CN104825615B - A kind of preparation method and its method of quality control of huanglian jiedu decoction granule - Google Patents
A kind of preparation method and its method of quality control of huanglian jiedu decoction granule Download PDFInfo
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Abstract
The invention discloses a kind of preparation method and its method of quality control of huanglian jiedu decoction granule, its preparation method are as follows：Taking the coptis, radix scutellariae, golden cypress, cape jasmine, totally four taste medicine materical crude slice add water to cook 2 times, filtration, merging filtrate, and filter vacuum, which is concentrated under reduced pressure, adds beta cyclodextrin stirs to obtain clear cream, then clear cream is spray-dried, dry granulation, produces huanglian jiedu decoction granule.Its method of quality control includes thin-layer qualitative discriminating and HPLC assays.Preparation method of the present invention can effectively solve the problems, such as to produce precipitation during the concentration of huanglian jiedu decoction medicinal extract, retain the active ingredient in raw material to greatest extent, can be widely applied in big production；The method of quality control is simple, comprehensively, can effectively control the quality of produced huanglian jiedu decoction granule, available in daily Quality Control work.
Description
Technical field
The invention belongs to Chinese medicinal granule technical field, and in particular to a kind of preparation side of huanglian jiedu decoction granule
Method and its method of quality control.
Background technology
Huanglian jiedu decoction is first recorded in Ge Hong《Handbook of Prescriptions for Emergencies》, temperature disease door when curing the wound cold, but the side's of not going out name；Tang Wang Tao
《Medical secrets of official》Draw Cui Shi side, begin named as huanglian jiedu decoction, so far the existing applicating history of 1700.The party is by the coptis, Huang
A kind of reed mentioned in ancient books, golden cypress, cape jasmine composition, are clearing heat and detoxicating representative side.The party collects the product in the coptis, radix scutellariae, golden cypress, cape jasmine big bitter Great Cold in one
Among side, using coptis purge the sthenic heart-fire as monarch, the simultaneous fire for rushing down middle Jiao；Minister is warm with radix scutellariae clearing lung-heat, rushes down the fire of the part of the body cavity above the diaphragm housing the heart and lungs；Assistant rushes down lower Jiao with golden cypress
Fire；Make the fire for rushing down three Jiao clearly with cape jasmine, heat conduction is descending；Four medicines share bitter cold and directly rolled over, and have the effect of heat-clearing, purging intense heat, removing toxic substances,
All real heat fiery poisons, the card of three burnt excess heats are cured mainly, the power of its purging intense heat and detonicating is very strong, three burnt fire-evil is gone, heat toxin must solve, all
Disease self-healing.
Modern pharmacological research shows that huanglian jiedu decoction has antibacterial, anti-inflammatory, antiendotoxin, anti-oxidant, antitumor, enhancing
Memory and improve memory disorders, improve cerebral ischemia, anoxic, protection stomach lining, intestinal mucosa, to suppress hepatic injury, anti-atherogenic hard
Other effects such as change, decompression, immunological regulation, are clinically widely used in hypertension, apoplexy sequelae, cerebrovascular disease, 2 type glycosurias
The treatment of disease, senile dementia and other diseases.
Chinese medicine compound prescription granule is under instruction of Chinese Medicine theory, to meet the high-quality Chinese medicine of concocted specification and Compatibility Law
Medicine materical crude slice is raw material, and the concentrated granular formed is refined using modern high technology, had both embodied middle medical drugs and has been particular about overall, dialectical apply
The characteristics of processed, meet people's tradition medication custom again.Chinese medicinal granule is a part for innovation of Chinese medicinal dosage form, is drunk instead of tradition
Piece uses, it is desirable to " medicine materical crude slice being come from, higher than medicine materical crude slice ".The " highly effective and safe, stably and controllable, square of medication is realized in Clinical practice
Just it is hygienic ".Because Chinese medicinal granule has small formulation, good effect, quick, take, carry, storing the features such as facilitating, it is non-
Often adapting to modern society includes needs of the international community to the nervous life of the demand of natural drug and modern society.
The preparation method of huanglian jiedu decoction granule is to make extraction solvent with water, and extract is concentrated through cryogenic vacuum, sprayed
Mist makes pellet after drying and formed.But during water boiling and extraction, the scutelloside in quaternary ammonium base and radix scutellariae in the coptis, golden cypress
React and produce a large amount of precipitations, if directly removed precipitation as impurity, mass efficient composition present in precipitation is small
Bark of a cork tree alkali, scutelloside etc. will also be removed as impurity, can cause the reduction of finished product drug effect；If not going the removal of impurity, what is largely precipitated deposits
When concentrating extract solution in the pasty state, no mobility, can not carry out drying production in next step.
