate amount of oleum Menthae Dementholatum, and tabletting.
The invention has the beneficial effects that:
1. the kudzuvine root and polygonatum sibiricum blood sugar reducing chewable tablet prepared by the invention has the advantages that: the dosage is accurate, and the decoction pieces are extracted to remove ineffective tissue components, so that the dosage is reduced; the chewable tablet is especially suitable for the old, children and other dysphagia patients to take, and compared with the common tablet, the chewable tablet is convenient to carry and take and has good food therapy effect. The aspartame and isomaltitol in the chewable tablet are sugar-free auxiliary materials, so that the application population is expanded, and a safe, efficient, novel and convenient health food is provided for the diabetics.
2. The method can achieve the purposes of saving energy and retaining the effective components of puerarin and polygonatum polysaccharide to the maximum extent, and provides a health-care food with good taste and convenient use for diabetics.
3. The extraction rate of puerarin extracted by adopting an ultrasonic method is 1.20 times that of a reflux method, and the extraction rate of polygonatum polysaccharide extracted by adopting an enzyme-assisted ultrasonic auxiliary method is 2.17 times that of single ultrasonic. The method of the invention achieves the purposes of saving energy and retaining the effective components of puerarin and polygonatum polysaccharide to the maximum extent.
4. The preparation process of the kudzuvine root and polygonatum sibiricum blood sugar reducing chewable tablet provided by the invention has the advantages that the taste, the properties, the appearance, the hardness, the friability, the weight difference and the microbial limit all accord with the regulations.
Drawings
FIG. 1 is a graph of the effect of different ethanol concentrations on puerarin extraction yield.
FIG. 2 is a graph showing the effect of different feed liquid ratios on the puerarin extraction rate.
Fig. 3 is a graph of the effect of different sonication times on puerarin extraction yield.
Fig. 4 is a graph of the effect of different ultrasound temperatures on puerarin extraction yield.
FIG. 5 is a standard chromatogram.
FIG. 6 is a chromatogram of sample 1.
FIG. 7 is a chromatogram of sample 2.
FIG. 8 is a chromatogram of sample 3.
FIG. 9 is a D-anhydroglucose standard curve.
FIG. 10 is a graph of the effect of different biological enzymes on the extraction yield of polygonatum polysaccharides.
FIG. 11 is a graph of the effect of different sonication times on the extraction yield of polygonatum polysaccharides.
FIG. 12 is a graph of the effect of different enzymatic hydrolysis times on the extraction yield of polygonatum polysaccharides.
FIG. 13 is a graph of the effect of different enzyme hydrolysis temperatures on the extraction yield of polygonatum polysaccharides.
FIG. 14 is a graph showing the effect of different enzyme addition amounts on the extraction yield of polygonatum polysaccharides.
Fig. 15 is a picture of pueraria sibirica hypoglycemic chewable tablets prepared in example 1 of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the invention, the pueraria flavone is puerarin.
The materials and reagents used in the examples of the present invention are shown in Table 1. Wherein, the kudzu root is identified as the dry root of Pueraria lobata Ohwi of Leguminosae; rhizoma Polygonati was identified as a dry rhizome of Polygonatum sibiricum of Liliaceae.
TABLE 1 materials and reagents
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
A method for improving the content of active ingredients in radix puerariae and rhizoma polygonati hypoglycemic chewable tablets comprises the following steps:
s1, extraction of pueraria flavone
S1.1, cleaning the kudzu root medicinal material with drinking water, drying in a drying oven at 105 ℃, crushing, and sieving with a 24-mesh sieve for later use.
S1.2, weighing 10.00g of kudzuvine root powder, adding 40% ethanol solution according to the material-liquid ratio of 1g to 14mL, carrying out ultrasonic extraction at 50 ℃ for 50min with the ultrasonic power of 500W, and filtering; repeatedly ultrasonically extracting the filter residue once, and filtering; the two filtrates were combined.
S1.3, concentrating the filtrate into an extract with the relative density of 1.10(60 ℃), and carrying out low-temperature spray drying to obtain the kudzu root dry extract powder. The extraction rate of pueraria flavone is 3.70%, and the dry extract rate is 31.5%.
S2, and extracting rhizoma polygonati polysaccharide
S2.1, cleaning the rhizoma polygonati medicinal material with drinking water, moistening thoroughly, slicing, drying in a 105 ℃ oven, and crushing into 30-mesh powder for later use.
S2.2, weighing 10.00g of rhizoma polygonati powder into a conical flask, and adding a complex enzyme which is 0.3 percent of the mass of the rhizoma polygonati powder, wherein the complex enzyme is the mixture of cellulase and pectinase according to the mass ratio of 2: 3; adding 30mL of purified water, adjusting the pH value to 6.5, and carrying out enzymolysis for 40min at the water bath temperature of 50 ℃;
adding 70mL of purified water, performing ultrasonic treatment for 60min at 50 ℃ by using an ultrasonic instrument with the ultrasonic power of 500W, cooling to room temperature, putting into a centrifuge, centrifuging for 15min at the rotating speed of 5000r/min, and performing suction filtration; repeatedly ultrasonically extracting the filter residue once, and performing suction filtration; the two filtrates were combined.
And S2.3, concentrating the filtrate into an extract with the relative density of 1.10(60 ℃), and performing low-temperature spray drying to obtain rhizoma polygonati dry extract powder. The extraction rate of the polygonatum polysaccharide is 66.42 percent, and the dry paste rate is 85.9 percent.
