CN113181123A - Anmian granules and preparation method thereof - Google Patents

Anmian granules and preparation method thereof Download PDF

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CN113181123A
CN113181123A CN202110518981.9A CN202110518981A CN113181123A CN 113181123 A CN113181123 A CN 113181123A CN 202110518981 A CN202110518981 A CN 202110518981A CN 113181123 A CN113181123 A CN 113181123A
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parts
solution
methanol
insomnia
granule
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王平
陈林霖
谢光璟
徐波
夏婧
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Hubei College of Chinese Medicine
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    • A61K9/00Medicinal preparations characterised by special physical form
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Abstract

The invention belongs to the technical field of traditional Chinese medicines, and discloses a insomnia granule and a preparation method thereof, wherein the insomnia granule is composed of 6-12 parts of ginseng, 4-8 parts of salvia miltiorrhiza, 6-12 parts of radix ophiopogonis, 2-4 parts of liquorice, 6-12 parts of poria with hostwood, 10-20 parts of raw jujube kernel, 10-20 parts of cooked jujube kernel, 2-4 parts of rhizoma acori graminei, 6-12 parts of angelica and 2-4 parts of schisandra chinensis according to parts by mass. The preparation method of the Anmian granules comprises the following steps: decocting Ginseng radix, Saviae Miltiorrhizae radix, radix Ophiopogonis, Glycyrrhrizae radix, Poria, semen Ziziphi Spinosae, cooked semen Ziziphi Spinosae, rhizoma Acori Graminei, radix Angelicae sinensis, and fructus Schisandrae with 10 times of water for 3 times; filtering, and mixing decoctions; standing for 12-16 hours, and concentrating to a proper amount; spray drying to obtain dry extract powder, adding maltodextrin and appropriate amount of aspartame equal to the dry extract powder, mixing, granulating with water spray, and drying. Scientific experiments prove that the granules have the traditional effect of the insomnia pill and stable and controllable quality.

Description

Anmian granules and preparation method thereof
Technical Field
The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to an insomnia granule and a preparation method thereof.
Background
With the acceleration of the pace of social life, the incidence of insomnia is on a rising trend. The patient has certain curative effect by using the sedative, but has large side effect after long-term use, and is easy to generate dependence and addiction. In recent years, the traditional Chinese medicine therapy is widely applied to the clinical treatment of insomnia due to the advantages of unique safety, effectiveness, no toxic or side effect and the like. Insomnia, called as insomnia in traditional Chinese medicine, is mainly caused by deficiency of heart and spleen, heart and blood deficiency, and heart and blood deficiency failing to nourish the heart, and mainly manifested as insomnia, dreaminess, fatigue, hypodynamia, and the like. Anmian Dan is from first volume of Shi Ju Mi Lu edited by famous physicians' Chen Shi ze Tou in Qing Dynasty, and is prepared from Ginseng radix, Saviae Miltiorrhizae radix, radix Ophiopogonis, Glycyrrhrizae radix, Poria, semen Ziziphi Spinosae, cooked semen Ziziphi Spinosae, rhizoma Acori Graminei, radix Angelicae sinensis, and fructus Schisandrae, and can be used for treating severe palpitation insomnia due to heart blood deficiency. The formula uses ginseng to benefit heart qi, salvia miltiorrhiza and angelica to supplement heart blood, ophiopogon root to nourish heart yin, calamus to open heart, poria with hostwood, jujube kernel and liquorice to supplement heart spirit, and schisandra chinensis to astringe heart qi. The medicines are combined to play the effects of tonifying qi, nourishing heart and soothing nerves. In the recipe, raw and cooked jujube kernels are used for five money, respectively, and heart-tonifying herbs are used as adjuvant drugs. The jujube kernel is a holy drug for relieving insomnia, and can be used for preventing people from lying down in the daytime when being used unprocessed, preventing people from waking up at night when being used cooked, and determining palpitation when being stable day and night. However, the traditional administration mode of the prescription is decoction, and the traditional administration mode is only applied in folks or is clinically used as a temporary preparation in hospitals in traditional Chinese medicine, so the clinical application of the Anmian Dan is limited due to the inconvenient administration and uncontrollable quality of the original prescription. Aiming at the problems, the invention adopts the modern preparation process, retains the traditional method of water decoction, takes maltodextrin as an auxiliary material, mixes with soft materials, granulates, and adds a proper amount of aspartame as a flavoring agent to improve the medicine taste. The invention aims to provide a novel preparation process of the insomnia granule, which is convenient to take, stable in curative effect and high in patient compliance; the invention also aims to provide a quality detection method of the insomnia granules.