Patent 200910028029.X discloses extracting method and the application of a kind of coptis detoxifcation decoction active site, the patent
Precipitation caused by being decocted to huanglian jiedu decoction has carried out separation and alcohol extracting processing, and precipitation alcohol extract and huanglian jiedu decoction are extracted
Liquid medicinal extract merges, and turns into coptis detoxifcation decoction active site.Although the method enables the active ingredient maximum limit of huanglian jiedu decoction
The reservation of degree, but this method is cumbersome, complex procedures, time-consuming, during used ethanol, be not used in big production, be only limitted to
Laboratory test.Therefore, being badly in need of one kind can solve the problems, such as to produce precipitation during huanglian jiedu decoction decoction, and and can is widely used in
The method produced greatly.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, it is an object of the invention to provide a kind of huanglian jiedu decoction granule
Preparation method and its method of quality control, the preparation method can effectively solve huanglian jiedu decoction medicinal extract concentration when produce precipitation
Problem, retain the active ingredient in raw material to greatest extent, can be widely applied in big production；The method of quality control is simple,
Comprehensively, the quality of produced huanglian jiedu decoction granule can be effectively controlled, available in daily Quality Control work.
The present invention is to be achieved through the following technical solutions；
A kind of preparation method of huanglian jiedu decoction granule, comprises the following steps：
A, the coptis, radix scutellariae, golden cypress, cape jasmine totally four taste medicine materical crude slice are taken, the mass ratio of four taste medicine materical crude slice is 1 ~ 2:0.5~1:1~2:0.5
~ 2, preferably 1.5:1:1:1.5, add water to cook twice, add the water of 5 ~ 15 times of amounts of inventory every time, decoct 0.5 ~ 2 hour, merge
Filtrate, filtration；
B, filter vacuum is concentrated under reduced pressure into the medicinal extract that the relative density under the conditions of 95 DEG C is 1.03 ~ 1.06, adds β-ring paste
Essence, it is sufficiently stirred, mixes to obtain clear cream；
C, take above-mentioned clear cream to be spray-dried, obtain dry extract, dry extract dry granulation obtains granularity in 16~40 mesh
Huanglian jiedu decoction granule.
Preferably, in above-mentioned steps b, the addition of beta-schardinger dextrin is 0.5 ~ 1 with the mass ratio of medicinal extract solid content:1, it is excellent
Elect 0.78 as:1.
In upper step b, the temperature of vacuum-concentrcted is 80 DEG C ~ 95 DEG C.
In above-mentioned steps b, when adding beta-schardinger dextrin, the temperature of medicinal extract is maintained at 60 DEG C ~ 100 DEG C, preferably 90 DEG C ~ 100 DEG C.
Because of beta-schardinger dextrin, solubility is very low at normal temperatures, with the rise of temperature, solubility rise, through repetition test, 90 DEG C ~ 100
DEG C when add effect it is best.
In above-mentioned steps c, the technological parameter of the spray drying is：Control 175 DEG C ~ 185 DEG C of EAT, leaving air temp
85℃~95℃。
In above-mentioned steps c, appropriate amount of auxiliary materials such as maltodextrin can be added according to actual conditions when being spray-dried, do leaching
Cream powder can also add after appropriate maltodextrin dry granulation again.
Beta-schardinger dextrin (β-Cyclodextrin) be by 7 glucose molecules continuously into cyclic structure compound, main body
There are cavity, the cylinder that both ends are not closed among configuration picture.In empty structure, due to the shielding work by C-H keys in cavity
With hydrophobic region is formd, openend has hydrophily.Beta-schardinger dextrin cavity size is moderate, and Binding ability is strong, can quilt in human body
Absorb, decompose, it is safe to the human body nontoxic, and can largely produce, material is included as new medicine, is obtained in recent years
Rapid development, is widely used in Chinese medicine preparation, has increase solubility and dissolution rate；Make liquid medicine powdered, prevent
Only volatilize；Cover bad stink, reduce excitant；Improve stability；Adjust drug release rate, target administration；Improve biological utilisation
The multiple actions such as degree.
A kind of method of quality control of the huanglian jiedu decoction granule prepared present invention also offers above-mentioned preparation method,
Including the one or more in following methods：
（1）Huanglian jiedu decoction granule 0.5g made from above-mentioned preparation method is taken, it is finely ground, add methanol 50ml, at ultrasound
Reason 30 minutes, filtration, filtrate is as need testing solution.Berberine hydrochloride reference substance separately is taken, adds methanol that every lml is made and contains 0.5mg
Solution, as reference substance solution.The coptis and each 0.5g of golden cypress control medicinal material are taken again, respectively adds water 50ml, are decocted 30 minutes, filter
Cross, filtrate is evaporated, and residue adds methanol 10ml to make dissolving, takes supernatant as control medicinal material solution.According to thin-layered chromatography（Middle traditional Chinese medicines
One B of annex VI of allusion quotation version in 2010）Experiment, it is molten to draw above-mentioned μ l of need testing solution 3, μ l of reference substance solution 2, coptis control medicinal material
μ l of liquid 1, the μ l of golden cypress control medicinal material solution 7, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-methanol-isopropyl
Alcohol-strong ammonia solution（6：3：1.5：1.5：0.5）For solvent, deploy, take out, dry, put ultraviolet lamp（365 nm）Under inspect.
