CN112618662A - Traditional Chinese medicine formula for treating leg cramp - Google Patents
Traditional Chinese medicine formula for treating leg cramp Download PDFInfo
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Abstract
The invention discloses a traditional Chinese medicine formula for treating leg cramps, which comprises the following components in parts by weight: 20-25 parts of white paeony root, 3-5 parts of liquorice, 1-3 parts of Chinese starjasmine stem, 1-3 parts of suberect spatholobus stem, 3-5 parts of tripterygium wilfordii, 6-8 parts of lycopodium clavatum, 3-5 parts of szechuan lovage rhizome, 10-15 parts of Chinese angelica, 8-10 parts of cassia twig, 8-10 parts of doubleteeth pubescent angelica root, 10-15 parts of astragalus root and 8-10 parts of tall gastrodia tuber; the capsule liquid is prepared in the process of preparing the traditional Chinese medicine capsule, the capsule liquid has a good antibacterial effect, when mould contacts the surface of the capsule, the synthesis of mould nucleic acid is inhibited, so that the mould protein can not be normally synthesized, the permeability of a cell membrane is changed, the synthesis of cell walls is interfered, the storage time of traditional Chinese medicine particles is prolonged, meanwhile, after the epidermis of the capsule is dissolved, the cells absorb vitamin C and chitosan, a human body can well absorb medicinal components in the traditional Chinese medicine particles, and the treatment effect of the traditional Chinese medicine formula is quick and obvious.
Description
Technical Field
The invention relates to the technical field of medicine preparation, and particularly relates to a traditional Chinese medicine formula for treating leg cramps.
Background
The calf cramp is known as muscle spasm, a spontaneous tonic contraction of muscle. Muscle spasm occurring in the lower legs and toes is the most common, pain is difficult to endure during the attack, and especially, people are often waken up when cramping in the middle of the night, pain cannot be relieved for a long time, and sleep is affected. The pain of people caused by cramp of the lower leg cannot be formed by language. Particularly in winter, some people may awaken in the middle of the night due to cramping of the lower leg. The cramp of the lower leg is the sudden involuntary contraction phenomenon of the muscle, thereby causing the muscle stiffness and the severe pain brought by the muscle stiffness. The reasons for cramping the lower leg include high fever, epilepsy, tetanus, rabies, calcium deficiency, etc. However, in general, most of the reasons for cramping of the lower leg are that the muscles continuously contract too fast due to cold stimulation. When the calcium is seriously deficient, the cramp phenomenon of the lower leg frequently occurs as soon as the human body is subjected to cold stimulation, such as night in winter.
The medicine prepared by the traditional Chinese medicine formula for treating leg cramps has a good treatment effect, but the treatment course is long, and when the medicine is stored, the capsules on the surface are easy to generate mould so as to influence the normal eating of the medicine.
Disclosure of Invention
The invention aims to provide a traditional Chinese medicine formula for treating leg cramps.
The technical problems to be solved by the invention are as follows:
the medicine prepared by the traditional Chinese medicine formula for treating leg cramps has a good treatment effect, but the treatment course is long, and when the medicine is stored, the capsules on the surface are easy to generate mould so as to influence the normal eating of the medicine.
The purpose of the invention can be realized by the following technical scheme:
a traditional Chinese medicine formula for treating leg cramps comprises the following components in parts by weight: 20-25 parts of white paeony root, 3-5 parts of liquorice, 1-3 parts of Chinese starjasmine stem, 1-3 parts of suberect spatholobus stem, 3-5 parts of tripterygium wilfordii, 6-8 parts of lycopodium clavatum, 3-5 parts of szechuan lovage rhizome, 10-15 parts of Chinese angelica, 8-10 parts of cassia twig, 8-10 parts of doubleteeth pubescent angelica root, 10-15 parts of astragalus root and 8-10 parts of tall gastrodia tuber;
the traditional Chinese medicine for treating leg cramps is prepared by the following steps:
step S1: weighing the raw materials, cleaning and drying the raw materials, adding the raw materials into a pulverizer, pulverizing, and sieving with a 80-100 mesh sieve to obtain pulverized materials;
step S2: mixing the crushed materials prepared in the step S1, adding water with the mass 6-8 times of that of the crushed materials, refluxing for 3-5h at the temperature of 120-130 ℃, filtering to remove filter residues, concentrating the filtrate into paste, and drying to obtain traditional Chinese medicine extraction particles;
step S3: making the capsule liquid into a hard capsule shell, filling the traditional Chinese medicine extraction particles prepared in the step S2 into the hard capsule shell, and obtaining the traditional Chinese medicine capsule.
