CN1843488A - Granula and its preparation method - Google Patents

Abstract

Disclosed is a Chinese medicinal granule and its preparing process, which comprises the following steps: (1) mixing 17 kinds of medicinal herbs, watering and boiling 2-4 times, (2) merging the grilling liquid, filtrating, concentrating the filtrate into thick grease with specific gravity of 1.0-1.5, (3) charging ethanol to a content of 40-80%, stewing, alcohol deposition, reclaiming ethanol from the supernatant fluid, condensating into thick form, (4) drying, disintegrating into fines, charging cane sugar, palletizing, drying, mixing homogenously.

Description

A kind of granula and preparation method thereof

Technical field

The present invention relates to the improvement technology of sweet dreams Chinese medicine preparation, be specially a kind of granula and preparation method thereof.

Background technology

The sweet dreams Chinese medicine preparation is formulated by Radix Et Caulis Acanthopanacis Senticosi, Rhizoma Polygonati, silkworm pretty young woman, Fructus Mori, Radix Codonopsis, Fructus Amomi, Fructus Lycii, Fructus Crataegi, Radix Rehmanniae Preparata, Herba Epimedii (system), Pericarpium Citri Reticulatae, Poria, Semen Strychni (system), Rhizoma Pinelliae Preparatum, Rhizoma Alismatis, Rhizoma Dioscoreae, effect with vital energy benefiting and the kidney invigorating, invigorating the spleen and regulating the stomach, tranquilizing by nourishing the heart, be used for dizziness and tinnitus, look to subtract to listen and decline, insomnia forgetfulness, inappetence, nervous is breathed hard apoplexy sequela at soreness of the waist and knees; To Aging, the coronary vasodilator illness, cerebral vessels embolism and alopecia also have certain effect.At present, the dosage form of sweet dreams Chinese medicine preparation only has oral liquid and capsule, and dosage form is comparatively single, and the capsule dysphagia can not satisfy people's medication demand.

According to the relevant drug act of China, changing dosage form needs as a kind of new drug research, based on the shortcoming that existing dosage form exists, is necessary product technology is done necessary improvement, forms new preparation.

Summary of the invention

The object of the present invention is to provide a kind of granula and preparation method thereof, its preparation technology is simple, reasonable, and the granular preparation onset of formation is rapid, good effect.

Technical scheme of the present invention is:

The prescription of granula is composed as follows:

Radix Et Caulis Acanthopanacis Senticosi 177.59g; Rhizoma Polygonati 222.01g; Bombycis mori 44.39g; Fructus Mori 110.99g; Radix Codonopsis 133.20g; Radix Astragali 133.20g; Fructus Amomi 17.75g; Fructus Lycii 133.20g; Fructus Crataegi 532.80g; Radix Rehmanniae Preparata 88.81g; Herba Epimedii (system) 88.81g; Pericarpium Citri Reticulatae 88.81g; Poria 88.81g; Semen Strychni (system) 4.43g; Rhizoma Pinelliae Preparatum 88.81g; Rhizoma Alismatis 133.20g; Rhizoma Dioscoreae 88.81g.

The preparation method of granula comprises the steps:

(1) above 17 flavors mix, and decoct with water 2～4 times, add the water of 5～15 times of ten seven flavor medicine gross weights, each 0.5～3 hour at every turn;

(2) collecting decoction filters, and it is 1.0～1.5 that filtrate is concentrated into relative density, and concentrated employing reduced vacuum concentrates or normal pressure concentrates;

(3) add ethanol and make and contain alcohol amount and reach 4080% (weight percentage), leave standstill, precipitate with ethanol, till precipitation fully, get supernatant and reclaim ethanol, be concentrated into the thick paste shape, concentrate and adopt reduced vacuum to concentrate or normal pressure concentrates, the relative density of thick paste is 1.25-1.45;

(4) drying is ground into fine powder, and powder particle size is 70～120 orders, adds the 2-12 sucrose doubly of dried cream powder weight, granulate, and drying, mixing, promptly; Or join in the thick paste with the sucrose of respective numbers, drying is ground into fine powder, granulates, and drying, mixing, promptly.