In test sample chromatogram, on position corresponding with reference substance chromatogram and control medicinal material chromatogram, show the fluorescence spot of same color.
（2）Huanglian jiedu decoction granule 0.5g made from above-mentioned preparation method is taken, it is finely ground, add methanol 50ml, at ultrasound
Reason 30 minutes, filtration, filtrate is as need testing solution；Gardenoside reference substance is taken, adds methanol that solution of every 1ml containing 4mg is made, is made
For reference substance solution.Cape jasmine control medicinal material 0.5g separately is taken, adds water 50ml, is decocted 30 minutes, filtration, filtrate is evaporated, and residue adds first
Alcohol 10ml makes dissolving, and supernatant is as control medicinal material solution.According to thin-layered chromatography（One B of annex VI of Chinese Pharmacopoeia version in 2010）
Experiment, μ l of need testing solution 15, μ l of reference substance solution 2, the μ l of control medicinal material solution 5 are drawn, is put respectively in same silica gel g thin-layer plate
On, with ethyl acetate-acetone-formic acid-water（5：5：1：1）For solvent, deploy, take out, dry, spray molten with 10% sulfuric acid ethanol
Liquid, it is clear to be heated to spot development at 105 DEG C.In test sample chromatogram, in position corresponding with reference substance and control medicinal material chromatogram
On, the spot of aobvious same color.
（3）Huanglian jiedu decoction granule 1g made from above-mentioned preparation method is taken, it is finely ground, add acetate-methanol（3：1）
40ml, it is heated to reflux 30 minutes, filters, filtrate is evaporated, and residue adds methanol 10ml to make dissolving, takes supernatant molten as test sample
Liquid.Wogonin reference substance separately is taken, adds methanol that solution of every 1ml containing 0.5mg is made, as reference substance solution.Radix scutellariae pair is taken again
According to medicinal material 0.5g, add water 50ml, decoct 30 minutes, filtration, filtrate is evaporated, and residue adds acetate-methanol（3：1）40ml, add
Heat backflow 30 minutes, filtration, residue adds methanol 5ml to make dissolving, takes supernatant as control medicinal material solution.According to thin-layered chromatography
（One B of annex VI of Chinese Pharmacopoeia version in 2010）Experiment, draws above-mentioned μ l of need testing solution 20, μ l of reference substance solution 5, comparison medicine
The μ l of material solution 15, put respectively on same polyamide film, with benzene-acetate-methanol-formic acid（10：3：1：1）For expansion
Agent, deploy, take out, dry, spray with 1% ferric trichloride ethanol solution.In test sample chromatogram, with reference substance and comparison medicine wood color
Compose on corresponding position, show the spot of same color.
（4）The assay of huanglian jiedu decoction granule, it is as follows using high performance liquid chromatography, method：
Chromatographic condition is with system suitability using octadecylsilane chemically bonded silica as filler；Using acetonitrile as flowing
Phase A, using acetic acid-ammonium acetate buffer solution of pH containing 1ml=6.0 in every 100ml water as Mobile phase B, binary gradient elutes；Detection
Wavelength is 260nm, and number of theoretical plate is calculated by Berberine hydrochloride peak should be not less than 5000.
The preparation of reference substance solution takes Gardenoside, scutelloside, palmatin hydrochloride, Berberine hydrochloride reference substance appropriate, accurate
It is weighed, add methanol that every 1ml is respectively prepared containing μ g of Gardenoside 100, μ g of scutelloside 80, μ g of palmatin hydrochloride 10, Berberine hydrochloride 100
μ g solution, is produced.
The preparation of need testing solution takes granule 0.3g made from above-mentioned preparation method, finely ground, accurately weighed, puts tool
Fill in conical flask, precision adds methanol 50ml, close plug, weighed weight, is ultrasonically treated（Power 200W, frequency 25kHz）30 minutes,
Let cool, then weighed weight, the weight of less loss is supplied with methanol, is shaken up, filters, takes subsequent filtrate, precision measures subsequent filtrate 5ml extremely
In 25ml volumetric flasks, methanol constant volume, shake up, produce.