Further, the capsule liquid is prepared by the following steps:
step A1: adding chitosan and isopropanol into a reaction kettle, stirring for 10-15min under the condition that the rotation speed is 150 plus one year at 200r/min, adding a sodium hydroxide solution, stirring for 3-5min, adding chloroacetic acid, reacting for 2-3h at the temperature of 70-75 ℃, adding deionized water, adjusting the pH value of the reaction solution to 7 by using glacial acetic acid, filtering to remove filtrate, washing a filter cake by using ethanol, and drying to obtain carboxymethyl chitosan;
step A2: adding concentrated sulfuric acid into a reaction kettle, stirring and sequentially adding graphite, sodium nitrate and potassium permanganate at the rotation speed of 150-200r/min and the temperature of 1-3 ℃, reacting for 1.5-2h, heating to the temperature of 35-40 ℃, reacting for 20-30min, adding deionized water, heating to the temperature of 80-90 ℃, adding hydrogen peroxide, reacting for 15-20min to obtain graphene oxide, dispersing the graphene oxide and the carboxymethyl chitosan prepared in the step A1 into deionized water, adding hydroxypropyl cyclodextrin, and performing ultrasonic treatment for 1-1.5h under the frequency of 3-5MHz to obtain a mixed peptization solution;
step A3: adding 3-methyl-5-nitrobenzoic acid, methanol and hydrochloric acid into a reaction kettle, carrying out reflux reaction for 1-1.5h under the conditions of the rotating speed of 150-110 ℃ and the temperature of 105-110 ℃ to obtain an intermediate 1, dissolving the intermediate 1 in tetrahydrofuran, carrying out reaction for 1-1.5h with chlorine under the illumination condition to obtain an intermediate 2, adding the intermediate 2, potassium carbonate, deionized water and tetraethylammonium bromide into the reaction kettle, and carrying out reflux reaction for 1-1.5h under the conditions of the rotating speed of 150-200r/min and the temperature of 110-120 ℃ to obtain an intermediate 3;
the reaction process is as follows:
step A4: adding gallic acid into a reaction kettle, drying for 2-3h under the condition of temperature of 100-;
the reaction process is as follows:
step A5: adding the mixed peptization prepared in the step A2 and the intermediate 5 prepared in the step A4 into a grinding bowl, grinding for 5-10min, adding 1-hydroxybenzotriazole, continuously grinding for 1-1.5h, adding deionized water, stirring for 15-20min at the rotation speed of 200-.
Further, the dosage ratio of the chitosan, the isopropanol, the sodium hydroxide solution and the chloroacetic acid in the step A1 is 1g to 10mL to 5mL to 0.8g, and the mass fraction of the sodium hydroxide solution is 35%.
Further, the use amount ratio of the concentrated sulfuric acid, the graphite, the sodium nitrate, the potassium permanganate, the deionized water and the hydrogen peroxide in the step A2 is 20mL:1g:0.5g:3g:44mL:6mL, the mass fraction of the concentrated sulfuric acid is 95%, the mass fraction of the hydrogen peroxide is 30%, and the use amount ratio of the graphene oxide, the carboxymethyl chitosan and the hydroxypropyl cyclodextrin is 1:1: 30.
Further, in the step A3, the dosage ratio of the 3-methyl-5-nitrobenzoic acid, the methanol and the hydrochloric acid is 5g:20mL:2.3mL, the mass fraction of the hydrochloric acid is 10%, the dosage molar ratio of the intermediate 1 to the chlorine gas is 2:1, and the dosage ratio of the intermediate 2, the potassium carbonate, the deionized water and the tetraethylammonium bromide is 10g:9g:70mL:2 mL.
Further, the molar ratio of the gallic acid, the intermediate 3 and the concentrated sulfuric acid in the step A4 is 1:3:0.2, the mass fraction of the concentrated sulfuric acid is 98%, the ratio of the intermediate 4, the iron powder, the ethanol and the hydrochloric acid solution is 1g:0.9g:11mL:2mL, the volume fraction of the ethanol is 90%, and the hydrochloric acid solution is a concentrated hydrochloric acid with the mass fraction of 36% and ethanol with the volume fraction of 95% which are mixed in the volume ratio of 1: 9.
Further, the dosage ratio of the mixed peptization, the intermediate 5, the deionized water and the 1-hydroxybenzotriazole in the step A5 is 15mL:4g:50mL:1.8g, and the dosage ratio of the substrate, the magnesium stearate, the starch, the deionized water and the vitamin C is 10g:1.2g:3g:20mL:1.5 g.