S3 preparation of radix puerariae and rhizoma polygonati hypoglycemic chewable tablets
Mixing radix Puerariae dry extract powder and rhizoma Polygonati dry extract powder at a mass ratio of 1: 2.9, adding aspartame, citric acid and isomaltitol, and mixing well, wherein the mass ratio of radix Puerariae dry extract powder to aspartame, citric acid and isomaltitol is 1: 4.47: 0.03: 0.1;
spraying appropriate wetting agent with 90% ethanol as wetting agent to make soft material, making into hand-held mass, and slightly pressing to disperse; extruding and granulating with 20 mesh screen, drying in 60 deg.C oven for 3 hr, and grading with 20 mesh sieve; finally adding magnesium stearate which is 0.3 percent of the total mass of the granules, and uniformly mixing; spraying appropriate amount of oleum Menthae Dementholatum, moistening for 1 hr, and tabletting.
Example 2
A single-factor test was conducted on the extraction process of pueraria flavones by using the ethanol concentration according to the method in example 1, so as to investigate the influence of the ethanol concentration on the extraction rate of pueraria flavones.
Weighing 10.00g of radix Puerariae powder, setting ethanol concentrations of 40%, 50%, 60%, 70% and 80%, respectively, performing ultrasonic treatment at 55 deg.C for 30min with 60mL of ethanol with different concentrations, and performing ultrasonic treatment at 55 deg.C for 20min with 40mL of ethanol with different concentrations to study the influence of ethanol concentration on extraction rate, and the result is shown in FIG. 1.
Example 3
According to the method in the embodiment 1, a single-factor test is carried out on the extraction process of pueraria flavonid according to the material-liquid ratio, so as to explore the influence of the material-liquid ratio on the extraction rate of the pueraria flavonid.
10.00g of kudzu powder is weighed, the material-liquid ratio (g/mL) is respectively set to be 1: 10, 1: 12, 1: 14, 1: 16 and 1: 18, the ethanol concentration is the optimal concentration of the embodiment 2, ultrasonic treatment is carried out at 55 ℃ for 30min, so as to research the influence of the material-liquid ratio on the extraction rate of the kudzu flavone, and the result is shown in figure 2.
Example 4
According to the method in the embodiment 1, a single-factor test is carried out on the extraction process of pueraria flavone by using ultrasonic time, so as to explore the influence of the ultrasonic time on the extraction rate of pueraria flavone.
10.00g of radix puerariae powder is weighed, the material-liquid ratio is the optimal material-liquid ratio of the embodiment 3, the ethanol concentration is the optimal ethanol concentration of the embodiment 2, the ultrasonic temperature is 55 ℃, and the ultrasonic time is respectively set to be 30min, 40min, 50min, 60min and 70min so as to research the influence of the ultrasonic time on the extraction rate of the radix puerariae flavone, and the result is shown in fig. 3.
Example 5
According to the method in the embodiment 1, a single-factor test is carried out on the extraction process of pueraria flavonid at the ultrasonic temperature, so as to explore the influence of the factor of the ultrasonic temperature on the extraction rate of the pueraria flavonid.
10.00g of kudzu root powder is weighed, the material-liquid ratio is the optimal material-liquid ratio of the embodiment 3, the ethanol concentration is the optimal ethanol concentration of the embodiment 2, the ultrasonic temperature is respectively set to be 45 ℃, 50 ℃, 55 ℃, 60 ℃ and 65 ℃, and the ultrasonic time is the optimal ultrasonic time of the embodiment 4, so as to study the influence of the ultrasonic temperature on the extraction rate, and the result is shown in fig. 4.
Example 6
A four-factor three-level orthogonal optimization test is carried out on the extraction process of pueraria flavones according to the method in the embodiment 1, and the specific factor levels are shown in a table 2.
TABLE 2 Quadrature optimization test factor levels for pueraria flavonoid extraction
Wherein A is ethanol concentration (%), B is material-liquid ratio (g/mL), C is ultrasonic time (min), and D is ultrasonic temperature (DEG C).
Example 7
The extraction process of pueraria flavonid was repeated for the verification test according to the method of example 1.
A parallel experiment was performed by using 3 parts of kudzu root powder (10.00g) according to the best extraction process obtained in example 6, and the results are shown in FIGS. 5 to 8 and Table 6.
Example 8
The extraction process of polygonatum polysaccharide was subjected to a screening test of biological enzymes according to the method of example 1.
In the enzymolysis process, methods without adding enzyme, alpha-amylase, xylanase, papain, cellulase, pectinase and complex enzyme are respectively adopted, and the influence of 6 biological enzymes on the extraction rate of the polygonatum polysaccharide is examined. Wherein test groups without enzymes, alpha-amylase, xylanase, papain, cellulase, pectinase and complex enzyme are respectively numbered as 0-6. The extraction rate of rhizoma Polygonati polysaccharide is used as index to find out the optimum biological enzyme for hydrolyzing rhizoma Polygonati, as shown in FIG. 10.
Example 9
The extraction process of polygonatum polysaccharide was subjected to a single factor test with ultrasound time according to the method of example 1 to investigate the effect of the ultrasound time on the extraction rate of polygonatum polysaccharide.
Weighing 10.00g of rhizoma polygonati powder, adding 30mL of purified water, adding the optimal complex enzyme determined in the embodiment 8, performing enzymolysis in water bath at 50 ℃ for 30min, adding 70mL of purified water, performing ultrasonic extraction twice at 55 ℃, and setting ultrasonic time for 30min, 40min, 50min, 60min and 70min respectively to explore the influence of the ultrasonic time on the extraction rate of rhizoma polygonati polysaccharide, wherein the result is shown in FIG. 11.