Determination method difference is accurate to draw reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, determines,
Produce;
The every 1 gram of particle of this product contains cape jasmine in terms of Gardenoside, containing radix scutellariae in terms of scutelloside, containing the coptis and golden cypress with hydrochloric acid bar horse
Spit of fland and Berberine hydrochloride meter, must not distinguish and be less than 30mg, 50mg, 5mg, 50mg.
The present invention compared with prior art, has the advantages that：
（1）Huanglian jiedu decoction granule is during water boiling and extraction, alkaloid component and radix scutellariae in the coptis, golden cypress
In flavone component can produce water insoluble active ingredient, form flocculent deposit, when further concentrating, clear cream is in semi-solid pasty state, nothing
Mobility, the production of next step can not be carried out.The present invention adds appropriate beta-schardinger dextrin when huanglian jiedu decoction medicinal extract concentrates, and fills
Divide stirring, you can the clear cream of semi-solid pasty state originally is recovered to liquid, there is mobility, effectively solve huanglian jiedu decoction
The problem of precipitation is produced when medicinal extract concentrates, enables follow-up spray drying to be smoothed out, and solves a great problem in production.
（2）Four medicines are decocted altogether in huanglian jiedu decoction, can produce flocculent deposit, and traditional method is to filter off precipitation, takes supernatant
Concentrated, the subsequent production such as spray drying.But it is the coptis containing compositions such as substantial amounts of jamaicin and scutellosides in caused precipitation
The effective component of Detoxication Decoction, simply precipitation is filtered off, can substantially reduce the huanglian jiedu decoction granule drug effect of production.This
Invention adds a small amount of beta-schardinger dextrin in concentration process and includes caused precipitation, and beta-schardinger dextrin enters and can point after human body
Solution, absorb, remain the active ingredient of huanglian jiedu decoction, the huanglian jiedu decoction granule effect of this method production to greatest extent
Fruit becomes apparent from, curative effect more precisely.
（3）The preparation method of the present invention is easy, quick, and work is extracted again without carrying out complicated precipitation, and added auxiliary material β-
Cyclodextrin is widely used in pharmaceutical industry, into human body after can be decomposed, absorb, safe and non-toxic, this method can be widely applied to
In big production.
（4）The method of quality control of the present invention can comprehensively, effectively control produced huanglian jiedu decoction granule
Quality, this method is simple and feasible, and repeatability is high, available in daily Quality Control detection.
Brief description of the drawings
Fig. 1 is the HPLC chromatogram of reference substance solution in comparative experimental example.
Fig. 2 is the HPLC chromatogram for the centrifuged supernatant that beta-schardinger dextrin is not added with comparative experimental example.
Fig. 3 is the HPLC chromatogram of the centrifuged supernatant after addition beta-schardinger dextrin in comparative experimental example；
Wherein, No. 1 peak is Gardenoside, No. 2 peaks are scutelloside, No. 3 peaks are palmatin hydrochloride, No. 4 peaks are hydrochloric acid barberry
Alkali.
Fig. 4 is the thin-layer chromatogram of embodiment 1, wherein 1 is Berberine hydrochloride reference substance, 2 be the scarce coptis, the Huang of golden cypress
Even Detoxication Decoction granule negative sample, 3-5 are huanglian jiedu decoction granule, and 6 be golden cypress control medicinal material, and 7 be that the coptis compares
Medicinal material.
Fig. 5 is the thin-layer chromatogram of embodiment 2, wherein 1 is Gardenoside reference substance, 2-4 is coptis detoxifcation soup formula
Grain, 5 be cape jasmine control medicinal material, and 6 be the huanglian jiedu decoction granule negative sample for lacking cape jasmine.
Fig. 6 is the thin-layer chromatogram of embodiment 3, wherein 1 is wogonin reference substance, 2-4 is coptis detoxifcation soup formula
Grain, 5 be radix scutellariae control medicinal material, and 6 be the huanglian jiedu decoction granule negative sample for lacking radix scutellariae.
Embodiment
The present invention is further illustrated below by embodiment, following examples are the specific embodiment party of the present invention
Formula, but embodiments of the present invention are not limited by following embodiments.
Embodiment 1：
A, coptis 750g, radix scutellariae 500g, golden cypress 500g, cape jasmine 750g are taken, is added water to cook twice, adds 25kg's for the first time
Water, decoct 1 hour；Second plus 30kg water, are decocted 1.5 hours, merging filtrate, filtration；
B, filter vacuum is concentrated under reduced pressure into the medicinal extract that the relative density under the conditions of 95 DEG C is 1.04, and now medicinal extract occurs a large amount of
Precipitation, 351g beta-schardinger dextrins are added, medicinal extract is maintained at 95 DEG C, is sufficiently stirred, and mixes to obtain clear cream；
C, above-mentioned clear cream is taken, addition maltodextrin is appropriate, spray drying, controls 175 DEG C ~ 185 DEG C of EAT, goes out wind-warm syndrome
85 DEG C ~ 95 DEG C of degree, obtains dry extract, and it is appropriate to add maltodextrin, total mixed, carries out dry granulation, and granularity is finally made 16
~40 mesh scopes, the particle of uniform color.