The invention has the beneficial effects as follows:

1, the present invention is modified into granular preparation with original dosage form, uses the modern pharmaceutical technology this product technology is done necessary improvement, forms new preparation, and this granular preparation has rapid, the eutherapeutic characteristics of onset, vital energy benefiting and the kidney invigorating, invigorating the spleen and regulating the stomach, tranquilizing by nourishing the heart.Be used for dizziness and tinnitus, look to subtract to listen and decline, insomnia forgetfulness, inappetence, soreness of the waist and knees is had palpitation and is breathed hard apoplexy sequela; To Aging, the coronary vasodilator illness, cerebral vessels embolism and alopecia also have certain effect.

2, production technology of the present invention is reasonable, and the quality standard of control product is higher.

The specific embodiment

Embodiment 1

Ten seven flavor medicines with the granula prescription decoct with water secondary, each 10 times of water, 1.5 hours for the first time, 1 hour for the second time, collecting decoction, filter, it is 1.0 that filtrate is concentrated into relative density, adds ethanol and makes and contain the alcohol amount and reach 65% (weight percentage), leave standstill, precipitate with ethanol, till precipitating fully, get supernatant and reclaim ethanol, be concentrated into the thick paste shape, concentrated employing reduced vacuum concentrates or normal pressure concentrates, and the relative density of thick paste is 1.25-1.45; Drying is ground into fine powder, and powder particle size is 70～120 orders, adds the 2-12 sucrose doubly of dried cream powder weight, granulate, and drying, mixing, promptly.Or join in the thick paste with the sucrose of respective numbers, drying is ground into fine powder, granulates, and drying, mixing is made 2000g, promptly.This product is tan granule, and it is little sweet, sour to distinguish the flavor of; Specification: every packed 6g; Usage and consumption: oral, one time 1 bag, 2 times on the one; Storage: sealing.

1, differentiates

(1) get this product 6g, add methanol 6ml, supersound process 15 minutes filters, and filtrate is as need testing solution.Other gets Pericarpium Citri Reticulatae control medicinal material 2g, adds methanol 10ml, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix of Chinese Pharmacopoeia version in 2005), draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively on the silica gel g thin-layer plate of same usefulness 0.5% sodium hydroxide preparation, with ethyl acetate-methanol-water (100: 17: 13, volume ratio) is developing solvent, launches about 3cm, take out, dry, upper solution with toluene-ethyl acetate-formic acid-water (20: 10: 1: 1, volume ratio) is developing solvent again, and exhibition is to about 8cm, take out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with the aluminum chloride test solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

(2) get this product 20g, add water 50ml, boiled 5 minutes, filter, the n-butyl alcohol liquid that filtrate water is saturated extracts 3 times, each 20ml, merge n-butyl alcohol liquid, with 1% sodium hydroxide washing 3 times, each 20ml, reuse water washing 2 times, each 20ml, n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VI B), draw need testing solution 5 μ l, reference substance solution 2 μ l put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (65: 35: 10, volume ratio) lower floor's solution is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and hot blast blows to clear spot.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical sepia speckle; Put again under the ultra-violet lamp (365nm) and inspect, show identical orange-yellow fluorescence speckle.

(3) get this product 6g, add water 50ml and make dissolving, add the chloroform jolting and extract 2 times, each 30ml, merge extractive liquid,, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Fructus Lycii control medicinal material 2g, decocts with water 10 minutes, filters, and adds chloroform 20ml jolting and extracts, and shines medical material solution in pairs with legal system.According to thin layer chromatography (appendix VI B) test, draw need testing solution 10 μ l, control medicinal material solution 5 μ l put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid (3: 2: 1, volume ratio) is developing solvent, launches, take out, dry, 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 fluorescence speckle of same color.

(4) get need testing solution under [discriminating] (3) as need testing solution.Other gets the isofraxidin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.According to thin layer chromatography (appendix VIB) test, draw need testing solution 10 μ l, control medicinal material solution 2 μ l put respectively on same silica gel g thin-layer plate, with chloroform-methanol (19: 1, volume ratio) is developing solvent, launches, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

(5) get this product 6g, the 30ml that adds diethyl ether, supersound process 20 minutes, filter, discard filtrate, residue is flung to ether, add water 40ml and make dissolving, add water saturated n-butyl alcohol jolting and extract 2 times, each 30ml, merge n-butyl alcohol liquid, with water saturated water washing 2 times, each 20ml, discard water lotion, n-butyl alcohol liquid evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Other gets the Herba Epimedii reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VI B), draw need testing solution 10 μ l, control medicinal material solution 2 μ l put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-methanol-water (10: 1: 1: 1, volume ratio) is developing solvent, launch, take out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with the aluminum chloride test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

2, check

Moisture: measure according to aquametry (appendix of Chinese Pharmacopoeia version in 2005), must not cross 8.0%; Other should meet the relevant every regulation of granule (appendix of Chinese Pharmacopoeia version in 2005).