The invention has the beneficial effects that: the invention prepares a capsule liquid in the process of preparing a traditional Chinese medicine for treating leg cramp, the capsule liquid takes chitosan as raw material, the chitosan is carried out carboxylation treatment to prepare carboxymethyl chitosan, graphene is oxidized to convert hydroxyl on the surface of the graphene into carboxyl to prepare graphene oxide, then the graphene oxide, the carboxymethyl chitosan and hydroxypropyl cyclodextrin are carried out ultrasonic treatment to ensure that hydroxyl on the hydroxypropyl cyclodextrin and carboxyl on the graphene oxide and the carboxymethyl chitosan form chemical bonds to prepare mixed peptization, then 3-methyl-5-nitrobenzoic acid and methanol are carried out esterification reaction under the action of hydrochloric acid to prepare an intermediate 1, the intermediate 1 and chlorine are carried out substitution reaction to prepare an intermediate 2, the intermediate 2 is further processed to prepare an intermediate 3, gallic acid and the intermediate 3 are reacted under the action of concentrated sulfuric acid, preparing an intermediate 4, reducing the intermediate 4 to convert nitro on the intermediate 4 into amino, preparing an intermediate 5, grinding the intermediate 5 and mixed sol, condensing the amino on the intermediate 5 with the rest carboxyl on graphene oxide and carboxymethyl chitosan under the action of 1-hydroxybenzotriazole, removing the excess 1-hydroxybenzotriazole to obtain a substrate, mixing the substrate, magnesium stearate, starch, deionized water and vitamin C to obtain a capsule solution, crushing and mixing the traditional Chinese medicine components to obtain a mixture, coating the mixture with the capsule solution to obtain the traditional Chinese medicine capsule for treating leg cramps, wherein the capsule solution has a good antibacterial effect, and when mould contacts the surface of the capsule, the synthesis of nucleic acid of the mould is inhibited, so that the normal synthesis of mould protein cannot be realized, and the permeability of cell membranes is changed, the synthesis of cell walls is interfered, so that the storage time of the traditional Chinese medicine particles is prolonged, and simultaneously, after the epidermis of the capsule is dissolved, the cells absorb vitamin C and chitosan, so that a human body can well absorb medicinal components in the traditional Chinese medicine particles, and the treatment effect of the traditional Chinese medicine formula is quick and obvious.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
Example 1
A traditional Chinese medicine formula for treating leg cramps comprises the following components in parts by weight: 20 parts of white paeony root, 3 parts of liquorice, 1 part of Chinese starjasmine stem, 1 part of suberect spatholobus stem, 3 parts of common threewingnut root, 6 parts of common clubmoss herb, 3 parts of szechuan lovage rhizome, 10 parts of Chinese angelica, 8 parts of cassia twig, 8 parts of doubleteeth pubescent angelica root, 10 parts of astragalus root and 8 parts of tall gastrodia tuber;
the traditional Chinese medicine for treating leg cramps is prepared by the following steps:
step S1: weighing the raw materials, cleaning and drying the raw materials, adding the raw materials into a pulverizer, pulverizing, and sieving with a 80-mesh sieve to obtain pulverized materials;
step S2: mixing the crushed materials prepared in the step S1, adding water with the mass 6 times of that of the crushed materials, refluxing for 3 hours at the temperature of 120 ℃, filtering to remove filter residues, concentrating the filtrate into paste, and drying to obtain traditional Chinese medicine extraction particles;
step S3: making the capsule liquid into a hard capsule shell, filling the traditional Chinese medicine extraction particles prepared in the step S2 into the hard capsule shell, and obtaining the traditional Chinese medicine capsule.
