CN1205971C - Naolejing granular preparation - Google Patents
Naolejing granular preparation Download PDFInfo
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- CN1205971C CN1205971C CN 02157241 CN02157241A CN1205971C CN 1205971 C CN1205971 C CN 1205971C CN 02157241 CN02157241 CN 02157241 CN 02157241 A CN02157241 A CN 02157241A CN 1205971 C CN1205971 C CN 1205971C
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Abstract
The present invention relates to a Naolejing granular preparation which is a traditional Chinese medicine for mainly treating insomnia. The Naolejing granular preparation has the effects on cultivating mind, strengthening the brain and tranquilizing; the Naolejing granular preparation is prepared by using 125 weight parts of Chinese date, 35.4 weight parts of liquorice extract and 416 weight parts of wheat as raw medicinal materials; the Naolejing granular preparation also contains 50 to 150 weight parts of at least one of an auxiliary material forming agent, polylactose and dextrin, 0 to 3 weight parts of stevioside as an auxiliary material and 0 to 10 weight parts of PVP. a spray-drying method and a dry granulation method are used in a preparation technique for completely reserving efficient ingredients, so large-scale production under a continuous GMP condition is convenient. The medicine does not contain sucrose or a preservative agent and has the advantages of safe administration, no side effect, high medicine stability, convenient administration and accurate dose.
Description
(technical field)
The present invention relates to a kind of have nourish heart, the effect of calming the nerves based on medicine of Cure for insomnia and preparation method thereof, belongs to the field of Chinese medicines.
(background technology)
Diseases such as depressed, easily frightened insomnia, agitation are commonly encountered diseases, frequently-occurring disease, particularly along with the quickening of social rhythm, the increasing of operating pressure and the aging of population, the further R and D for the treatment of such disease medicament have been received bigger concern.Also there be not a kind of the safe, efficient of such disease for the treatment of in the modern chemistry medicine, can be for the medicine of taking for a long time, and develop the Chinese medicine traditional advantage, exploitation preparation stabilization, drug safety, dosage is accurate, quality controllable, the reliable Chinese medicine preparation of curative effect is significant.
The Chinese medicine Naolejing be a kind of be used for the treatment of depressed, easily frightened insomnia, agitation and the children's's night restlessness Chinese medicine patent medicine preparation of disease such as sleep is made by main material medicine Fructus Jujubae, Radix Glycyrrhizae extractum and Semen Tritici aestivi, have nourish heart, brain-strengthening, sedative action.But said preparation is the liquid sugar sirup preparation at present, and dosage form falls behind, and medicine stability is poor; Contain antiseptic and a large amount of sucrose, the absorption of antiseptic and too much sugar there is no benefit to human body, influences the safe handling of preparation; Also can produce untoward reaction such as hyperglycemia to suffering from some patient who avoids sugared disease simultaneously; According to the literature, take the food and the medicine that contain preservative benzoic acid for a long time and can cause liver dysfunction, have potential liver toxicity, particularly, can increase the weight of liver dysfunction, because of containing preservative benzoic acid in the Naolejing syrup for the hepatic disease patient, the abnormal liver function person should not take.
In addition, the each dosage of syrup is measured by patient oneself, and dosage is inaccurate, influences the curative effect of preparation.
(summary of the invention)
The invention provides the agent of a kind of Chinese medicine NAOLEJING KELI, contain the harmful effect to human body of antiseptic and a large amount of multitudinous sugar to overcome liquid preparation, and reach taking convenience, the amount of getting is purpose accurately.Another object of the present invention provides the preparation method of this NAOLEJING KELI preparation.
NAOLEJING KELI agent of the present invention is that crude drug is made by 125 weight portion Fructus Jujubaes, 35.4 weight portion Radix Glycyrrhizae extractum and 416 weight portion Semen Tritici aestivis, and medicament also contains forming agent 50-150 weight portion, and this forming agent is at least a in poly lactose and the dextrin; Contain adjuvant polyvinylpyrrolidone (calling PVP in the following text) 0-10 weight portion in addition, stevioside 0-0.5 weight portion.