Through the above analysis, the problems and defects of the prior art are as follows: the effect of the chemical medicine for treating insomnia is quick, but the treatment is temporary and permanent, and the long-term administration can generate drug resistance and dependence with more side effects. The traditional Chinese medicine prescription is used for treating pathogenesis, treats both principal and secondary aspects of diseases, has small side effect and has unique advantages which are incomparable with western medicine. The traditional formulation of Annaodan as a classic prescription for treating insomnia has the defects of decoction before use, large dose, poor taste and difficult storage and transportation, so that the Annaodan is limited to be widely used, and the clinical curative effect is influenced because the medicinal components and quality are unstable due to the difference of the quality of medicinal materials and the prescription, so that a simple, convenient and reliable quality control method is urgently needed.
The difficulty in solving the above problems and defects is: in order to ensure that the effective components of the new preparation form of the Anmian Dan are close to the original formula, simultaneously reduce the dosage, improve the taking convenience and consider the pharmaceutical cost, the proper preparation form needs to be selected and the extraction process needs to be investigated and optimized. The medicinal materials contain more sugar and saponin, the paste yield is high, the moisture absorption is strong, and the adopted drying and granulating forming modes and the types and the addition amounts of auxiliary materials need to be considered. In order to improve the taste of the medicine and simultaneously not increase the blood sugar, a non-caloric sweetener is required. In order to ensure the quality consistency of the preparation in different raw materials, manufacturers and production batches, a simple and effective quality control method is necessary to be established.
The significance of solving the problems and the defects is as follows: the traditional Chinese medicine preparation is prepared into granules by combining laboratory pilot test, factory pilot test and mass production of the inventor with clinical requirements and improving the traditional process of the classic famous prescription Anmian Dan, the granules have good particle size, uniform color and luster, good dissolubility, controllable quality, good curative effect, simple process, convenient taking and good taste compared with the original prescription, and the Aspartame replaces cane sugar or honey, so that the medicine for patients with diabetes is satisfied, and the preparation has good stability and easy storage.
Disclosure of Invention
The invention aims to provide an insomnia granule and a preparation method thereof.
The medicine granule for relieving insomnia is prepared from 6-12 parts of ginseng, 4-8 parts of salvia miltiorrhiza, 6-12 parts of radix ophiopogonis, 2-4 parts of liquorice, 6-12 parts of poria with hostwood, 10-20 parts of raw date kernel, 10-20 parts of cooked date kernel, 2-4 parts of rhizoma acori graminei, 6-12 parts of angelica sinensis and 2-4 parts of schisandra chinensis in parts by mass.
The invention also aims to provide a preparation method of the insomnia granule, which comprises the following steps: extracting Ginseng radix, Saviae Miltiorrhizae radix, radix Ophiopogonis, Glycyrrhrizae radix, Poria, semen Ziziphi Spinosae, cooked semen Ziziphi Spinosae, rhizoma Acori Graminei, radix Angelicae sinensis, and fructus Schisandrae with hot water, concentrating, drying, adding maltodextrin, and granulating.
Further, the preparation method of the insomnia granule also comprises the following steps:
step one, adding 10 times of water into ginseng, salvia miltiorrhiza, radix ophiopogonis, liquorice, poria with hostwood, raw date kernels, cooked date kernels, rhizoma acori graminei, angelica sinensis and schisandra chinensis for decocting for 3 times each time; filtering, and mixing decoctions;
step two, standing for 12-16 hours and then concentrating to a proper amount; spray drying to obtain dry extract powder, adding adjuvants such as maltodextrin and aspartame, spray granulating with appropriate amount of water, and drying.
Further, in step one, the decocting comprises: decocting for 2 hr each time.
The invention also aims to provide an identification method of the insomnia granule, which comprises the following steps:
(1) grinding 4g of the prepared Anmian granule, adding 30ml of methanol, heating and refluxing for 1 hour, filtering, evaporating the filtrate, and dissolving the residue in 1ml of methanol to obtain a sample solution;
(2) taking 1g of spina date seed reference medicinal material, adding 30ml of petroleum ether (60-90 ℃), heating and refluxing for 2 hours, filtering, removing petroleum ether liquid, volatilizing medicinal residues, adding 30ml of methanol, heating and refluxing for 1 hour, filtering, evaporating filtrate to dryness, and adding 1ml of methanol to dissolve residues to obtain a reference medicinal material solution;
(3) taking semen Ziziphi Spinosae saponin A, B reference substance, adding methanol to make into solutions each containing 1mg per 1ml as reference substance solution;
(4) sucking 5 μ l of prepared test solution, 10 μ l of control solution and 5 μ l of control solution, respectively dropping on the same silica gel G thin layer plate, developing with water saturated n-butanol as developing agent, taking out, air drying, and spraying 1% vanillin sulfuric acid solution;
(5) respectively placing under sunlight and ultraviolet lamp 365nm to inspect whether spots or fluorescent spots with the same color appear on the chromatogram of the test sample at the positions corresponding to the chromatograms of the reference sample and the reference medicinal material.