After preparation, thin-layer qualitative discriminating is carried out to granule, specific method is as follows：
The said goods 0.5g is taken, it is finely ground, add methanol 50ml, be ultrasonically treated 30 minutes, filtration, filtrate is molten as test sample
Liquid.Berberine hydrochloride reference substance separately is taken, adds methanol that solution of every lml containing 0.5mg is made, as reference substance solution.The coptis is taken again
And each 0.5g of golden cypress control medicinal material, respectively plus water 50ml, decoction 30 minutes, filtration, filtrate are evaporated, and it is molten that residue adds methanol 10ml to make
Solution, supernatant is as control medicinal material solution.According to thin-layered chromatography（One B of annex VI of Chinese Pharmacopoeia version in 2010）Experiment, draw
Above-mentioned μ l of need testing solution 3, μ l of reference substance solution 2, μ l of coptis control medicinal material solution 1, the μ l of golden cypress control medicinal material solution 7, respectively
Point is on same silica gel g thin-layer plate, with toluene-ethyl acetate-methanol-isopropanol-strong ammonia solution（6：3：1.5：1.5：0.5）For
Solvent, deploy, take out, dry, put ultraviolet lamp（365 nm）Under inspect.As shown in figure 4, in test sample chromatogram, with it is right
According in product chromatogram and the corresponding position of control medicinal material chromatogram, show the fluorescence spot of same color.
Embodiment 2：
A, coptis 450g, radix scutellariae 300g, golden cypress 300g, cape jasmine 450g are taken, is added water to cook twice, adds 15kg's for the first time
Water, decoct 1.5 hours；Second plus 12kg water, are decocted 1 hour, merging filtrate, filtration；
B, filter vacuum is concentrated under reduced pressure into the medicinal extract that the relative density under the conditions of 95 DEG C is 1.05, and now medicinal extract occurs a large amount of
Precipitation, 210g beta-schardinger dextrins are added, medicinal extract is maintained at 100 DEG C, is sufficiently stirred, and mixes to obtain clear cream；
C, above-mentioned clear cream is taken, addition maltodextrin is appropriate, spray drying, controls 175 DEG C ~ 185 DEG C of EAT, goes out wind-warm syndrome
85 DEG C ~ 95 DEG C of degree, obtains dry extract, and it is appropriate to add maltodextrin, total mixed, carries out dry granulation, and granularity is finally made 16
~40 mesh scopes, the particle of uniform color.
After preparation, thin-layer qualitative discriminating is carried out to granule, specific method is as follows：
The said goods 0.5g is taken, it is finely ground, add methanol 50ml, be ultrasonically treated 30 minutes, filtration, filtrate is molten as test sample
Liquid.Gardenoside reference substance is taken, adds methanol that solution of every 1ml containing 4mg is made, as reference substance solution.Separately take cape jasmine control medicinal material
0.5g, add water 50ml, decoct 30 minutes, filtration, filtrate is evaporated, and residue adds methanol 10ml to make dissolving, and supernatant is as comparison medicine
Material solution.According to thin-layered chromatography（One B of annex VI of Chinese Pharmacopoeia version in 2010）Experiment, draw above-mentioned μ l of need testing solution 15,
μ l of reference substance solution 2, the μ l of control medicinal material solution 5, put respectively on same silica gel g thin-layer plate, with ethyl acetate-acetone-formic acid-
Water（5：5：1：1）For solvent, deploy, take out, dry, spray with 10% ethanol solution of sulfuric acid, spot development is heated at 105 DEG C
Clearly.As shown in figure 5, in test sample chromatogram, on position corresponding with reference substance and control medicinal material chromatogram, show same color
Spot.
Embodiment 3：
A, coptis 900g, radix scutellariae 600g, golden cypress 600g, cape jasmine 900g are taken, is added water to cook twice, adds 24kg's for the first time
Water, decoct 2 hours；Second plus 36kg water, are decocted 1.5 hours, merging filtrate, filtration；
B, filter vacuum is concentrated under reduced pressure into the medicinal extract that the relative density under the conditions of 95 DEG C is 1.03, and now medicinal extract occurs a large amount of
Precipitation, 421g beta-schardinger dextrins are added, medicinal extract is maintained at 90 DEG C, is sufficiently stirred, and mixes to obtain clear cream；
C, above-mentioned clear cream is taken, addition maltodextrin is appropriate, spray drying, controls 175 DEG C ~ 185 DEG C of EAT, goes out wind-warm syndrome
85 DEG C ~ 95 DEG C of degree, obtains dry extract, and it is appropriate to add maltodextrin, total mixed, carries out dry granulation, and granularity is finally made 16
~40 mesh scopes, the particle of uniform color.