The preparation method of this NAOLEJING KELI agent is as follows:
Extracting liquorice extractum 35.4 weight portions, it is an amount of to add water, and heating is dissolved, and filters, and filtrate is concentrated in right amount.Other gets Fructus Jujubae 125 weight portions, decocts with water secondary by 8～10 times of amounts, decocts 2 hours at every turn, merges the secondary decocting liquid, filters, and filtrate is concentrated into relative density and reaches 1.07～1.13 (50 ℃), adds the ethanol of equivalent after cold, stirs evenly, and leaves standstill 24 hours; Get Semen Tritici aestivi 416 weight portions, add 4～5 times in water, boil after 10 minutes in 70～80 ℃ of warm macerating, repeat secondary, each warm macerating 2 hours merges the secondary immersion, filters, and filtrate is concentrated in right amount, adds the ethanol of equivalent again, stirs evenly, and leaves standstill 24 hours; The pure liquid of above-mentioned Fructus Jujubae and Semen Tritici aestivi is filtered, reclaim ethanol, 70 ℃ of following distilling under reduced pressure are concentrated into relative density and reach 1.07～1.13 (50 ℃), merge and add the Radix Glycyrrhizae extractum concentrated solution, add 0-0.5 weight portion stevioside, boil dissolving, at least a in add-on type agent oligomeric lactose and the dextrin, the forming agent total amount is the 50-150 weight portion, filter, under atomize, feed hot-air, carry out spray drying, 160-200 ℃ of hot-air inlet temperature, leaving air temp 70-100 ℃, add PVP 0-10 weight portion, material is dry granulation under≤60 ℃ of temperature, and granulate promptly gets product.
The present invention changes the Naolejing syrup into granule (solid preparation), and medicine stability is good, easily storage.Granule medicament packing error is very little, and is convenient to packing; Can be distributed into bag by each dose, each 1 bag, taking convenience, dosage are accurate, and said preparation does not contain antiseptic and sucrose, take safety and have no side effect.
NAOLEJING KELI agent of the present invention is that the new technique by spray drying, dry granulation is prepared from.Spray drying technology is by nebulizer medicinal liquid to be sprayed into droplet, be dispersed in the thermal current, make moisture flash evapn drying, and the loose powdered granule of formation, effective ingredient such as liquirtin are not destroyed and keep fully, overcome present syrup and be aqueous solution state, effective ingredient is easily degraded and unsettled drawback.Dry granulation is that medicine dry powder is added binding agent adjuvant PVP, mechanical compaction under the convection drying state, becomes whole and forms, and makes effective ingredient such as liquirtin constant.The said method operating process is simple, is convenient to large-scale production under the seriality GMP condition.
(specific embodiment)
The preparation (one) of embodiment one NAOLEJING KELI agent
Take by weighing materials of wheat 416g, Radix Glycyrrhizae extractum 35.4g, Fructus Jujubae 125g.
It is an amount of that Radix Glycyrrhizae extractum 35.4g adds water, and heating is dissolved, and filters, and it is 1.10 (50 ℃) that filtrate is concentrated into proportion.Other gets Fructus Jujubae 125g, decocts with water secondary, decocts for the first time to add water by 10 times of amounts, decocts for the second time to add water by 8 times of amounts, each decoction amount of water is 2 hours, merges the secondary decocting liquid, filters, and filtrate is concentrated in right amount, add the ethanol of equivalent after cold, stir evenly, left standstill 24 hours; Get Semen Tritici aestivi 416g, boil after 10 minutes in 70～80 ℃ of warm macerating, repeat secondary, secondary decocts respectively by 5 times and 4 times of amounts and adds water, and each warm macerating 2 hours merges immersion, filtration, and filtrate is concentrated in right amount, adds the ethanol of equivalent again, stirs evenly, and leaves standstill 24 hours; The pure liquid of above-mentioned Fructus Jujubae and Semen Tritici aestivi is filtered, decompression recycling ethanol (temperature is below 70 ℃), being concentrated into proportion is 1.10 (50 ℃), merge and add the Radix Glycyrrhizae extractum concentrated solution, add stevioside glycosides 0.2g, boil dissolving, add dextrin 75g, filter spray drying (180 ℃ of inlet temperature, 80 ℃ of leaving air temps), get dry fine powder, add binding agent PVP28, dry granulation (temperature of charge is below 60 ℃), granulate gets brown yellow granule 165g, feeble QI, it is sweet to distinguish the flavor of.Be distributed into bag by each dose 5g.