The invention also aims to provide an identification method of the insomnia granule, which comprises the following steps:
1) grinding 4g of the prepared Anmian granules, adding 30ml of trichloromethane, heating and refluxing for 2 hours, removing the trichloromethane liquid, volatilizing the solvent from the residue, adding 20ml of water-saturated n-butyl alcohol, carrying out ultrasonic treatment for 30 minutes, and filtering;
2) adding 5 times of ammonia test solution into the filtrate, shaking, standing for layering, collecting supernatant, evaporating to dry, and dissolving the residue with 2ml of methanol to obtain test solution;
3) preparing 1g of ginseng reference medicinal material into a reference medicinal material solution by the same method; collecting ginsenoside Rb1Ginsenoside Re, ginsenoside Rf, and ginsenoside Rg1Adding methanol to obtain solutions each containing 1mg per 1ml as reference solution;
4) sucking 10 μ l of test solution, 5 μ l of control solution and 5 μ l of control solution, respectively dropping on the same silica gel G thin layer plate, developing with lower layer solution of chloroform, methanol and water at 10 deg.C below overnight as developing agent, taking out, and air drying;
5) spraying 10% sulphuric acid ethanol solution, heating at 105 deg.C until the spots are clearly developed, and respectively placing in sunlight and ultraviolet lamp 365nm to check whether spots or fluorescent spots with the same color appear on the corresponding positions of the reference medicinal material and the reference substance in the chromatogram of the test solution.
Further, the mixing ratio of the trichloromethane to the methanol to the water is 13:6: 2.
The invention also aims to provide a content determination method of the insomnia granules, which comprises the following steps:
octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile is taken as a mobile phase A, and water is taken as a mobile phase B; eluting according to gradient; the detection wavelength is 335 nm; the flow rate is 1.0 ml/min; the temperature is 25 ℃; taking a proper amount of the spinosad reference substance, precisely weighing, and adding methanol to prepare a solution containing 50 mu g of the spinosad per 1ml, thus obtaining a reference substance solution; taking a proper amount of sample, grinding, taking about 2g, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of 75% methanol, sealing the plug, weighing, carrying out ultrasonic treatment for 30 minutes, cooling, weighing again, supplementing the lost weight with 75% methanol, shaking up, filtering, and taking a subsequent filtrate to obtain a sample solution; precisely sucking 5 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
Further, the ultrasonic treatment comprises: ultrasonic power 500W, frequency 40 kHz.
By combining all the technical schemes, the invention has the advantages and positive effects that: scientific experiments prove that the granules have the traditional efficacy of the insomnia pill and stable and controllable quality. The invention discloses a content determination and identification method of insomnia granules.
Technical effect or experimental effect of comparison.
Pharmacodynamic experiments of the invention:
pharmacodynamic experiments of the sedative effect of the insomnia granules prepared by the process of the invention prove that the insomnia granules have the same efficacy as the traditional decoction.
Reagent: the invention provides the sleep-improving granule (prepared by the method of example 1) and the sleep-improving pill decoction, which are provided by Lishizhen pharmaceutical group Limited company, and the granule is prepared into uniform suspension with required concentration by grinding with 0.5 percent CMC-Na before use.