The capsule liquid is prepared by the following steps:
step A1: adding chitosan and isopropanol into a reaction kettle, stirring for 10min at the rotation speed of 150r/min, adding a sodium hydroxide solution, stirring for 3min, adding chloroacetic acid, reacting for 2h at the temperature of 70 ℃, adding deionized water, adjusting the pH value of the reaction solution to 7 with glacial acetic acid, filtering to remove filtrate, washing a filter cake with ethanol, and drying to obtain carboxymethyl chitosan;
step A2: adding concentrated sulfuric acid into a reaction kettle, stirring and sequentially adding graphite, sodium nitrate and potassium permanganate at the rotation speed of 150r/min and the temperature of 1 ℃, reacting for 1.5 hours, heating to 35 ℃, reacting for 20 minutes, adding deionized water, heating to 80 ℃, adding hydrogen peroxide, reacting for 15 minutes to obtain graphene oxide, dispersing the graphene oxide and the carboxymethyl chitosan prepared in the step A1 in the deionized water, adding hydroxypropyl cyclodextrin, and performing ultrasonic treatment for 1 hour under the frequency of 3-5MHz to obtain a mixed peptization solution;
step A3: adding 3-methyl-5-nitrobenzoic acid, methanol and hydrochloric acid into a reaction kettle, performing reflux reaction for 1h at the rotation speed of 150r/min and the temperature of 105 ℃ to obtain an intermediate 1, dissolving the intermediate 1 in tetrahydrofuran, performing reaction for 1h with chlorine under the illumination condition to obtain an intermediate 2, adding the intermediate 2, potassium carbonate, deionized water and tetraethylammonium bromide into the reaction kettle, and performing reflux reaction for 1h at the rotation speed of 150r/min and the temperature of 110 ℃ to obtain an intermediate 3;
step A4: adding gallic acid into a reaction kettle, drying for 2h at the temperature of 100 ℃, adding an intermediate 3, stirring for 5min at the rotation speed of 200r/min, adding concentrated sulfuric acid after the gallic acid is completely dissolved, performing reflux reaction for 3h at the temperature of 110 ℃, cooling to 80 ℃, distilling to remove ethanol to obtain an intermediate 4, adding the intermediate 4, iron powder and ethanol into the reaction kettle, performing reflux reaction for 3h at the temperature of 80 ℃, adding a hydrochloric acid solution, adding for 20min, continuing to react for 5h, and adjusting the pH value of the reaction solution to 7 to obtain an intermediate 5;
step A5: adding the mixed peptization prepared in the step A2 and the intermediate 5 prepared in the step A4 into a grinding bowl, grinding for 5min, adding 1-hydroxybenzotriazole, continuously grinding for 1h, adding deionized water, stirring for 15min at the rotation speed of 200r/min, filtering to remove the deionized water, preserving the temperature of a filter cake for 10min at 160 ℃, filtering to remove the 1-hydroxybenzotriazole again, adding the substrate, magnesium stearate, starch, deionized water, gelatin and vitamin C into a stirring kettle, and stirring for 1h at the rotation speed of 500-600r/min to prepare the capsule solution.
Example 2
A traditional Chinese medicine formula for treating leg cramps comprises the following components in parts by weight: 21 parts of white paeony root, 4 parts of liquorice, 2 parts of Chinese starjasmine stem, 2 parts of suberect spatholobus stem, 4 parts of common threewingnut root, 7 parts of common clubmoss herb, 4 parts of szechuan lovage rhizome, 12 parts of Chinese angelica, 9 parts of cassia twig, 9 parts of doubleteeth pubescent angelica root, 12 parts of astragalus root and 9 parts of tall gastrodia tuber;
the traditional Chinese medicine for treating leg cramps is prepared by the following steps:
step S1: weighing the raw materials, cleaning and drying the raw materials, adding the raw materials into a pulverizer, pulverizing, and sieving with a 80-mesh sieve to obtain pulverized materials;
step S2: mixing the crushed materials prepared in the step S1, adding water with the mass of 8 times of that of the crushed materials, refluxing for 5 hours at the temperature of 120 ℃, filtering to remove filter residues, concentrating the filtrate into paste, and drying to obtain traditional Chinese medicine extraction particles;
step S3: making the capsule liquid into a hard capsule shell, filling the traditional Chinese medicine extraction particles prepared in the step S2 into the hard capsule shell, and obtaining the traditional Chinese medicine capsule.