After preparation, thin-layer qualitative discriminating is carried out to granule, specific method is as follows：
Product 1g of the present invention is taken, it is finely ground, add acetate-methanol（3：1）40ml, it is heated to reflux 30 minutes, filters, filtrate
It is evaporated, residue adds methanol 10ml to make dissolving, takes supernatant as need testing solution.Wogonin reference substance separately is taken, adds methanol system
Into solution of every 1ml containing 0.5mg, as reference substance solution.Radix scutellariae control medicinal material 0.5g is taken again, adds water 50ml, is decocted 30 minutes,
Filtration, filtrate are evaporated, and residue adds acetate-methanol（3：1）40ml, it is heated to reflux 30 minutes, filters, residue adds methanol 5ml
Make dissolving, take supernatant as control medicinal material solution.According to thin-layered chromatography（One B of annex VI of Chinese Pharmacopoeia version in 2010）Examination
Test, draw above-mentioned μ l of need testing solution 20, μ l of reference substance solution 5, the μ l of control medicinal material solution 15, put respectively thin in same polyamide
On film, with benzene-acetate-methanol-formic acid（10：3：1：1）For solvent, deploy, take out, dry, spray with 1% ferric trichloride
Ethanol solution.As shown in fig. 6, in test sample chromatogram, on position corresponding with reference substance and control medicinal material chromatogram, show identical face
The spot of color.
Embodiment 4：
A, coptis 600g, radix scutellariae 400g, golden cypress 400g, cape jasmine 600g are taken, is added water to cook twice, adds 16kg's for the first time
Water, decoct 1 hour；Second plus 20kg water, are decocted 1.5 hours, merging filtrate, filtration；
B, filter vacuum is concentrated under reduced pressure into the medicinal extract that the relative density under the conditions of 95 DEG C is 1.04, and now medicinal extract occurs a large amount of
Precipitation, 2811g beta-schardinger dextrins are added, medicinal extract is maintained at 95 DEG C, is sufficiently stirred, and mixes to obtain clear cream；
C, above-mentioned clear cream is taken, addition maltodextrin is appropriate, spray drying, controls 175 DEG C ~ 185 DEG C of EAT, goes out wind-warm syndrome
85 DEG C ~ 95 DEG C of degree, obtains dry extract, and it is appropriate to add maltodextrin, total mixed, carries out dry granulation, and granularity is finally made 16
~40 mesh scopes, the particle of uniform color.
After preparation, assay is carried out to granule, it is as follows using high-efficient liquid phase technique, specific method：
Chromatographic condition is with system suitability using octadecylsilane chemically bonded silica as filler；Using acetonitrile as flowing
Phase A, using acetic acid-ammonium acetate buffer solution of pH containing 1ml=6.0 in every 100ml water as Mobile phase B, binary gradient elutes；Detection
Wavelength is 260nm, and number of theoretical plate is calculated by Berberine hydrochloride peak should be not less than 5000.
The preparation of reference substance solution takes Gardenoside, scutelloside, palmatin hydrochloride, Berberine hydrochloride reference substance appropriate, accurate
It is weighed, add methanol that every 1ml is respectively prepared containing μ g of Gardenoside 100, μ g of scutelloside 80, μ g of palmatin hydrochloride 10, Berberine hydrochloride 100
μ g solution, is produced.
The preparation of need testing solution takes product 0.3g of the present invention, finely ground, accurately weighed, puts in conical flask with cover, and precision adds
Enter methanol 50ml, close plug, weighed weight, be ultrasonically treated（Power 200W, frequency 25kHz）30 minutes, let cool, then weighed weight,
The weight of less loss is supplied with methanol, is shaken up, filters, takes subsequent filtrate, precision measures subsequent filtrate 5ml into 25ml volumetric flasks, methanol
Constant volume, shake up, produce.
Determination method difference is accurate to draw reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, determines,
Produce.
Measure 35.97mg containing Gardenoside, scutelloside 56.72mg, palmatin hydrochloride 8.96mg, hydrochloric acid barberry in every 1g particles
Alkali 54.24mg.