Example 10
According to the method in the embodiment 1, a single-factor test is carried out on the extraction process of polygonatum polysaccharide by using enzymolysis time, so as to explore the influence of the enzymolysis time on the extraction rate of polygonatum polysaccharide.
Weighing 10.00g of rhizoma polygonati powder, adding 30mL of purified water, adding the optimal complex enzyme determined in the embodiment 8, carrying out enzymolysis in water bath at 50 ℃, setting the enzymolysis time to be 10min, 20min, 30min, 40min and 50min respectively, adding 70mL of purified water, carrying out ultrasonic extraction twice at 55 ℃, and researching the influence of the enzymolysis time of the enzyme in the water bath on the polysaccharide extraction rate, wherein the result is shown in figure 12.
Example 11
According to the method in the embodiment 1, a single-factor test is carried out on the extraction process of the polygonatum polysaccharide by using the enzymolysis temperature so as to explore the influence of the enzymolysis temperature on the extraction rate of the polygonatum polysaccharide.
Weighing 10.00g of rhizoma polygonati powder, adding 30mL of purified water, adding the optimal complex enzyme determined in the embodiment 8, setting the enzymolysis temperature to be 30 ℃, 40 ℃, 50 ℃, 60 ℃ and 70 ℃ respectively, setting the enzymolysis time to be the optimal time in the embodiment 10, adding 70mL of purified water, and setting the ultrasonic time to be the optimal time in the embodiment 9 at 55 ℃ so as to explore the influence of the enzymolysis temperature of the enzyme in the water bath on the polysaccharide extraction rate, wherein the result is shown in FIG. 13.
Example 12
According to the method in the embodiment 1, a single-factor test is carried out on the extraction process of the polygonatum polysaccharide according to the percentage of the enzyme in the substrate, so as to explore the influence of the factor of the percentage of the enzyme in the substrate on the extraction rate of the polygonatum polysaccharide.
Weighing 10.00g of rhizoma polygonati powder, adding 30mL of purified water, adding the optimal enzyme, setting the enzyme adding amount as 0.20%, 0.25%, 0.30%, 0.35% and 0.40% of the substrate, the enzymolysis temperature as the optimal temperature of example 11, the enzymolysis time as the optimal time of example 10, adding 70mL of purified water, and the ultrasonic time as the optimal time of example 9, so as to investigate the influence of the enzyme adding amount on the polysaccharide extraction rate, wherein the result is shown in FIG. 14.
Example 13
A four-factor three-level orthogonal optimization test is carried out on the extraction process of the polygonatum polysaccharide according to the method in the embodiment 1, and the specific factor levels are shown in a table 3.
TABLE 3 orthogonal optimization test factor levels for Polygonatum polysaccharide extraction
Wherein A is ultrasonic time (min), B is enzymolysis time (min), C is enzymolysis temperature (DEG C), and D is enzyme addition amount (%).
Example 14
The extraction process of polygonatum polysaccharide was subjected to repeated verification tests according to the method of example 1.
3 parts of Polygonatum sibiricum powder (10.00g) were taken and subjected to parallel tests in accordance with the optimum extraction process obtained in example 13, and the results are shown in Table 11.
Example 15
A method for improving the content of active ingredients in radix puerariae and rhizoma polygonati hypoglycemic chewable tablets comprises the following steps:
s1, extracting pueraria flavone according to the method of the embodiment 1;
s2, and extracting rhizoma polygonati polysaccharide
S2.1, cleaning the rhizoma polygonati medicinal material with drinking water, moistening thoroughly, slicing, drying in a 105 ℃ oven, and crushing into 30-mesh powder for later use.
S2.2, weighing 10.00g of polygonatum sibiricum powder into a conical flask, and adding a complex enzyme which is 0.3 percent of the mass of the polygonatum sibiricum powder, wherein the complex enzyme is a mixture of cellulase and pectinase according to the mass ratio of 2: 2; adding 20mL of purified water, adjusting the pH value to 6.7, and carrying out enzymolysis for 40min at the water bath temperature of 50 ℃; adding 80mL of purified water, performing ultrasonic treatment at 50 ℃ for 60min by using an ultrasonic instrument with the ultrasonic power of 500W, cooling to room temperature, putting into a centrifuge, centrifuging at the rotating speed of 5000r/min for 15min, and performing suction filtration; repeatedly carrying out ultrasonic extraction on filter residues once, and carrying out suction filtration; the two filtrates were combined.
And S2.3, concentrating the filtrate into an extract with the relative density of 1.10(60 ℃), and performing low-temperature spray drying to obtain rhizoma polygonati dry extract powder.
S3 preparation of radix puerariae and rhizoma polygonati hypoglycemic chewable tablets
Mixing radix Puerariae dry extract powder and rhizoma Polygonati dry extract powder at a mass ratio of 1: 2, adding aspartame, citric acid and isomaltitol, and mixing well, wherein the mass ratio of radix Puerariae dry extract powder to aspartame, citric acid and isomaltitol is 1: 4: 0.03: 0.1; spraying appropriate wetting agent with 90% ethanol as wetting agent to obtain soft material, making into hand-held mass, and dispersing under light pressure; extruding and granulating with 20 mesh screen, drying in 60 deg.C oven for 3 hr, and grading with 20 mesh sieve; finally adding magnesium stearate which is 0.3 percent of the total mass of the granules, and uniformly mixing; spraying appropriate amount of oleum Menthae Dementholatum, moistening for 1 hr, and tabletting.