The capsule liquid is prepared by the following steps:
step A1: adding chitosan and isopropanol into a reaction kettle, stirring for 15min at the rotation speed of 150r/min, adding a sodium hydroxide solution, stirring for 3min, adding chloroacetic acid, reacting for 2h at the temperature of 75 ℃, adding deionized water, adjusting the pH value of the reaction solution to 7 with glacial acetic acid, filtering to remove filtrate, washing a filter cake with ethanol, and drying to obtain carboxymethyl chitosan;
step A2: adding concentrated sulfuric acid into a reaction kettle, stirring and sequentially adding graphite, sodium nitrate and potassium permanganate at the rotation speed of 200r/min and the temperature of 1 ℃, reacting for 2 hours, heating to 35 ℃, reacting for 30 minutes, adding deionized water, heating to 80 ℃, adding hydrogen peroxide, reacting for 20 minutes to obtain graphene oxide, dispersing the graphene oxide and the carboxymethyl chitosan prepared in the step A1 in the deionized water, adding hydroxypropyl cyclodextrin, and performing ultrasonic treatment for 1.5 hours at the frequency of 3MHz to obtain a mixed peptization solution;
step A3: adding 3-methyl-5-nitrobenzoic acid, methanol and hydrochloric acid into a reaction kettle, performing reflux reaction for 1h at the rotation speed of 150r/min and the temperature of 110 ℃ to obtain an intermediate 1, dissolving the intermediate 1 in tetrahydrofuran, performing reaction for 1.5h with chlorine under the illumination condition to obtain an intermediate 2, adding the intermediate 2, potassium carbonate, deionized water and tetraethylammonium bromide into the reaction kettle, and performing reflux reaction for 1h at the rotation speed of 150r/min and the temperature of 120 ℃ to obtain an intermediate 3;
step A4: adding gallic acid into a reaction kettle, drying for 2h at the temperature of 110 ℃, adding an intermediate 3, stirring for 5min at the rotation speed of 300r/min, adding concentrated sulfuric acid after the gallic acid is completely dissolved, performing reflux reaction for 3h at the temperature of 120 ℃, cooling to 80 ℃, distilling to remove ethanol to obtain an intermediate 4, adding the intermediate 4, iron powder and ethanol into the reaction kettle, performing reflux reaction for 3h at the temperature of 85 ℃, adding a hydrochloric acid solution, adding for 20min, continuing to react for 8h, and adjusting the pH value of the reaction solution to 7 to obtain an intermediate 5;
step A5: adding the mixed peptization prepared in the step A2 and the intermediate 5 prepared in the step A4 into a grinding bowl, grinding for 10min, adding 1-hydroxybenzotriazole, continuously grinding for 1h, adding deionized water, stirring for 15min at the rotation speed of 300r/min, filtering to remove the deionized water, preserving the temperature of a filter cake for 10min at the temperature of 170 ℃, filtering to remove the 1-hydroxybenzotriazole again, adding the substrate, magnesium stearate, starch, deionized water, gelatin and vitamin C into a stirring kettle, and stirring for 1h at the rotation speed of 600r/min to prepare the capsule solution.
Example 3
A traditional Chinese medicine formula for treating leg cramps comprises the following components in parts by weight: 23 parts of white paeony root, 4 parts of liquorice, 2 parts of Chinese starjasmine stem, 2 parts of suberect spatholobus stem, 4 parts of common threewingnut root, 7 parts of common clubmoss herb, 4 parts of szechuan lovage rhizome, 14 parts of Chinese angelica, 9 parts of cassia twig, 9 parts of doubleteeth pubescent angelica root, 14 parts of astragalus root and 9 parts of tall gastrodia tuber;
the traditional Chinese medicine for treating leg cramps is prepared by the following steps:
step S1: weighing the raw materials, cleaning and drying the raw materials, adding the raw materials into a pulverizer, pulverizing, and sieving with a 100-mesh sieve to obtain pulverized materials;
step S2: mixing the crushed materials prepared in the step S1, adding water with the mass 6 times of that of the crushed materials, refluxing for 3 hours at the temperature of 130 ℃, filtering to remove filter residues, concentrating the filtrate into paste, and drying to obtain traditional Chinese medicine extraction particles;
step S3: making the capsule liquid into a hard capsule shell, filling the traditional Chinese medicine extraction particles prepared in the step S2 into the hard capsule shell, and obtaining the traditional Chinese medicine capsule.
The capsule liquid is prepared by the following steps:
step A1: adding chitosan and isopropanol into a reaction kettle, stirring for 10min at the rotation speed of 200r/min, adding a sodium hydroxide solution, stirring for 5min, adding chloroacetic acid, reacting for 3h at the temperature of 70 ℃, adding deionized water, adjusting the pH value of the reaction solution to 7 with glacial acetic acid, filtering to remove filtrate, washing a filter cake with ethanol, and drying to obtain carboxymethyl chitosan;
step A2: adding concentrated sulfuric acid into a reaction kettle, stirring and sequentially adding graphite, sodium nitrate and potassium permanganate at the rotation speed of 150r/min and the temperature of 3 ℃, reacting for 1.5h, heating to 40 ℃, reacting for 20min, adding deionized water, heating to 90 ℃, adding hydrogen peroxide, reacting for 15min to obtain graphene oxide, dispersing the graphene oxide and the carboxymethyl chitosan prepared in the step A1 in the deionized water, adding hydroxypropyl cyclodextrin, and performing ultrasonic treatment for 1h at the frequency of 5MHz to obtain a mixed peptization solution;
step A3: adding 3-methyl-5-nitrobenzoic acid, methanol and hydrochloric acid into a reaction kettle, performing reflux reaction for 1.5h at the rotation speed of 200r/min and the temperature of 105 ℃ to obtain an intermediate 1, dissolving the intermediate 1 in tetrahydrofuran, performing reaction for 1h with chlorine under the illumination condition to obtain an intermediate 2, adding the intermediate 2, potassium carbonate, deionized water and tetraethylammonium bromide into the reaction kettle, and performing reflux reaction for 1.5h at the rotation speed of 200r/min and the temperature of 110 ℃ to obtain an intermediate 3;