Comparative experimental example：
Filtrate made from the huanglian jiedu decoction granule preparation method step a of Example 1 is appropriate, and vacuum-concentrcted is extremely
Relative density is 1.04 medicinal extract 500ml under the conditions of 95 DEG C, takes two parts, every part of 100ml, 1 part to be not added with auxiliary material from this medicinal extract,
(ratio of auxiliary material amount and solid content is 0.78 to 1 part of addition beta-schardinger dextrin:1), stir, cool down, centrifugation, take supernatant to steam
Distilled water is settled to 100ml, and taking 1ml, water bath method, residue is dissolved with methanol into evaporating dish, and with methanol constant volume to 100ml,
Shake up, as need testing solution；
Reference substance solution is prepared by the reference substance solution preparation method under above-mentioned content assaying method item；
Above-mentioned each 10 μ L of 3 kinds of solution are drawn respectively, are contained according to the content assaying method in above-mentioned method of quality control
It is fixed to measure, and as Figure 1-3, measurement result is as shown in table 1 below for HPLC collection of illustrative plates：
Each component content test result in the centrifuged supernatant of table 1
| The content (mg/mL) of Gardenoside | The content (mg/mL) of scutelloside | The content (mg/mL) of palmatin hydrochloride | Content of berberine hydrochloride (mg/mL) | |
| It is not added with auxiliary material | 4.07 | 0.88 | 0.44 | 0.94 |
| Add beta-schardinger dextrin | 6.92 | 2.11 | 0.99 | 2.53 |
As can be seen from the above table, after adding beta-schardinger dextrin in contrast experiment's example, each active ingredient contains in centrifuged supernatant
Measure significantly raised, illustrate that preparation method of the present invention can retain the active ingredient of huanglian jiedu decoction to greatest extent.
Claims (8)
1. a kind of quality determining method of huanglian jiedu decoction granule, it is characterised in that including following methods：
（1）Huanglian jiedu decoction granule 0.5g is taken, it is finely ground, add methanol 50ml, be ultrasonically treated 30 minutes, filtration, filtrate conduct
Need testing solution；Berberine hydrochloride reference substance separately is taken, adds methanol that solution of every lml containing 0.5mg is made, as reference substance solution；
The coptis and each 0.5g of golden cypress control medicinal material are taken again, and respectively plus water 50ml, decoction 30 minutes, filtration, filtrate are evaporated, and residue adds methanol
10ml makes dissolving, takes supernatant as control medicinal material solution；Tested according to one B of annex VI of Chinese Pharmacopoeia version in 2010, in absorption
μ l of need testing solution 3, μ l of reference substance solution 2, μ l of coptis control medicinal material solution 1, the μ l of golden cypress control medicinal material solution 7 are stated, respectively point
In on same silica gel g thin-layer plate, with toluene-ethyl acetate-methanol-isopropanol-strong ammonia solution 6：3：1.5：1.5：0.5 is exhibition
Agent is opened, is deployed, is taken out, is dried, put and inspected under the nm of ultraviolet lamp 365, in test sample chromatogram, with reference substance chromatogram and compareing
On the corresponding position of medicinal material chromatogram, show the fluorescence spot of same color；
（2）Huanglian jiedu decoction granule 0.5g is taken, it is finely ground, add methanol 50ml, be ultrasonically treated 30 minutes, filtration, filtrate conduct
Need testing solution；Gardenoside reference substance is taken, adds methanol that solution of every 1ml containing 4mg is made, as reference substance solution；Separately take cape jasmine
Control medicinal material 0.5g, add water 50ml, decoct 30 minutes, filtration, filtrate is evaporated, and residue adds methanol 10ml to make dissolving, takes supernatant
As control medicinal material solution；According to Chinese Pharmacopoeia one B of annex VI experiment of version in 2010, μ l of need testing solution 15, reference substance are drawn
μ l of solution 2, the μ l of control medicinal material solution 5, put respectively on same silica gel g thin-layer plate, with ethyl acetate-acetone-formic acid-water 5：
5：1：1 is solvent, is deployed, and takes out, dries, spray with 10% ethanol solution of sulfuric acid, and it is clear to be heated to spot development at 105 DEG C, is supplied
In test product chromatogram, on position corresponding with reference substance and control medicinal material chromatogram, show the spot of same color；
（3）Huanglian jiedu decoction granule 1g is taken, it is finely ground, add 40ml acetate-methanols 3：1, it is heated to reflux 30 minutes, filters
Cross, filtrate is evaporated, and residue adds methanol 10ml to make dissolving, takes supernatant as need testing solution；Wogonin reference substance separately is taken, is added
Solution of every 1ml containing 0.5mg is made in methanol, as reference substance solution；Radix scutellariae control medicinal material 0.5g is taken again, adds water 50ml, is decocted