The preparation (two) of embodiment two NAOLEJING KELI agent
Preparation process is with embodiment one, and different is to add forming agent oligomeric lactose 75g, adds binding agent PVP 1.5g, stevioside 0.3g, and dry granulation (temperature of charge is below 60 ℃), granulate gets brown yellow granule 165g, feeble QI, it is sweet to distinguish the flavor of.Be distributed into bag by each dose 5g.
Embodiment three concentrated solution relative densities are to the influence of drying process with atomizing
The spray drying efficient of medicinal liquid is relevant with the concentration of medicinal liquid, according to following table, with the relative density 1.07～1.13 (50 ℃) of concentrated solution as striking point.
Table 1 concentrated solution relative density is to the influence of drying process with atomizing
The relative density of concentrated solution is to the influence of drying process with atomizing
＜1.07 spray-dried granules are too thin, and yield is low, the energy consumption height
1.07～1.13 normal spray dryings, uniform particles
＞1.13 medicinal liquid thickness, drying time is long, and granule is thick, moisture is high
Embodiment four outlet and inlet temperature are to the influence of spray drying powder
The spray drying condition is very important to the reservation and the grain forming of composition.For the benefit of the reservation of effective ingredient and grain forming compare as table 2 inlet temperature, leaving air temp.
Table 2 outlet and inlet temperature is to the influence of spray drying powder
Inlet temperature (℃) leaving air temp (℃) influence of liquirtin retention rate (%) water content (%) to granulating
200 90 95.3 3.6 is poor slightly
180 80 98.6 4.1 is very good
170 80 99.1 5.8 is better
The granulation result of the test shows, the water content of this preparation semi-finished product fine silt is at 4.0～6.0% o'clock, and directly dry type makes granularity, granule that hardness is suitable; Water content is higher than at 8.0% o'clock, and mobility of particle is relatively poor, and the back moisture of granulating is difficult to be controlled in 5%; Water content was less than 4.0% o'clock, and particulate fine powder is many slightly, and productive rate can descend.Therefore should control spray-dired inlet temperature is 160-200 ℃, leaving air temp 70-100 ℃.
The stability study of embodiment five Naolejing syrup, NAOLEJING KELI
Naolejing syrup, NAOLEJING KELI having been carried out stable contrast test, adopted the room temperature test that keeps sample, is index with hygiene inspection and liquirtin content, experimental result such as table 3.
The stable contrast test of table 3 Naolejing syrup, NAOLEJING KELI
Embodiment six Naolejing syrup, NAOLEJING KELI are to the influence of mouse blood sugar
Get 30 of healthy adult kunming mices, be divided into three groups, 10 every group.Fasting 12 hours is freely drunk water, and irritates stomach respectively and gives Naolejing syrup 10ml/kg, NAOLEJING KELI 2g/kg and normal saline 0.2ml.After the administration 1 hour, blood sugar concentration (GLU) was measured in the eyeball blood sampling, the results are shown in Table 4.
Table 4 Naolejing syrup, NAOLEJING KELI are to the influence of blood glucose
Sample GLU (mmol/L)
Naolejing syrup 5.23 ± 0.79 (p＜0.05)
NAOLEJING KELI 3.51 ± 0.60
Normal saline 3.82 ± 0.90
The result shows, the blood sugar concentration of mice obviously raise after taking the Naolejing syrup, and it is constant substantially to take after the NAOLEJING KELI blood sugar concentration of mice.Illustrate that this medicine also can be used for diabetics, can not cause blood sugar increasing.