And (3) spontaneous activity detection: SD rats are divided into a control group, a model group, a treatment group (a group with low and high-dose Anmian granules and Anmian Dan group) and a positive drug group (melatonin), the model group is injected into the abdominal cavity of the rat to carry out model building, and the treatment group is continuously administrated for 1 week. Monitoring with Ethovision video analysis system, keeping the ambient environment quiet during the experiment, placing each group of rats into a movable test box, and detecting the rats at 2mThe behavioral indexes in include moving distance, moving speed, moving time and the like. The administration dosage of Anmiandan (decoction) is 4.55 g/kg based on crude drug amount-1·d-1The administration dosage of the low-dose and high-dose groups of the Anmian granules is respectively 4.55 g.kg-1·d-1And 18.18 g.kg-1·d-1
The results show (see table 1) that the mean moving distance of the rats in the model group is prolonged and the mean moving speed is increased (P < 0.01) compared with the control group, and the moving distance of the rats is shortened and the moving speed is reduced (P < 0.01) after the intervention of the high-dose group of the insomnia granules compared with the model group. However, the low dose group of Anmo particles showed no statistical difference in distance traveled and mean velocity compared to the model group (P > 0.05). Meanwhile, compared with the Anmiandan group, the high dose of the Anmiandan granules further reduces the moving distance and the moving speed of the rats (P is less than 0.05), but the low dose group has no statistical difference (P is more than 0.05) compared with the Anmiandan group. The cumulative time of movement of the rats in each group was further counted, and the results showed that the cumulative time of movement of the rats in the model group was prolonged (P < 0.01) compared with that in the control group. Compared with the model group, the low-insomnia granule and high-dose group can obviously shorten the movement accumulated time of rats (P is less than 0.01). Meanwhile, compared with the somnan group, the somnan granule low dose group has no statistical difference (P is more than 0.05).
TABLE 1 comparison of distance, speed and time of locomotion for voluntary activities between groups
Figure BDA0003063146350000051
Figure BDA0003063146350000052
Figure BDA0003063146350000061
Note: compared with the control group, the compound of the formula,*P<0.05,**p is less than 0.01; in comparison with the set of models,#P<0.05,##p is less than 0.01. Compared with the group of Anmiandan, the ^ P is less than 0.05,^^P<0.01。
drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained from the drawings without creative efforts.
Fig. 1 is a flow chart of a method for preparing an insomnia granule provided by an embodiment of the present invention.
Fig. 2 is a flowchart of an identification method for insomnia granules provided in the embodiment of the present invention.
Fig. 3 is a flowchart of an identification method for insomnia granules according to an embodiment of the present invention.
FIG. 4 is a flow chart of a content determination method provided by an embodiment 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 further described in detail with reference to the following 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.
Aiming at the problems in the prior art, the invention provides an insomnia granule and a preparation method thereof, and the invention is described in detail with reference to the accompanying drawings.
The insomnia particle provided by the embodiment of the invention is composed of 6-12 parts of ginseng, 4-8 parts of salvia miltiorrhiza, 6-12 parts of radix ophiopogonis, 2-4 parts of liquorice, 6-12 parts of poria with hostwood, 10-20 parts of raw date kernel, 10-20 parts of cooked date kernel, 2-4 parts of rhizoma acori graminei, 6-12 parts of angelica and 2-4 parts of schisandra chinensis according to parts by mass.
As shown in fig. 1, the preparation method of the insomnia granule provided by the embodiment of the present invention includes the following steps:
s101, adding 10 times of water into 9 parts of ginseng, 6 parts of salvia miltiorrhiza, 9 parts of radix ophiopogonis, 3 parts of liquorice, 9 parts of poria with hostwood, 15 parts of raw jujube kernel, 15 parts of cooked jujube kernel, 3 parts of rhizoma acori graminei, 9 parts of angelica and 3 parts of schisandra chinensis for decocting for 3 times, and each time lasts for 2 hours; filtering, and mixing decoctions;
s102, standing for 12 hours, and concentrating to a proper amount (the specific gravity is 1.10-1.20); spray drying to obtain dry extract powder, adding maltodextrin and 2 ‰ aspartame equal in amount to the dry extract powder, mixing, spray granulating with appropriate amount of water as wetting agent, drying at 60-80 deg.C until water content is 3.3%, and sieving with vibration sieve (upper layer of 12 mesh and lower layer of 50 mesh).
As shown in fig. 2, the method for identifying insomnia particles provided in the embodiment of the present invention includes:
s201, taking 4g of prepared insomnia granules, grinding, adding 30ml of methanol, heating and refluxing for 1 hour, filtering, evaporating filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain a test solution;
s202, taking 1g of spina date seed reference medicinal material, adding 30ml of petroleum ether (60-90 ℃), heating and refluxing for 2 hours, filtering, removing petroleum ether liquid, volatilizing dregs, adding 30ml of methanol, heating and refluxing for 1 hour, filtering, evaporating filtrate to dryness, and adding 1ml of methanol to dissolve residues to obtain a reference medicinal material solution;
s203, adding methanol into a spina date seed saponin A, B reference substance to prepare solutions containing 1mg of each 1ml of the spina date seed saponin as reference substance solutions;
s204, sucking 5 mul of the prepared test solution, 10 mul of the prepared reference medicinal material solution and 5 mul of the prepared reference solution, respectively dropping the solutions on the same silica gel G thin layer plate, developing by using water-saturated n-butanol as a developing agent, taking out, airing, and spraying 1% vanillin sulfuric acid solution;
s205, respectively placing the sample in the sunlight and the ultraviolet lamp under 365nm to check whether spots or fluorescent spots with the same color appear on the corresponding positions of the reference substance and the reference medicine in the chromatogram of the sample.