Example 16
A method for improving the content of active ingredients in radix puerariae and rhizoma polygonati hypoglycemic chewable tablets comprises the following steps:
s1, extracting pueraria flavone according to the method of the embodiment 1;
s2, extraction of polygonatum polysaccharide
S2.1, cleaning the rhizoma polygonati medicinal material with drinking water, moistening thoroughly, slicing, drying in a 105 ℃ oven, and crushing into 30-mesh powder for later use.
S2.2, weighing 10.00g of polygonatum sibiricum powder into a conical flask, and adding a complex enzyme which is 0.3 percent of the mass of the polygonatum sibiricum powder, wherein the complex enzyme is a mixture of cellulase and pectinase according to the mass ratio of 2: 4; adding 40mL of purified water, adjusting the pH value to 6.8, and carrying out enzymolysis for 40min at the water bath temperature of 50 ℃; adding 60mL of purified water, performing ultrasonic treatment at 50 ℃ for 60min by using an ultrasonic instrument with the ultrasonic power of 500W, cooling to room temperature, putting into a centrifuge, centrifuging at the rotating speed of 5000r/min for 15min, and performing suction filtration; repeatedly carrying out ultrasonic extraction on filter residues once, and carrying out suction filtration; the two filtrates were combined.
And S2.3, concentrating the filtrate into an extract with the relative density of 1.10(60 ℃), and performing low-temperature spray drying to obtain rhizoma polygonati dry extract powder.
S3 preparation of radix puerariae and rhizoma polygonati hypoglycemic chewable tablets
Mixing radix Puerariae dry extract powder and rhizoma Polygonati dry extract powder at a mass ratio of 1: 3, adding aspartame, citric acid and isomaltitol, and mixing well, wherein the mass ratio of radix Puerariae dry extract powder to aspartame, citric acid and isomaltitol is 1: 5: 0.03: 0.1; spraying appropriate wetting agent with 90% ethanol as wetting agent to obtain soft material, making into hand-held mass, and dispersing under light pressure; extruding and granulating with 20 mesh screen, drying in 60 deg.C oven for 3 hr, and grading with 20 mesh sieve; finally adding magnesium stearate which is 0.3 percent of the total mass of the granules, and uniformly mixing; spraying appropriate amount of oleum Menthae Dementholatum, moistening for 1 hr, and tabletting.
Comparative example 1
The extraction method of pueraria flavone comprises the following steps:
s1.1, cleaning the kudzu root medicinal material with drinking water, drying in a drying oven at 105 ℃, crushing, and sieving with a 24-mesh sieve for later use.
S1.2, weighing 10.00g of kudzuvine root powder, adding 40 wt% ethanol solution according to the material-liquid ratio of 1g to 16mL, and carrying out reflux extraction at 50 ℃ for 50 min; extracting the residue under reflux, filtering, and mixing the filtrates.
S1.3, concentrating the filtrate into an extract with the relative density of 1.10(60 ℃), and carrying out low-temperature spray drying to obtain the kudzu root dry extract powder.
Comparative example 2
The extraction method of the polygonatum polysaccharide comprises the following steps:
s2.1, cleaning the rhizoma polygonati medicinal material with drinking water, moistening thoroughly, slicing, drying in a 105 ℃ oven, and crushing into 30-mesh powder for later use.
S2.2, weighing 10.00g of rhizoma polygonati powder in a conical flask, adding 70mL of purified water, carrying out ultrasonic treatment for 60min at 50 ℃ by using an ultrasonic instrument with the ultrasonic power of 500W, cooling to room temperature, putting the mixture into a centrifugal machine, centrifuging for 15min at the rotating speed of 5000r/min, and carrying out suction filtration; repeatedly ultrasonically extracting the filter residue once, and performing suction filtration; the two filtrates were combined.
And S2.3, concentrating the filtrate into an extract with the relative density of 1.10(60 ℃), and performing low-temperature spray drying to obtain rhizoma polygonati dry extract powder.
The process methods of examples 1 to 14 and comparative examples 1 to 2 are followed to detect the extraction rate of pueraria flavone, the extraction rate of polygonatum polysaccharide and the quality of pueraria polygonatum hypoglycemic chewable tablets.
1. Method for detecting extraction rate of pueraria flavone
1.1 chromatographic conditions
Methanol-0.3% phosphoric acid water solution (25: 75) is used as a mobile phase, octadecylsilane chemically bonded silica is used as a filler, the detection wavelength is 250nm, the flow rate is 1.00mL/min, the sample injection amount is 20 mu L, the column temperature is 30 ℃, and the theoretical plate number is not less than 4000 according to the puerarin peak.
1.2 preparation of Puerarin reference solution
Accurately weighing 0.0100g puerarin standard, dissolving with 30% ethanol for several times, diluting to constant volume in 10mL volumetric flask, transferring 0.8mL from the solution after constant volume, diluting with 30% ethanol to constant volume in 10mL volumetric flask, and making into solution containing 80 μ g per 1 mL.