step A4: adding gallic acid into a reaction kettle, drying for 3h at the temperature of 100 ℃, adding an intermediate 3, stirring for 10min at the rotation speed of 200r/min, adding concentrated sulfuric acid after the gallic acid is completely dissolved, performing reflux reaction for 5h at the temperature of 110 ℃, cooling to 80 ℃, distilling to remove ethanol to obtain an intermediate 4, adding the intermediate 4, iron powder and ethanol into the reaction kettle, performing reflux reaction for 5h at the temperature of 80 ℃, adding a hydrochloric acid solution for 20min, continuing to react for 5h, and adjusting the pH value of the reaction solution to 8 to obtain an intermediate 5;
step A5: adding the mixed peptization prepared in the step A2 and the intermediate 5 prepared in the step A4 into a grinding bowl, grinding for 5min, adding 1-hydroxybenzotriazole, continuously grinding for 1.5h, adding deionized water, stirring for 20min at the rotation speed of 200r/min, filtering to remove the deionized water, keeping the temperature of a filter cake at 160 ℃ for 15min, filtering to remove the 1-hydroxybenzotriazole again, adding the substrate, magnesium stearate, starch, deionized water, gelatin and vitamin C into a stirring kettle, and stirring for 1.5h at the rotation speed of 500r/min to prepare the capsule solution.
Example 4
A traditional Chinese medicine formula for treating leg cramps comprises the following components in parts by weight: 25 parts of white paeony root, 5 parts of liquorice, 3 parts of Chinese starjasmine stem, 3 parts of suberect spatholobus stem, 5 parts of common threewingnut root, 8 parts of common clubmoss herb, 5 parts of szechuan lovage rhizome, 15 parts of Chinese angelica, 10 parts of cassia twig, 10 parts of doubleteeth pubescent angelica root, 15 parts of astragalus root and 10 parts of tall gastrodia tuber;
the traditional Chinese medicine for treating leg cramps is prepared by the following steps:
step S1: weighing the raw materials, cleaning and drying the raw materials, adding the raw materials into a pulverizer, pulverizing, and sieving with a 100-mesh sieve to obtain pulverized materials;
step S2: mixing the crushed materials prepared in the step S1, adding water with the mass of 8 times of that of the crushed materials, refluxing for 5 hours at the temperature of 130 ℃, filtering to remove filter residues, concentrating the filtrate into paste, and drying to obtain traditional Chinese medicine extraction particles;
step S3: making the capsule liquid into a hard capsule shell, filling the traditional Chinese medicine extraction particles prepared in the step S2 into the hard capsule shell, and obtaining the traditional Chinese medicine capsule.
The capsule liquid is prepared by the following steps:
step A1: adding chitosan and isopropanol into a reaction kettle, stirring for 15min at the rotation speed of 200r/min, adding a sodium hydroxide solution, stirring for 5min, adding chloroacetic acid, reacting for 3h at the temperature of 75 ℃, adding deionized water, adjusting the pH value of the reaction solution to 7 with glacial acetic acid, filtering to remove filtrate, washing a filter cake with ethanol, and drying to obtain carboxymethyl chitosan;
step A2: adding concentrated sulfuric acid into a reaction kettle, stirring and sequentially adding graphite, sodium nitrate and potassium permanganate at the rotation speed of 200r/min and the temperature of 3 ℃, reacting for 2 hours, heating to 40 ℃, reacting for 30 minutes, adding deionized water, heating to 90 ℃, adding hydrogen peroxide, reacting for 20 minutes to obtain graphene oxide, dispersing the graphene oxide and the carboxymethyl chitosan prepared in the step A1 in the deionized water, adding hydroxypropyl cyclodextrin, and performing ultrasonic treatment for 1.5 hours at the frequency of 5MHz to obtain a mixed peptization solution;
step A3: adding 3-methyl-5-nitrobenzoic acid, methanol and hydrochloric acid into a reaction kettle, performing reflux reaction for 1.5h at the rotation speed of 200r/min and the temperature of 110 ℃ to obtain an intermediate 1, dissolving the intermediate 1 in tetrahydrofuran, performing reaction for 1.5h with chlorine under the illumination condition to obtain an intermediate 2, adding the intermediate 2, potassium carbonate, deionized water and tetraethylammonium bromide into the reaction kettle, and performing reflux reaction for 1.5h at the rotation speed of 200r/min and the temperature of 120 ℃ to obtain an intermediate 3;
step A4: adding gallic acid into a reaction kettle, drying for 3h at the temperature of 110 ℃, adding an intermediate 3, stirring for 10min at the rotation speed of 300r/min, adding concentrated sulfuric acid after the gallic acid is completely dissolved, performing reflux reaction for 5h at the temperature of 120 ℃, cooling to 80 ℃, distilling to remove ethanol to obtain an intermediate 4, adding the intermediate 4, iron powder and ethanol into the reaction kettle, performing reflux reaction for 5h at the temperature of 85 ℃, adding a hydrochloric acid solution, adding for 20min, continuing to react for 8h, and adjusting the pH value of the reaction solution to 8 to obtain an intermediate 5;
step A5: adding the mixed peptization prepared in the step A2 and the intermediate 5 prepared in the step A4 into a grinding bowl, grinding for 10min, adding 1-hydroxybenzotriazole, continuously grinding for 1.5h, adding deionized water, stirring for 20min at the rotation speed of 300r/min, filtering to remove the deionized water, keeping the temperature of a filter cake at 170 ℃ for 15min, filtering to remove the 1-hydroxybenzotriazole again, adding the substrate, magnesium stearate, starch, deionized water, gelatin and vitamin C into a stirring kettle, and stirring for 1.5h at the rotation speed of 600r/min to prepare the capsule solution.