As shown in fig. 3, the method for identifying insomnia granules provided in the embodiment of the present invention includes:
s301, taking 4g of prepared insomnia granules, grinding, adding 30ml of trichloromethane, heating and refluxing for 2 hours, discarding trichloromethane liquid, volatilizing solvent from medicine residues, adding 20ml of water-saturated n-butyl alcohol, carrying out ultrasonic treatment for 30 minutes, and filtering;
s302, adding 5 times of ammonia test solution into the filtrate, shaking uniformly, standing for layering, taking the supernatant, evaporating to dryness, and dissolving the residue in 2ml of methanol to obtain a test solution;
s303, preparing 1g of a ginseng reference medicinal material, and preparing a reference medicinal material solution in the same way; collecting ginsenoside Rb1Ginsenoside Re, ginsenoside Rf, and ginsenoside Rg1Adding methanol to obtain solutions each containing 1mg per 1ml as reference solution;
s304, sucking 10 mul of a test solution, 5 mul of a reference medicinal material solution and 5 mul of a reference solution, respectively dropping the solutions on the same silica gel G thin-layer plate, taking a lower-layer solution which is a mixture of chloroform, methanol and water and is placed overnight at a temperature of below 10 ℃ as a developing agent, developing, taking out and airing;
s305, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color of the spots is clear, and respectively placing the spots under the conditions of sunlight and 365nm ultraviolet lamps to check whether the spots or fluorescent spots with the same color appear on the positions, corresponding to the color spectrums of the reference medicinal material and the reference substance, in the color spectrum of the test sample.
The mixing ratio of the trichloromethane, the methanol and the water provided by the embodiment of the invention is 13:6: 2.
The content determination method of the insomnia granules provided by the embodiment of the invention comprises the following steps:
s401, using octadecylsilane chemically bonded silica as a filler; acetonitrile is taken as a mobile phase A, and water is taken as a mobile phase B; eluting according to gradient; the detection wavelength is 335 nm; the flow rate is 1.0 ml/min; the temperature is 25 ℃; taking a proper amount of the spinosad reference substance, precisely weighing, and adding methanol to prepare a solution containing 50 mu g of the spinosad per 1ml, thus obtaining a reference substance solution;
s402, taking a proper amount of samples, grinding, taking about 2g, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of 75% methanol, sealing the plug, weighing, ultrasonically treating for 30 minutes, and cooling;
s403, weighing, supplementing the lost weight with 75% methanol, shaking up, filtering, and taking the subsequent filtrate to obtain a test solution;
s404, precisely sucking 5 mu l of each of the reference solution and the test solution, injecting the reference solution and the test solution into a liquid chromatograph, and measuring to obtain the test solution.
The ultrasonic treatment provided by the embodiment of the invention comprises the following steps: ultrasonic power 500W, frequency 40 kHz.
The technical effects of the present invention will be further described with reference to specific embodiments.
Example 1
The insomnia granule provided by the embodiment of the invention is composed of 9 parts of ginseng, 6 parts of salvia miltiorrhiza, 9 parts of radix ophiopogonis, 3 parts of liquorice, 9 parts of poria with hostwood, 15 parts of raw date kernel, 15 parts of cooked date kernel, 3 parts of rhizoma acori graminei, 9 parts of angelica and 3 parts of schisandra chinensis in parts by mass.
Example 2
The insomnia granule provided by the embodiment of the invention is composed of 6 parts of ginseng, 4 parts of salvia miltiorrhiza, 6 parts of radix ophiopogonis, 2 parts of liquorice, 6 parts of poria with hostwood, 10 parts of raw date kernel, 10 parts of cooked date kernel, 2 parts of rhizoma acori graminei, 6 parts of angelica and 2 parts of schisandra chinensis in parts by mass.
Example 3
The insomnia granule provided by the embodiment of the invention is composed of 12 parts of ginseng, 8 parts of salvia miltiorrhiza, 12 parts of radix ophiopogonis, 4 parts of liquorice, 12 parts of poria with hostwood, 20 parts of raw date kernel, 20 parts of cooked date kernel, 4 parts of rhizoma acori graminei, 12 parts of angelica and 4 parts of schisandra chinensis in parts by mass.