Following method quality discrimination is pressed in NAOLEJING KELI agent of the present invention:
(1) get this product 4g, put in the separatory funnel, add water 30ml, jolting, add diethyl ether respectively 40ml, 30ml extract twice, and merging filtrate volatilizes, and residue adds methanol 2ml makes dissolving, as need testing solution.Other gets Fructus Jujubae control medicinal material powder 2g, adds petroleum ether (60-90) 10ml and soaks 10 minutes, and about 10 minutes of supersound process filters, discard petroleum ether liquid, medicinal residues dry, and the 20ml that adds diethyl ether soaked 1 hour, supersound process 20 minutes, filter, filtrate is concentrated into 2ml, in contrast medical material solution.Test according to thin layer chromatography (appendix VI B).Drawing need testing solution 10 μ l, reference substance solution 3 μ l, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-glacial acetic acid (14: 4: 0.5), launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get this product 4g, add water 40ml, shake up, with water saturated n-butanol extraction 2 times, each 40ml merges n-butyl alcohol liquid, washes with water 2 times, each 15ml, and n-butyl alcohol liquid is put evaporate to dryness in the water-bath, and residue adds methanol 5ml makes dissolving, as need testing solution.Other gets extracting liquorice control medicinal material 1g, adds methanol 40ml, puts in the water-bath reflux 1 hour, filter, filtrate evaporate to dryness, residue add water 40ml makes dissolving, aqueous solution n-butanol extraction 3 times, each 20ml, merge n-butyl alcohol liquid, wash with water 2 times, put evaporate to dryness in the water-bath, residue adds methanol 5ml makes dissolving, as need testing solution.According to thin layer chromatography (appendix VI B) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (22: 2: 0.5: 0.5) be developing solvent, launch that taking-up is dried, spray was with 3%AlCl with ethyl acetate-methanol-glacial acetic acid-water
3Alcoholic solution, 105 ℃ be heated to the colour developing clear, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(3) get this product 4g, add water 40ml, extract 3 times with the petroleum ether jolting, each 30ml merges petroleum ether layer, puts 45 ℃ of water-baths and volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Semen Tritici aestivi control medicinal material powder 10g, adds dehydrated alcohol 30ml, supersound process 40 minutes, filter, filtrate adds 50% sodium hydroxide 1ml, reflux 15 minutes, cooling, in the dislocation separatory funnel, water 20ml gradation washing container, washing liquid is incorporated in the separatory funnel, extracts 3 times with the petroleum ether jolting, each 30ml, merge petroleum ether layer, put in 45 ℃ of water-baths and volatilize, residue adds ethyl acetate 1ml dissolving, medical material solution in contrast.Test according to thin layer chromatography (appendix VI B), drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with petroleum ether (60-90 ℃)-ethyl acetate (3: 1), launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to the colour developing clear, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
This preparation carries out the liquirtin assay according to high performance liquid chromatography (" 2000 editions one appendix VI D of Chinese pharmacopoeia).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler, and acetonitrile-0.1% trifluoroacetic acid aqueous solution (13: 83) is a mobile phase (v/v); The detection wavelength is 218-320nm.Number of theoretical plate calculates by the liquirtin peak should be not less than 3000.
The preparation of reference substance solution: precision takes by weighing in 60 ℃ of liquirtin reference substances that are dried to constant weight an amount of, makes the solution that every 1ml contains 0.2mg with mobile phase, promptly.
The preparation of need testing solution: precision takes by weighing the liquirtin reference substance that is dried to constant weight in exsiccator, is made into the solution that contains liquirtin 0.04mg among every 1ml with methanol, shakes up, promptly.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, calculate with external standard method, promptly.This product contains Radix Glycyrrhizae in liquirtin for every bag, must not be less than 5mg.