1.3 detection of Pueraria flavone extraction rate
Mixing the two extraction filtrates, adding ethanol to a volumetric flask with a constant volume of 200mL, shaking up, precisely transferring 1.0mL of the above solution, adding ethanol to a volumetric flask with a constant volume of 25mL, and shaking up. According to HPLC, 20. mu.L of each of the control solution and the sample solution passed through a 0.45 μm microporous membrane was precisely aspirated, and the solutions were injected into a liquid chromatograph, measured, and the extraction rate was calculated.
Wherein Ax is the peak area of the test solution; ar is the peak area of the reference substance solution; cr is the concentration of the reference solution; m is the weight of the weighed medicinal materials.
2. Method for detecting extraction rate of polygonatum polysaccharide
2.1 preparation of Anhydrous glucose reference solution
Taking a D-anhydroglucose standard substance, drying the D-anhydroglucose standard substance in an oven at 105 ℃ to constant weight, precisely weighing 0.0100g of D-anhydroglucose standard substance, dissolving the D-anhydroglucose standard substance in a small amount of purified water, placing the D-anhydroglucose standard substance in a 10mL volumetric flask, washing the container for multiple times, transferring the washing solution to the volumetric flask, fixing the volume by using the purified water, precisely transferring 3.3mL of the D-anhydroglucose standard substance from the solution after fixing the volume, placing the D-anhydroglucose standard substance in the 10mL volumetric flask, fixing the volume by using the purified water, and preparing a solution containing 0.33mg of D-anhydroglucose per 1 mL.
2.2 preparation of Standard Curve
Precisely measuring 0.0mL, 0.1mL, 0.2mL, 0.3mL, 0.4mL, 0.5mL and 0.6mL of anhydrous glucose reference substance solution, respectively placing the anhydrous glucose reference substance solution into 25mL test tubes with plugs, adding purified water to 2.0mL respectively, shaking up, slowly dripping 0.2% anthrone-sulfuric acid solution into an ice water bath until the volume is 10mL of scale mark, shaking up, cooling down, placing in the water bath for heat preservation for 10min, taking out, immediately placing in the ice water bath for cooling for 10 min. Each solution was placed in sequence in an ultraviolet-visible spectrophotometer and absorbance was measured at a wavelength of 582 nm. The standard curve was plotted, as shown in FIG. 9 and Table 7.
2.3 detection of the extraction yield of Polygonatum sibiricum polysaccharide
And combining the two extraction filtrates, adding purified water to a constant volume of 100mL, shaking up, precisely transferring 0.2mL of the solution into a 100mL volumetric flask, adding purified water to a constant volume, precisely transferring 2.0mL to 10mL volumetric flask, and adding purified water to a scale mark. Precisely transferring 1.0mL of the solution into a 25mL test tube with a plug, adding purified water to 2.0mL according to the method under the item of a standard curve, shaking up, slowly dropwise adding a 0.2% anthrone-sulfuric acid solution into an ice water bath to 10mL of scale mark, shaking up, cooling, placing in a 98 ℃ water bath, preserving the temperature for 10min, taking out, immediately placing in the ice water bath, cooling for 10min, and taking out corresponding reagents as blank. The mixture was placed in an ultraviolet-visible spectrophotometer and absorbance was measured at a wavelength of 582 nm. And finally, calculating the extraction rate of the polygonatum polysaccharide.
3. Quality investigation of radix puerariae and rhizoma polygonati hypoglycemic chewable tablets
3.1, appearance: the product should be complete, smooth and uniform in color.
3.2, Properties: the product should be light brown yellow tablet, fragrant and sweet.
3.3, hardness: sequentially taking 5 tablets of the radix puerariae and rhizoma polygonati hypoglycemic chewable tablets, putting the tablets into a tablet hardness tester, recording data, and carrying out hardness inspection according to the specification of the tablet hardness tester, wherein the hardness is 50-200N, as shown in Table 14.
3.4, friability: taking 10 tablets of kudzuvine root and polygonatum sibiricum blood sugar reducing chewable tablets, blowing off powder on the surfaces of the tablets by using a blower, precisely weighing, placing the tablets in a roller, rotating for 4min, namely 100 times, taking out, blowing off the powder on the surfaces by using the blower, precisely weighing, and checking the tablets with the loss weight not exceeding 1 percent according to the regulation of pharmacopoeia, wherein the tablets with the breakage, cracking and crushing are not checked, and shown in a table 15.
3.5, weight difference: taking 20 tablets of radix puerariae and rhizoma polygonati hypoglycemic chewable tablets, precisely weighing the total tablet weight, and calculating the average tablet weight. And precisely weighing each piece, recording the weight of each piece, and comparing the weight of each piece with the average weight. According to pharmacopoeia regulations, there must be no more than 2 tablets out of weight difference limit and no more than one time of 1 tablet out of limit, as in table 16.
3.6, microbial limit: the inspection is carried out according to the pharmacopoeia microorganism limit inspection method dish method, and the inspection is in accordance with the regulations.
4. Results and analysis
4.1 radix Puerariae extraction Process result analysis
4.1.1, preliminary test
TABLE 4 comparison of the reflux method with the ultrasonic method
Wherein the peak area of the control solution is 3023210.300. As shown in Table 4, the ultrasonic extraction method was used since the extraction rate of puerarin was high.
4.1.2 analysis of Single factor test results
4.1.2.1 influence of different ethanol concentrations on puerarin extraction rate
As shown in fig. 1, when the ethanol concentration is 50%, the extraction rate of puerarin is the maximum, and is 3.44%, the extraction rate is decreased when the ethanol concentration is increased, and the decrease is slow when the ethanol concentration reaches 70% or 80%, so the optimal ethanol concentration is 50%.