Comparative example 1
The comparative example is a common traditional Chinese medicine formula for treating leg cramps in the market, and the formula is used for preparing traditional Chinese medicine capsules by using the capsule solution in the same manner as in example 1.
Comparative example 2
Compared with the comparative example 2, the traditional Chinese medicine capsule prepared by using the common gelatin capsule shell is adopted in the comparative example.
The traditional Chinese medicine capsules prepared in examples 1-4 and comparative examples 1-2 were tested for therapeutic effect, and 120 patients with leg cramps, 60 patients for male and female, were evenly divided into 6 groups, and taken twice in the morning and evening in the tomorrow, and the therapeutic effect was observed;
TABLE 1
As can be seen from table 1 above, the cure rate of the traditional Chinese medicine capsules prepared in examples 1 to 4 is 20 to 30% when the patient takes the capsules for 5 days, 70 to 80% when the patient takes the capsules for 10 days, and 100% when the capsules for 15 days, the cure rate of the traditional Chinese medicine capsules prepared in comparative example 1 is 10% when the patient takes the capsules for 5 days, 50% when the capsules for 10 days, 80% when the capsules for 15 days, and 100% when the capsules for 20 days, the cure rate of the traditional Chinese medicine capsules prepared in comparative example 2 is 0% when the patient takes the capsules for 5 days, 20% when the capsules for 10 days, 60% when the capsules for 15 days, and 95% when the capsules for 20 days.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (7)
1. A traditional Chinese medicine formula for treating leg cramps is characterized in that: comprises the following components in parts by weight: 20-25 parts of white paeony root, 3-5 parts of liquorice, 1-3 parts of Chinese starjasmine stem, 1-3 parts of suberect spatholobus stem, 3-5 parts of tripterygium wilfordii, 6-8 parts of lycopodium clavatum, 3-5 parts of szechuan lovage rhizome, 10-15 parts of Chinese angelica, 8-10 parts of cassia twig, 8-10 parts of doubleteeth pubescent angelica root, 10-15 parts of astragalus root and 8-10 parts of tall gastrodia tuber;
the traditional Chinese medicine for treating leg cramps is prepared by the following steps:
step S1: weighing the raw materials, cleaning and drying the raw materials, adding the raw materials into a pulverizer, pulverizing, and sieving with a 80-100 mesh sieve to obtain pulverized materials;
step S2: mixing the crushed materials prepared in the step S1, adding water with the mass 6-8 times of that of the crushed materials, refluxing for 3-5h at the temperature of 120-130 ℃, filtering to remove filter residues, concentrating the filtrate into paste, and drying to obtain traditional Chinese medicine extraction particles;
step S3: making the capsule liquid into a hard capsule shell, filling the traditional Chinese medicine extraction particles prepared in the step S2 into the hard capsule shell, and obtaining the traditional Chinese medicine capsule.