Example 4
A quality detection method of Anmian granules comprises the following steps:
and (3) identification: grinding 4g of the product, adding 30ml of methanol, heating and refluxing for 1 hour, filtering, evaporating the filtrate to dryness, and dissolving the residue in 1ml of methanol to obtain a sample solution. And adding 30ml of petroleum ether (60-90 ℃) into 1g of spina date seed reference medicinal material, heating and refluxing for 2 hours, filtering, removing petroleum ether liquid, volatilizing the residue, adding 30ml of methanol, and preparing the reference medicinal material solution by the same method. Taking semen Ziziphi Spinosae saponin A, B reference substance, adding methanol to make into solutions containing 1mg per 1ml as reference substance solution. Performing thin layer chromatography (0502 of the four ministerial general rules of the design reside in the Chinese pharmacopoeia 2015), collecting 5 μ l of the sample solution, 10 μ l of the reference medicinal material solution, and 5 μ l of the reference solution, respectively dropping on the same silica gel G thin layer plate, developing with water saturated n-butanol as developing agent, taking out, air drying, spraying 1% vanillin sulfuric acid solution, and inspecting in sunlight. Spots of the same color should appear on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution and the reference medicinal material; inspecting under ultraviolet lamp (365nm), wherein the same blue fluorescent spot appears on the sample chromatogram at the position corresponding to the control chromatogram.
Taking 4g of the product, grinding, adding 30ml of trichloromethane, heating and refluxing for 2 hours, removing trichloromethane liquid, volatilizing the solvent from the dregs, adding 20ml of saturated n-butyl alcohol, carrying out ultrasonic treatment for 30 minutes, filtering, adding 5 times of ammonia test solution into the filtrate, shaking uniformly, standing for layering, taking the upper layer liquid, evaporating to dryness, and adding 2ml of methanol into the residue for dissolving to obtain a test solution. Preparing 1g of ginseng reference medicinal material, and preparing a reference medicinal material solution by the same method. Collecting ginsenoside Rb1Ginsenoside Re, ginsenoside Rf, and ginsenoside Rg1As a control, 1mg of each solution was prepared by adding methanol to 1ml of the solution. Performing thin layer chromatography (0502 of the four ministry of the national formulary of the national pharmacopoeia 2015), sucking 10 μ l of test solution, 5 μ l of control solution and 5 μ l of control solution, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol-water (13:6:2) solution at a temperature below 10 deg.C overnight as developing agent, taking out, air drying, spraying with 10% ethanol sulfate solution, heating at 105 deg.C until the color of spots is clear, and inspecting under sunlight and ultraviolet lamp (365 nm). In the chromatogram of the test solution, spots or fluorescent spots of the same color should appear at the positions corresponding to those of the reference medicinal material and the reference solution.
Content determination: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile is taken as a mobile phase A, and water is taken as a mobile phase B; elution was performed with a gradient as specified in the table below; the detection wavelength is 335 nm; the flow rate is 1.0 ml/min; the temperature was 25 ℃.
Figure BDA0003063146350000101
Taking a proper amount of the spinosad reference substance, precisely weighing, and adding methanol to prepare a solution containing 50 mu g of the spinosad per 1ml, thus obtaining the reference substance solution. Taking a proper amount of sample, grinding, taking about 2g, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of 75% methanol, sealing the plug, weighing, carrying out ultrasonic treatment (power 500W and frequency 40kHz) for 30 minutes, cooling, weighing again, supplementing the weight loss by using 75% methanol, shaking up, filtering, and taking a subsequent filtrate to obtain a sample solution. Precisely sucking 5 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
The insomnia granule is prepared by 15 parts of raw wild jujube kernel, 15 parts of cooked spina date seed, 9 parts of ginseng, 6 parts of salvia miltiorrhiza, 9 parts of radix ophiopogonis, 9 parts of poria with hostwood, 9 parts of angelica, 3 parts of schisandra chinensis, 3 parts of rhizoma acori graminei and 3 parts of liquorice, adding 10 times of water for decocting for 3 times each time for 2 hours each time, combining decoctions, filtering, standing for 12 hours and concentrating to a proper amount; spray drying to obtain dry extract powder, adding maltodextrin and appropriate amount of aspartame equal to the dry extract powder, mixing, spray granulating with water, drying, and sieving.