4.1.2.2, influence of different feed liquid ratios on puerarin extraction rate
As shown in figure 2, the extraction rate of puerarin is continuously increased along with the increase of the feed-liquid ratio, the solid-liquid ratio is in the range of 1: 10 to 1: 16, the extraction rate of puerarin is in an increasing trend, the feed-liquid ratio is 1 g: 16mL, the extraction rate of puerarin is the highest and is 3.42%, and when the feed-liquid ratio reaches 1: 18, the extraction rate of puerarin is in a decreasing trend obviously. Therefore, the optimal feed-liquid ratio is 1 g: 16 mL.
4.1.2.3 influence of different ultrasonic time on puerarin extraction rate
As shown in FIG. 3, when the ultrasound time was 40min, the extraction rate of puerarin reached the highest, 3.39%. When the ultrasonic time exceeds 50min, the extraction rate begins to decrease after the ultrasonic time reaches 60-70 min although the ultrasonic time rises. And the extraction rate is lower than 40min at 60 min. Therefore, the optimal ultrasonic time is 40 min.
4.1.2.4 influence of different ultrasonic temperatures on Puerarin extraction
As shown in FIG. 4, the ultrasonic temperature is 45-55 ℃, and the extraction rate is increased; the extraction rate is reduced in the range of 55-65 ℃. The rising trend is steeper than the falling trend, and the extraction rate at 55 ℃ is the highest, 3.41%, so the optimum sonication temperature is 55 ℃.
4.1.3 analysis of orthogonal test results
TABLE 5 orthogonal test results for Pueraria lobata
In the case of a of 0.05, analysis of variance was performed with the ultrasonic temperature (D) as an error, as shown in table 4.
TABLE 6 analysis of variance
Orthogonal test results and variance analysis in tables 5 and 6 show that the factor C has greater significance, and the influence sequence of each factor on the puerarin extraction rate is C & gt A & gt B & gt D, namely, the ultrasonic time & gt the ethanol concentration & gt the material-liquid ratio & gt the ultrasonic temperature. The best process combination from the orthogonal experimental optimization is C 3 A 1 B 1 D 3 However, in order to save energy, the optimum process combination determined is C 3 A 1 B 1 D 1 Namely, the ultrasonic time is 50min, the ethanol concentration is 40 percent, the material-liquid ratio is 1 g: 14mL, and the ultrasonic temperature isThe best process is used when the temperature is 50 ℃.
4.1.4, repeated verifiability test results
TABLE 7 repeated verifiability test results
The above scheme was subjected to three parallel verifications, as per experiment scheme C 3 A 1 B 1 D 1 The mean extraction rate of puerarin was 3.70%, which is higher than any set of data in the orthogonal table, and the test was considered to be feasible.
4.2 analysis of the Process results of Polygonatum sibiricum Red extraction
4.2.1 drawing of glucose standard curve and measuring result of standard solution absorbance
Drawing a standard curve by taking the concentration (X) of the D-anhydrous glucose standard solution as an abscissa and the absorbance value (Y) as an ordinate, and fitting to obtain a regression equation: Y37.654X +0.0929 (R) 2 0.9996). The result shows that the concentration of the glucose standard solution is 0.0033-0.0198 mg/mL, and the absorbance and the glucose concentration present a good linear relationship.
TABLE 8D Absorbance-concentration table of standard anhydrous dextrose solution
4.2.2 analysis of preliminary test results
As can be seen from fig. 10, when the polygonatum polysaccharide is extracted under the optimal enzymolysis conditions of the above 6 kinds of biological enzymes, the extraction rates of the cellulase 4 and the pectinase 5 are high, respectively 49.54% and 50.21%, and the two enzymes 4 and 5 with higher extraction rates are selected as the complex enzyme 6, i.e., the mass ratio of the cellulase to the pectinase is 2: 3, and the result shows that the extraction rate of the complex enzyme polygonatum polysaccharide is the highest, which can reach 51.80%, which is 2.17 times that of the enzyme without adding. The best enzymolysis effect of the complex enzyme is shown, so the experiment determines that the complex enzyme is adopted to carry out enzymolysis treatment on the sealwort.
4.2.3 analysis of Single factor test results
4.2.3.1 influence of different ultrasonic time on extraction rate of rhizoma Polygonati polysaccharide
As shown in FIG. 11, the extraction time is prolonged, the extraction rate of polysaccharide is increased, and the extraction rate is increased rapidly when the time interval is 50-60 min. When the extraction time reaches 60min, the extraction rate of the polysaccharide reaches the maximum value of 65.52%, the extraction time is continuously prolonged, and the extraction rate shows a descending trend, so that the optimal ultrasonic time is selected to be 60 min.
4.2.3.2, influence of different enzymolysis time on the extraction rate of Polygonatum sibiricum polysaccharide
As shown in fig. 12, the enzymolysis time is prolonged, the polysaccharide extraction rate is continuously increased, and when the enzymolysis time is 30min, the polysaccharide extraction rate is the highest, which is 65.34%, and when the enzymolysis time is continuously prolonged, the extraction rate is reduced, and the reduction trend is obvious. Therefore, the optimal enzymolysis time is 30 min.