2. The traditional Chinese medicine formula for treating leg cramps according to claim 1, wherein: the capsule liquid is prepared by the following steps:
step A1: adding chitosan and isopropanol into a reaction kettle, stirring for 10-15min under the condition that the rotation speed is 150 plus one year at 200r/min, adding a sodium hydroxide solution, stirring for 3-5min, adding chloroacetic acid, reacting for 2-3h at the temperature of 70-75 ℃, adding deionized water, adjusting the pH value of the reaction solution to 7 by using glacial acetic acid, filtering to remove filtrate, washing a filter cake by using ethanol, and drying to obtain carboxymethyl chitosan;
step A2: adding concentrated sulfuric acid into a reaction kettle, stirring and sequentially adding graphite, sodium nitrate and potassium permanganate at the rotation speed of 150-200r/min and the temperature of 1-3 ℃, reacting for 1.5-2h, heating to the temperature of 35-40 ℃, reacting for 20-30min, adding deionized water, heating to the temperature of 80-90 ℃, adding hydrogen peroxide, reacting for 15-20min to obtain graphene oxide, dispersing the graphene oxide and the carboxymethyl chitosan prepared in the step A1 into deionized water, adding hydroxypropyl cyclodextrin, and performing ultrasonic treatment for 1-1.5h under the frequency of 3-5MHz to obtain a mixed peptization solution;
step A3: adding 3-methyl-5-nitrobenzoic acid, methanol and hydrochloric acid into a reaction kettle, carrying out reflux reaction for 1-1.5h under the conditions of the rotating speed of 150-110 ℃ and the temperature of 105-110 ℃ to obtain an intermediate 1, dissolving the intermediate 1 in tetrahydrofuran, carrying out reaction for 1-1.5h with chlorine under the illumination condition to obtain an intermediate 2, adding the intermediate 2, potassium carbonate, deionized water and tetraethylammonium bromide into the reaction kettle, and carrying out reflux reaction for 1-1.5h under the conditions of the rotating speed of 150-200r/min and the temperature of 110-120 ℃ to obtain an intermediate 3;
step A4: adding gallic acid into a reaction kettle, drying for 2-3h under the condition of temperature of 100-;
step A5: adding the mixed peptization prepared in the step A2 and the intermediate 5 prepared in the step A4 into a grinding bowl, grinding for 5-10min, adding 1-hydroxybenzotriazole, continuously grinding for 1-1.5h, adding deionized water, stirring for 15-20min at the rotation speed of 200-.
3. The traditional Chinese medicine formula for treating leg cramps according to claim 2, which is characterized in that: the dosage ratio of the chitosan, the isopropanol, the sodium hydroxide solution and the chloroacetic acid in the step A1 is 1g to 10mL to 5mL to 0.8g, and the mass fraction of the sodium hydroxide solution is 35%.
4. The traditional Chinese medicine formula for treating leg cramps according to claim 2, which is characterized in that: the dosage ratio of the concentrated sulfuric acid, the graphite, the sodium nitrate, the potassium permanganate, the deionized water and the hydrogen peroxide in the step A2 is 20mL:1g:0.5g:3g:44mL:6mL, the mass fraction of the concentrated sulfuric acid is 95%, the mass fraction of the hydrogen peroxide is 30%, and the dosage mass ratio of the graphene oxide, the carboxymethyl chitosan and the hydroxypropyl cyclodextrin is 1:1: 30.
5. The traditional Chinese medicine formula for treating leg cramps according to claim 2, which is characterized in that: the dosage ratio of the 3-methyl-5-nitrobenzoic acid, the methanol and the hydrochloric acid in the step A3 is 5g:20mL:2.3mL, the mass fraction of the hydrochloric acid is 10%, the dosage molar ratio of the intermediate 1 to the chlorine gas is 2:1, and the dosage ratio of the intermediate 2, the potassium carbonate, the deionized water and the tetraethylammonium bromide is 10g:9g:70mL:2 mL.
6. The traditional Chinese medicine formula for treating leg cramps according to claim 2, which is characterized in that: the molar ratio of the gallic acid to the intermediate 3 to the concentrated sulfuric acid in the step A4 is 1:3:0.2, the mass fraction of the concentrated sulfuric acid is 98%, the ratio of the intermediate 4 to the iron powder to the ethanol to the hydrochloric acid solution is 1g:0.9g:11mL:2mL, the volume fraction of the ethanol is 90%, and the hydrochloric acid solution is a concentrated hydrochloric acid with the mass fraction of 36% and ethanol with the volume fraction of 95% which are mixed according to the volume ratio of 1: 9.
7. The traditional Chinese medicine formula for treating leg cramps according to claim 2, which is characterized in that: the dosage ratio of the mixed peptization, the intermediate 5, the deionized water and the 1-hydroxybenzotriazole in the step A5 is 15mL to 4g to 50mL to 1.8g, and the dosage ratio of the substrate, the magnesium stearate, the starch, the deionized water and the vitamin C is 10g to 1.2g to 3g to 20mL to 1.5 g.
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