The technical scheme of the invention is further described by combining pharmacodynamic experiments.
Pharmacodynamic experiments of the sedative effect of the insomnia granules prepared by the process of the invention prove that the sedative effect of the insomnia granules has the same efficacy as that of the traditional decoction.
Reagent: the invention provides the sleep-improving granule (prepared by the method of example 1) and the sleep-improving pill decoction, which are provided by Lishizhen pharmaceutical group Limited company, and the granule is prepared into uniform suspension with required concentration by grinding with 0.5 percent CMC-Na before use.
And (3) spontaneous activity detection: SD rats are divided into a control group, a model group, a treatment group (a group with low and high-dose Anmian granules and Anmian Dan group) and a positive drug group (melatonin), the model group is injected into the abdominal cavity of the rat to carry out model building, and the treatment group is continuously administrated for 1 week. Monitoring by using an Ethovision video analysis system, keeping the ambient environment quiet in the experimental process, putting each group of rats into an activity test box, and detecting various behavioral indexes of the rats within 2min, including moving distance, activity speed, activity time and the like. The administration dosage of Anmiandan (decoction) is 4.55 g/kg based on crude drug amount-1·d-1The administration dosage of the low-dose and high-dose groups of the Anmian granules is respectively 4.55 g.kg-1·d-1And 18.18 g.kg-1·d-1
The results show (see table 1) that the mean moving distance of the rats in the model group is prolonged and the mean moving speed is increased (P < 0.01) compared with the control group, and the moving distance of the rats is shortened and the moving speed is reduced (P < 0.01) after the intervention of the high-dose group of the insomnia granules compared with the model group. However, the low dose group of Anmo particles showed no statistical difference in distance traveled and mean velocity compared to the model group (P > 0.05). Meanwhile, compared with the Anmiandan group, the high dose of the Anmiandan granules further reduces the moving distance and the moving speed of the rats (P is less than 0.05), but the low dose group has no statistical difference (P is more than 0.05) compared with the Anmiandan group. The cumulative time of movement of the rats in each group was further counted, and the results showed that the cumulative time of movement of the rats in the model group was prolonged (P < 0.01) compared with that in the control group. Compared with the model group, the low-insomnia granule and high-dose group can obviously shorten the movement accumulated time of rats (P is less than 0.01). Meanwhile, compared with the somnan group, the somnan granule low dose group has no statistical difference (P is more than 0.05).
TABLE 1 comparison of distance, speed and time of locomotion for voluntary activities between groups
Figure BDA0003063146350000111
Figure BDA0003063146350000112
Note: compared with the control group, the compound of the formula,*P<0.05,**p is less than 0.01; in comparison with the set of models,#P<0.05,##p is less than 0.01. Compared with the group of Anemarrhena, SP is less than 0.05 and SP is less than 0.01.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The insomnia particle is characterized by comprising, by mass, 6-12 parts of ginseng, 4-8 parts of salvia miltiorrhiza, 6-12 parts of radix ophiopogonis, 2-4 parts of liquorice, 6-12 parts of poria with hostwood, 10-20 parts of raw jujube kernel, 10-20 parts of cooked jujube kernel, 2-4 parts of rhizoma acori graminei, 6-12 parts of angelica and 2-4 parts of schisandra chinensis.
2. The method for preparing the insomnia granule according to claim 1, wherein the method for preparing the insomnia granule comprises:
step one, ginseng, salvia miltiorrhiza, radix ophiopogonis, liquorice, poria with hostwood, raw date kernels, cooked date kernels, rhizoma acori graminei, angelica and schisandra chinensis are decocted with water each time; filtering, and mixing decoctions;
step two, standing for 12-16 hours and then concentrating to a proper amount; spray drying to obtain dry extract powder, adding maltodextrin and appropriate amount of aspartame equal to the dry extract powder, mixing, granulating with water spray, and drying.
3. The method for preparing Anmian granules according to claim 2, wherein in the first step, 10 times of water is added and decocted for 3 times each time; each time for 2 hours.
4. The method for identifying the insomnia granule according to claim 1, wherein the method for identifying the insomnia granule comprises:
(1) grinding the prepared Anmian granule, adding methanol, refluxing under heating, filtering, evaporating the filtrate to dryness, and dissolving the residue in methanol to obtain sample solution;
(2) adding petroleum ether into semen Ziziphi Spinosae control material, heating and refluxing, filtering, removing petroleum ether solution, volatilizing residue, adding methanol, heating and refluxing, filtering, evaporating filtrate, and dissolving residue with methanol to obtain control solution;
(3) dissolving semen Ziziphi Spinosae saponin A, B reference substance in methanol to obtain reference solution;
(4) sucking the prepared test solution, reference medicinal material solution and reference solution, respectively dropping on the same silica gel G thin layer plate, developing with water saturated n-butanol as developing agent, taking out, air drying, and spraying vanillin sulfuric acid solution;
(5) inspecting whether spots or fluorescent spots with the same color appear in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution and the reference medicinal material under the daylight and ultraviolet lamps respectively.