4.2.3.3, influence of different enzymolysis temperatures on the extraction rate of rhizoma Polygonati polysaccharide
As seen in FIG. 13, the enzyme hydrolysis temperature increased and the extraction rate increased. When the enzymolysis temperature is in the range of 30 ℃ to 50 ℃, the rising trend of the extraction rate is not obvious, when the enzymolysis temperature reaches 60 ℃, the extraction rate is obviously increased, the extraction rate of the polysaccharide reaches 61.68%, when the enzymolysis temperature reaches 70 ℃, the enzyme activity is possibly damaged, the reduction trend of the extraction rate is larger, and therefore, the optimal enzymolysis temperature is 60 ℃.
4.2.3.4, influence of different enzyme addition amounts on extraction rate of rhizoma Polygonati polysaccharide
As shown in FIG. 14, the enzyme dosage is 0.30% of the substrate, and the extraction rate of polysaccharide can reach 60.26%. When the enzyme dosage is increased, the extraction rate is in a descending trend, so that the optimal enzyme dosage is 0.30 percent.
4.2.4 analysis of orthogonal test results
TABLE 9 results of orthogonal experiments
In the case of a of 0.05, analysis of variance was performed with the enzymolysis temperature (C) as an error, as shown in Table 10.
TABLE 10 analysis of variance
Orthogonal test results and variance analysis in tables 9 and 10 show that the factor A, B has greater significance, A is greater than B, and the influence sequence of the factors on the extraction rate of the polygonatum polysaccharide is A greater than B greater than D greater than C, namely, the ultrasonic time is greater than the enzymolysis time, the enzyme adding amount is greater than the enzymolysis temperature. The optimum process combination resulting from the optimization of the orthogonal test is A 2 B 3 D 2 C 1 The optimum extraction process of rhizoma Polygonati polysaccharide comprises ultrasonic treatment for 60min, enzymolysis for 40min, enzyme addition of 0.30%, and enzymolysis temperature of 50 deg.C.
4.2.5, repeated verifiability test results
TABLE 11 repeated verifiability test results
The above scheme was subjected to three parallel validations, as per experimental scheme A 2 B 3 D 2 C 1 The mean value of the extraction rate of the polygonatum polysaccharide is 66.42%, which is higher than any group of results in an orthogonal test, the method saves solvent, has high extraction rate, and considers that the optimized extraction process has feasibility.
4.3 analysis of preparation Process results
Weighing 600g radix Puerariae powder, extracting according to the optimum process under item 4.1.3, concentrating to obtain extract with relative density of 1.10(60 deg.C), and spray drying at low temperature. And (3) taking a proper amount of extract, and drying in a vacuum drier with the pressure of-0.09 MPa and the temperature of 70 ℃, wherein the dry extract rate is calculated to be 31.5%.
Weighing 390g of rhizoma Polygonati powder, extracting according to the best process under the item of '4.2.4', concentrating into extract with relative density of 1.10(60 ℃), and spray drying at low temperature. Taking a proper amount of extract, and drying in a vacuum drier with vacuum degree of-0.09 MPa and temperature of 70 ℃, wherein the dry extract rate is 85.9%.
According to the regulation of pharmacopeia, the daily dosage of the kudzuvine root is 10-15 g, the daily dosage of the polygonatum is 9-15 g, and the daily dosage is equivalent to 10g of dried powder of kudzuvine root decoction pieces and polygonatum decoction pieces.
TABLE 12 comprehensive evaluation standard table for radix Puerariae and rhizoma Polygonati hypoglycemic chewable tablets
Remarking: the kudzu root extract is slightly bitter in taste, and the polygonatum sibiricum extract is bitter in taste if the drying temperature is too high and the drying time is too long, and is normally sweet.
Due to the addition of the xylan, white spots appear on the surface of the tablet, and the appearance is not attractive; dextrin has strong caking property and can cause pockmarks on the surface of the tablet. Thus, no xylan alcohol and dextrin were selected as bulking agents for this experiment.
TABLE 13 prescription optimization based on comprehensive evaluation (100 prescription amount)
As can be seen from Table 13, the overall evaluation of formula 4 was optimized to 96 points. The batch formulation can be carried out as described herein.
1g of kudzuvine root dry extract powder is equivalent to 3.17g of kudzuvine root decoction pieces, 1g of polygonatum sibiricum dry extract powder is equivalent to 1.16g of polygonatum sibiricum decoction pieces, therefore, 60g of kudzuvine root dry extract powder, 174g of polygonatum sibiricum dry extract powder, 267.6g of isomaltitol, 1.8g of aspartame, 6g of citric acid and 0.6g of peppermint oil are weighed, mixed evenly, granulated, dried and granulated, 0.3 percent of magnesium stearate of the weight of the granules is added as a lubricant, and 600 chewable tablets of 0.85g of each tablet are prepared, and the chewable tablets have good properties, appearance and mouthfeel.
4.4 analysis of quality evaluation results
4.4.1, appearance: the picture of the kudzuvine root and polygonatum sibiricum blood glucose reducing chewable tablet prepared in the embodiment 1 of the invention is shown in figure 15, and the kudzuvine root and polygonatum sibiricum blood glucose reducing chewable tablet is complete, smooth and uniform in color.
3.4.2, property: the product is light brown yellow tablet; fragrant and sweet.
3.4.3 hardness
TABLE 14 hardness
The hardness of the kudzuvine root and polygonatum sibiricum blood sugar reducing chewable tablets is proper and meets the specification.
4.4.4 results of friability test
Table 15 friability test results table
The weight loss is 0 calculated from table 15, no fracture, crack and crushed pieces appear, and the friability meets the requirements of Chinese pharmacopoeia.