30 minutes, filtration, filtrate was evaporated, and residue adds 40ml acetate-methanols 3：1, it is heated to reflux 30 minutes, filters, residue adds first
Alcohol 5ml makes dissolving, takes supernatant as control medicinal material solution；Tested according to one B of annex VI of Chinese Pharmacopoeia version in 2010, in absorption
μ l of need testing solution 20, μ l of reference substance solution 5, the μ l of control medicinal material solution 15 are stated, is put respectively on same polyamide film, with
Benzene-acetate-methanol-formic acid 10：3：1：1 is solvent, is deployed, and takes out, dries, spray with 1% ferric trichloride ethanol solution,
In test sample chromatogram, on position corresponding with reference substance and control medicinal material chromatogram, show the spot of same color；
（4）The assay of huanglian jiedu decoction granule, using high performance liquid chromatography, comprise the following steps that：
Chromatographic condition is with system suitability using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase A,
Using acetic acid-ammonium acetate buffer solution of pH containing 1ml=6.0 in every 100ml water as Mobile phase B, binary gradient elutes；Detection wavelength
For 260nm, number of theoretical plate is calculated by Berberine hydrochloride peak should be not less than 5000；
The preparation of reference substance solution takes Gardenoside, scutelloside, palmatin hydrochloride, Berberine hydrochloride reference substance appropriate, and precision claims
It is fixed, add methanol that every 1ml is respectively prepared containing μ g of Gardenoside 100, μ g of scutelloside 80, μ g of palmatin hydrochloride 10, the μ g of Berberine hydrochloride 100
Solution, produce；
The preparation of need testing solution takes huanglian jiedu decoction granule 0.3g, finely ground, accurately weighed, puts in conical flask with cover, essence
Close addition methanol 50ml, close plug, weighed weight, it is ultrasonically treated 30 minutes, lets cool, then weighed weight, supply less loss with methanol
Weight, shake up, filter, take subsequent filtrate, precision measures subsequent filtrate 5ml into 25ml volumetric flasks, methanol constant volume, shakes up, produce；
Determination method is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, measure, produces；
The every 1 gram of particle of this product containing cape jasmine in terms of Gardenoside, containing radix scutellariae in terms of scutelloside, containing the coptis and golden cypress with palmatin hydrochloride and
Berberine hydrochloride meter, must not distinguish and be less than 30mg, 50mg, 5mg, 50mg.
2. the quality determining method of huanglian jiedu decoction granule according to claim 1, it is characterised in that the coptis
The preparation method of Detoxication Decoction granule, comprises the following steps：
A, the coptis, radix scutellariae, golden cypress, cape jasmine totally four taste medicine materical crude slice are taken, the mass ratio of four taste medicine materical crude slice is 1 ~ 2:0.5~1:1~2:0.5 ~ 2,
Add water to cook twice, add the water of 5 ~ 15 times of amounts of inventory every time, decoct 0.5 ~ 2 hour, merging filtrate, filtration；
B, filter vacuum is concentrated under reduced pressure into the medicinal extract that the relative density under the conditions of 95 DEG C is 1.03 ~ 1.06, adds beta-schardinger dextrin, fills
Divide stirring, mix to obtain clear cream；In step b, the addition and the mass ratio of medicinal extract solid content of beta-schardinger dextrin are：0.5~1:1；
C, take above-mentioned clear cream to be spray-dried, obtain dry extract, dry extract dry granulation obtains Huang of the granularity in 16~40 mesh
Even Detoxication Decoction granule.
3. the quality determining method of huanglian jiedu decoction granule according to claim 2, it is characterised in that in step a,
The mass ratio of four taste medicine materical crude slice is 1.5:1:1:1.5.
4. the quality determining method of huanglian jiedu decoction granule according to claim 2, it is characterised in that in step b,
The addition of beta-schardinger dextrin is 0.78 with the mass ratio of medicinal extract solid content:1.
5. the quality determining method of huanglian jiedu decoction granule according to claim 2, it is characterised in that in step b,
The temperature of vacuum-concentrcted is 80 DEG C ~ 95 DEG C.
6. the quality determining method of huanglian jiedu decoction granule according to claim 2, it is characterised in that in step b,
When adding beta-schardinger dextrin, the temperature of medicinal extract is maintained at 60 DEG C ~ 100 DEG C.
7. the quality determining method of huanglian jiedu decoction granule according to claim 6, it is characterised in that in step b,
When adding beta-schardinger dextrin, the temperature of medicinal extract is maintained at 90 DEG C ~ 100 DEG C.
8. the quality determining method of huanglian jiedu decoction granule according to claim 2, it is characterised in that in step c,
The technological parameter of the spray drying is：Control 175 DEG C ~ 185 DEG C of EAT, 85 DEG C ~ 95 DEG C of leaving air temp.
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