3, assay

Measure according to high performance liquid chromatography (appendix of Chinese Pharmacopoeia version in 2005).

4, chromatographic condition and system suitability test

With octadecylsilane chemically bonded silica is filler; Second eyeball-0.2% phosphoric acid solution (19: 81, volume ratio) is a mobile phase; Detect wavelength 283nm.Theoretical cam curve is calculated by the Hesperidin peak should be not less than 2000.

5, the preparation of reference substance liquid

It is an amount of to get the Hesperidin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 15 μ g, promptly.

6, the preparation of test sample liquid

Get the content under this product content uniformity item, porphyrize, mixing is got 1g, the accurate methanol 25ml that adds, close plug claims decide weight, and supersound process (250W, 50Hz) 40 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methanol, and filtration is got subsequent filtrate, promptly.

7, algoscopy

Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.

This product contains Pericarpium Citri Reticulatae with Hesperidin (C for every bag ₂₈H ₃₄O ₁₅) meter, must not be less than 1.8mg.

Embodiment 2

Ten seven flavor medicines with the granula prescription decoct with water each 5 times of water four times, 3 hours for the first time, 2 hours for the second time, 1 hour for the third time, the 4th time 0.5 hour, collecting decoction filtered, it is 1.5 that filtrate is concentrated into relative density, adds ethanol and makes and contain alcohol amount and reach 40% (weight percentage), leaves standstill, precipitate with ethanol, till precipitating fully, get supernatant and reclaim ethanol, be concentrated into the thick paste shape, drying, be ground into fine powder, powder particle size is 70～120 orders, adds the 2-12 sucrose doubly of dried cream powder weight, granulates, dry, mixing is made 2000g, promptly.This product is tan granule, and it is little sweet, sour to distinguish the flavor of; Specification: every packed 6g; Usage and consumption: oral, one time 1 bag, 2 times on the one; Storage: sealing.

Embodiment 3

Ten seven flavor medicines with the granula prescription decoct with water each 15 times of water three times, 2 hours for the first time, 1 hour for the second time, 0.5 hour for the third time, collecting decoction filters, and it is 1.2 that filtrate is concentrated into relative density, adding ethanol makes the alcohol amount of containing reach 80% (weight percentage), leave standstill, precipitate with ethanol, till precipitation fully, get supernatant and reclaim ethanol, be concentrated into the thick paste shape, drying is ground into fine powder, and powder particle size is 70～120 orders, the 2-12 sucrose doubly that adds dried cream powder weight, granulate drying, mixing, make 2000g, promptly.This product is tan granule, and it is little sweet, sour to distinguish the flavor of; Specification: every packed 6g; Usage and consumption: oral, one time 1 bag, 2 times on the one; Storage: sealing.

Claims (2)

1, a kind of granula is characterized in that: dosage form is a granule.

2,, it is characterized in that comprising the steps: according to the preparation method of the described granula of claim 1

(1) ten seven flavor medicines with granula mix, and decoct with water 2～4 times, add the water of 5～15 times of ten seven flavor medicine gross weights, each 0.5～3 hour at every turn;

(2) collecting decoction filters, and it is 1.0～1.5 that filtrate is concentrated into relative density;

(3) add ethanol and make and contain alcohol amount and reach 40～80%, leave standstill, precipitate with ethanol, till precipitation fully, get supernatant and reclaim ethanol, be concentrated into the thick paste shape;

(4) drying is ground into fine powder, and powder particle size is 70～120 orders, adds the 2-12 sucrose doubly of dried cream powder weight, granulate, and drying, mixing, promptly; Or join in the thick paste with the sucrose of respective numbers, drying is ground into fine powder, granulates, and drying, mixing, promptly.