4.4.5, weight Difference
TABLE 16 weight variation limits
The total weight of 20 tablets is 16.6000g, the average tablet weight is 0.8300g, the specified weight difference limit is +/-5 percent, namely the tablet weight range is 0.7885 g-0.8715 g, and tablets without exceeding the range are all in accordance with the specification.
4.4.6, microbial Limit: the microbial limit of the product meets the requirements according to the dish test of the microbial limit inspection method.
5. Conclusion
In the embodiment of the invention, the best extraction process conditions are obtained through a single-factor test and an orthogonal test, pueraria flavone and polygonatum polysaccharide are extracted to the maximum, and then different auxiliary materials are selected to prepare the pueraria polygonatum blood sugar-reducing chewable tablets. The kudzuvine root and polygonatum sibiricum blood sugar reducing chewable tablets prepared in each embodiment of the invention are light brown yellow tablets, fragrant and sweet in taste. The surface is bright, the mint oil has cool fragrance, the hardness and the friability meet the requirements, and the microbial limit meets the regulations, so the mint oil is an ideal health food for reducing blood sugar.
In the embodiment of the invention, kudzu root and rhizoma polygonati from Xinyang Dabieshan mountain are taken as raw materials, the kudzu flavone is extracted by adopting an ultrasonic method, the polygonatum polysaccharide is extracted by an enzyme synergistic ultrasonic method, the influence of different factors on the extraction rates of puerarin and polygonatum polysaccharide is respectively inspected through a single-factor test and an orthogonal test design, and the extraction process of the kudzu root and rhizoma polygonati sugar-reducing chewable tablet is optimized. The preparation method comprises the steps of carrying out amplification test, extracting active ingredients of the radix puerariae and the rhizoma polygonati in batches according to the optimized process conditions, concentrating the active ingredients into extract, respectively preparing the radix puerariae and the rhizoma polygonati extract into dry extract powder by adopting a proper drying mode, and developing the radix puerariae and rhizoma polygonati blood glucose reducing chewable tablet health-care product by taking the dry extract powder of the radix puerariae and the rhizoma polygonati as raw materials and adding proper auxiliary materials. The health product is convenient for administration and carrying, fully utilizes rich Chinese medicinal material resources of Xinyang Dabieshan mountain, has better taste and high solubility compared with common tablets, can reduce the burden of the medicament on gastrointestinal tract, is suitable for people of all ages, is especially suitable for patients with dysphagia to take, can take the medicament on time even in the absence of water, and is convenient for administration. The kudzu root and the rhizoma polygonati are special Chinese medicinal materials in Xinyang local areas and are medicinal and edible Chinese medicinal materials, and the chewable tablets are developed, so that the chewable tablets have a good food therapy effect, the additional value of the Chinese medicinal materials is improved, the Chinese medicinal material resources in the Xinyang Dabie mountain areas are fully utilized, and the local economic development is promoted.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for improving the content of active ingredients in radix puerariae and rhizoma polygonati hypoglycemic chewable tablets is characterized by comprising the following steps:
s1, mixing the kudzu vine root powder with an ethanol solution according to the material-liquid ratio of 1 g: 14-18 mL, then carrying out ultrasonic extraction, concentrating the filtrate into an extract, and drying to obtain a kudzu vine root extract;
s2, mixing the polygonatum sibiricum powder with water, and adding complex enzyme for enzymolysis;
s3, mixing the mixed solution obtained after the enzymolysis of the S2 with water, then carrying out ultrasonic extraction, concentrating the filtrate into an extract, and drying to obtain a sealwort extract;
s4, mixing the kudzu root extract and the rhizoma polygonati extract according to the mass ratio of 1: 2-3, adding auxiliary materials, and then preparing the chewable tablet by a wet granulation and tabletting method.
2. The method for improving the content of the active ingredients in the pueraria and polygonatum hypoglycemic chewable tablet according to claim 1, wherein in the step S1, the mass percentage concentration of the ethanol solution is 40-60%.
3. The method for improving the content of the active ingredients in the pueraria and polygonatum hypoglycemic chewable tablet according to claim 1, wherein in S1, the ultrasonic extraction conditions are as follows: the ultrasonic temperature is 50-60 ℃; the ultrasonic time is 30-50 min.
4. The method for improving the content of the effective ingredients in the radix puerariae and rhizoma polygonati sugar-reducing chewable tablets according to claim 1, wherein in S2, the mass ratio of rhizoma polygonati powder to water is 10 g: 20-40 mL.
5. The method for improving the content of the effective ingredients in the pueraria and polygonatum hypoglycemic chewable tablet according to claim 1, wherein in the step S2, the complex enzyme is cellulase and/or pectinase.
6. The method for improving the content of the effective ingredients in the pueraria and polygonatum hypoglycemic chewable tablet according to claim 5, wherein in the step S2, the complex enzyme is a mixture of cellulase and pectinase according to a mass ratio of 2: 2-4.
7. The method for improving the content of the effective ingredients in the pueraria and polygonatum hypoglycemic chewable tablet according to claim 1, wherein in the S2, the addition amount of the complex enzyme is 0.2-0.5% of the mass of the polygonatum powder.
8. The method for improving the content of the active ingredients in the pueraria and polygonatum hypoglycemic chewable tablet according to claim 1, wherein in S2, the conditions of enzymolysis are as follows: the pH value of enzymolysis is 6.5-6.8; the enzymolysis time is 20-40 min; the temperature of enzymolysis is 50-70 ℃.
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