The agent of this NAOLEJING KELI adopts said method to carry out quality control, the discriminating of Fructus Jujubae and Semen Tritici aestivi and the assay of liquirtin have been increased, compare with the national standard of the existing quality control of Naolejing syrup, quality standard of the present invention has had significant raising, has controlled the quality of product effectively.
Claims (2)
1, a kind of granule of Cure for insomnia, it is characterized in that by:
125 weight portion Fructus Jujubaes, 35.4 weight portion Radix Glycyrrhizae extractum and 416 weight portion Semen Tritici aestivis;
Forming agent 50-150 weight portion, this forming agent are at least a in poly lactose and the dextrin; With adjuvant PVP 2 weight portions, adjuvant stevioside 0-0.5 weight portion is made.
2, the preparation method of the granule of a kind of Cure for insomnia according to claim 1 is characterized in that:
A. take by weighing Radix Glycyrrhizae extractum, Fructus Jujubae, Semen Tritici aestivi, standby;
B. to add water an amount of for Radix Glycyrrhizae extractum, and heating is dissolved, and filters, and filtrate is concentrated into appropriateness, and is standby;
Fructus Jujubae decocts with water secondary by 8～10 times of amounts, decocts 2 hours at every turn, merges the secondary decocting liquid, filters, and filtrate is concentrated into appropriateness, adds the ethanol of equivalent after cold, stirs evenly, and leaves standstill 24 hours;
Semen Tritici aestivi adds 4～5 times in water, boils after 10 minutes in 70～80 ℃ of warm macerating, repeats secondary, and each warm macerating 2 hours merges the secondary immersion, filters, and filtrate is concentrated into appropriateness, adds the ethanol of equivalent again, stirs evenly, and leaves standstill 24 hours;
The pure liquid of above-mentioned Fructus Jujubae and Semen Tritici aestivi is filtered, reclaim ethanol, 70 ℃ of relative densities 1.07～1.13 when being evaporated to 50 ℃ merge and add the Radix Glycyrrhizae extractum concentrated solution;
C. with stevioside 0-0.5 weight portion, boil and dissolve, add at least a in forming agent poly lactose and the dextrin, total amount is the 50-150 weight portion; Filter, spray drying, dry granulation, granulate promptly get product;
D. wherein the relative density of the concentrated medicament of Radix Glycyrrhizae extractum, Fructus Jujubae and Semen Tritici aestivi is 1.07～1.13 in the time of 50 ℃; Spray-dired inlet temperature is that 160-200 ℃, leaving air temp are 70-100 ℃;
Make powder and contain moisture 4%～6%;
Add the PVP2 weight portion, directly dry granulation;
Temperature of charge is below 60 ℃ during granulation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02157241 CN1205971C (en) | 2002-12-25 | 2002-12-25 | Naolejing granular preparation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02157241 CN1205971C (en) | 2002-12-25 | 2002-12-25 | Naolejing granular preparation |
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| CN1425434A CN1425434A (en) | 2003-06-25 |
| CN1205971C true CN1205971C (en) | 2005-06-15 |
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| CN 02157241 Expired - Fee Related CN1205971C (en) | 2002-12-25 | 2002-12-25 | Naolejing granular preparation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108969692A (en) * | 2018-08-15 | 2018-12-11 | 康美保宁（四川）制药有限公司 | A kind of preparation method of Naolejing medicinal extract |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103705774A (en) * | 2013-12-30 | 2014-04-09 | 江苏省中医院 | Compound composition with effect of treating depression as well as preparation method and application thereof |
| CN110433253A (en) * | 2018-05-03 | 2019-11-12 | 杭州市妇产科医院 | A kind of liquorice-wheat-jujube particle and its preparation method and application |
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- 2002-12-25 CN CN 02157241 patent/CN1205971C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108969692A (en) * | 2018-08-15 | 2018-12-11 | 康美保宁（四川）制药有限公司 | A kind of preparation method of Naolejing medicinal extract |
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