5. The method for identifying insomnia granule according to claim 4, wherein the step (1) specifically comprises: grinding 4g of the prepared Anmian granule, adding 30ml of methanol, heating and refluxing for 1 hour, filtering, evaporating the filtrate, and dissolving the residue in 1ml of methanol to obtain a sample solution;
the step (2) specifically comprises: taking 1g of spina date seed reference medicinal material, adding 30ml of petroleum ether (60-90 ℃), heating and refluxing for 2 hours, filtering, removing petroleum ether liquid, volatilizing medicinal residues, adding 30ml of methanol, heating and refluxing, filtering, evaporating filtrate to dryness, and adding 1ml of methanol to dissolve residues to obtain a reference medicinal material solution.
6. The method for identifying insomnia granule according to claim 4, wherein in the step (3), methanol is added to prepare solutions each containing 1mg per 1ml as a control solution;
the step (4) specifically comprises: sucking 5 μ l of prepared test solution, 10 μ l of control solution and 5 μ l of control solution, respectively dropping on the same silica gel G thin layer plate, developing with water saturated n-butanol as developing agent, taking out, air drying, and spraying 1% vanillin sulfuric acid solution;
and (5) respectively placing the sample in the sunlight and ultraviolet lamp 365nm to inspect whether spots or fluorescent spots with the same color appear on the chromatogram of the test sample at the positions corresponding to the chromatograms of the reference substance and the reference medicinal material.
7. The method for identifying the insomnia granule according to claim 1, wherein the method for identifying the insomnia granule comprises:
1) grinding 4g of the prepared Anmian granules, adding 30ml of trichloromethane, heating and refluxing for 2 hours, removing the trichloromethane liquid, volatilizing the solvent from the residue, adding 20ml of water-saturated n-butyl alcohol, carrying out ultrasonic treatment for 30 minutes, and filtering;
2) adding 5 times of ammonia test solution into the filtrate, shaking, standing for layering, collecting supernatant, evaporating to dry, and dissolving the residue with 2ml of methanol to obtain test solution;
3) collecting Ginseng radix reference material 1g, and preparing reference material solution by the same methodLiquid; collecting ginsenoside Rb1Ginsenoside Re, ginsenoside Rf, and ginsenoside Rg1Adding methanol to obtain solutions each containing 1mg per 1ml as reference solution;
4) sucking 10 μ l of test solution, 5 μ l of control solution and 5 μ l of control solution, respectively dropping on the same silica gel G thin layer plate, developing with lower layer solution of chloroform, methanol and water at 10 deg.C below overnight as developing agent, taking out, and air drying;
5) spraying 10% sulphuric acid ethanol solution, heating at 105 deg.C until the spots are clearly developed, and respectively placing in sunlight and ultraviolet lamp 365nm to check whether spots or fluorescent spots with the same color appear on the corresponding positions of the reference medicinal material and the reference substance in the chromatogram of the test solution.
8. The method for identifying insomnia granule as claimed in claim 7, wherein the mixing ratio of chloroform, methanol and water is 13:6: 2.
9. The content determination method of the safety particles as claimed in claim 1, wherein the content determination method of the safety particles comprises:
octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile is taken as a mobile phase A, and water is taken as a mobile phase B; eluting according to gradient; the detection wavelength is 335 nm; the flow rate is 1.0 ml/min; the temperature is 25 ℃; taking a proper amount of the spinosad reference substance, precisely weighing, and adding methanol to prepare a solution containing 50 mu g of the spinosad per 1ml, thus obtaining a reference substance solution; taking a proper amount of sample, grinding, taking about 2g, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of 75% methanol, sealing the plug, weighing, carrying out ultrasonic treatment for 30 minutes, cooling, weighing again, supplementing the lost weight with 75% methanol, shaking up, filtering, and taking a subsequent filtrate to obtain a sample solution; precisely sucking 5 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
10. The method for determining content of insomnia particles according to claim 9, wherein the ultrasonic treatment comprises: ultrasonic power 500W, frequency 40 kHz.
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