CN105168390A - Anti-inflammation and detoxification preparation as well as preparation method and quality control method - Google Patents
Anti-inflammation and detoxification preparation as well as preparation method and quality control method Download PDFInfo
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Abstract
The invention provides an anti-inflammation and detoxification preparation. The preparation mainly refers to tablets and is prepared from the following components in parts by weight: 1100 to 1300 parts of common andrographis herb, 900 to 1100 parts of Chinese knotweed herb, 700 to 900 parts of wikstroemia indica, 900 to 1100 parts of jasminum elongatum, 300 to 360 parts of pomegranate bark, 300 to 360 parts of plantain herb and 640 to 700 parts of ilex rotunda thunb. The anti-inflammation and detoxification preparation provided by the invention has remarkable curative effects on phlegm-heat cough and asthma, acute and chronic tonsillitis, sphagitis, pulmonitis, stomachache, diarrhea, vomit, acute gastroenteritis and acute bacillary dysentery. The invention also provides a preparation method of the anti-inflammation and detoxification preparation. The tablets prepared by using the preparation method are high in purity of active ingredients and prone to mechanical and automatic production. The invention also provides a quality control method for the anti-inflammation and detoxification preparation. The anti-inflammation and detoxification preparation is a pure traditional Chinese medicine preparation, is accurate in dosage, stable in product quality, convenient to take, safe and free of toxic and side effects and has relatively strong competitive power in terms of product cost and brand effect on the market; the cost is reduced and the product quality is ensured.
Description
Technical field
The present invention relates to traditional Chinese medicine preparation, refer to a kind of 'Xiaoyanjiedu ' and preparation method and method of quality control especially, belong to technical field of traditional Chinese medicine pharmacy.
Background technology
'Xiaoyanjiedu ' is mainly used in that expectorant heat syndrome cough is breathed heavily, acute and chronic tonsillitis, pharyngolaryngitis, pneumonia, stomachache, diarrhoea, vomiting, acute gastroenteritis, acute bacillary dysentery has significant curative effect, wherein " andrographis tablet " is on the books in Chinese Pharmacopoeia version one in 2010, but this product is single component, Chinese medical theory " monarch, minister, help, make " effect cannot be played well, for this reason, provide a kind of 'Xiaoyanjiedu ' with Chinese medicine effect to necessitate.
Summary of the invention
The object of the invention is to: provide one and treat that expectorant heat syndrome cough is breathed heavily, acute and chronic tonsillitis, pharyngolaryngitis, pneumonia, stomachache, diarrhoea, vomiting, acute gastroenteritis, acute bacillary dysentery has the 'Xiaoyanjiedu ' of significant curative effect, and said preparation exists; This preparation mainly refers to tablet: this preparation method is for the difference of medical material dissolubility, adopt alcohol extraction, water extraction to combine, refine process, belt rapid draing of reducing pressure adds the method for adjuvant pelletizing press sheet again, the tablet made greatly remains active component content, production cost can be reduced, reduce industrial energy consumption, there is taking convenience, workinprocess cost and market brand effect have the stronger mistake market competitiveness; Present invention also offers a kind of method of quality control of 'Xiaoyanjiedu ', this quality control side's products quality guarantee.
In order to realize technique scheme, the invention provides a kind of 'Xiaoyanjiedu ', (unit: weight portion) composed of the following components:
Herba Andrographis 1100 ~ 1300
Herb Polygoni Chinensis 900 ~ 1100
Radix Wikstroemae 700 ~ 900
Herba Oxalidis strictae 900 ~ 1100
Pericarpium Granati 300 ~ 360
Herba Plantaginis 300 ~ 360
Cortex Ilicis Rotundae 640 ~ 700.
By above formula, the invention additionally provides a kind of preparation method of 'Xiaoyanjiedu ', (unit: weight portion):
Step 1, Herba Andrographis extracts: 1100 ~ 1300 parts of Herba Andrographis are broken into 40 order coarse powder, and adding concentration is that 85% ethanol is heated to 70 ~ 80 DEG C, lixiviate secondary, each 2 hours, then extracting solution is condensed into the creat extract of relative density 1.30 ~ 1.40;
Step 2, Radix Wikstroemae extracts; By 700 ~ 900 parts of Radix Wikstroemae extracting in water secondaries, each 5 hours, then Radix Wikstroemae extractum extracting solution being condensed into relative density 1.30 ~ 1.40;
Step 3, Herba Oxalidis strictae, Pericarpium Granati, Herba Plantaginis, Herb Polygoni Chinensis, Cortex Ilicis Rotundae extract; By Herba Oxalidis strictae 900 ~ 1100 parts, Pericarpium Granati 300 ~ 360 parts, Herba Plantaginis 300 ~ 360 parts, Herb Polygoni Chinensis 900 ~ 1100 parts, Cortex Ilicis Rotundae 640 ~ 700 parts mixing, add water and extract secondary in right amount, each 2 hours, adding concentration is 65% ethanol, purification secondary, then mixing extractum extracting solution being condensed into relative density 1.30 ~ 1.40;
Step 4: creat extract, Radix Wikstroemae extractum and mixing extractum are blended in and put in band drier, drying under reduced pressure becomes dry extract at 50 DEG C ~ 70 DEG C;
Step 5: dry extract is broken into 100 ~ 120 object fine powders;
Step 6: fine powder 75% ethanol is made wet granular, then wet grain drying is become dry granule,
Add disintegrating agent and lubricant, dry granule, disintegrating agent, lubricant are pressed 100:1:5 mixing, tabletted, obtained 'Xiaoyanjiedu '.
Disintegrating agent described in step 6 is carboxymethyl starch sodium, and lubricant is magnesium stearate.
Wherein, step 1,2, the preparation process of 3 is preparation process arranged side by side.
Present invention also offers a kind of method of quality control of 'Xiaoyanjiedu ', effective property of medicine composition of medicine can effectively be identified and ensure to the method.
Comprise discriminating project to detect and content detection,
Discriminating project detects and comprises the detection of Herba Andrographis medical material, the detection of Radix Wikstroemae medical material and the detection of Herba Oxalidis strictae medical material,
Content detection comprises rutin content in Herba Andrographis medical material content detection and preparation and detects.
Particularly, (1) Herba Andrographis medical material detects: get tablet 2-3g, porphyrize, add chloroform 20ml, supersound process 15 minutes, and filter, filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution,
Get Herba Andrographis control medicinal material 1g, add methanol 10ml, supersound process 15 minutes, filter, filtrate is medical material solution in contrast,
Get dehydrorographolide reference substance appropriate, add methanol and make the solution of every 1ml containing 1mg, product solution in contrast,
Test according to thin layer chromatography (Chinese Pharmacopoeia version in 2010 annex VIB), draw above-mentioned need testing solution 4 ~ 10 μ l, control medicinal material solution 5 μ l, reference substance solution 4 μ l, put respectively on same silica GF254 lamellae, with chloroform-acetate-methanol (4:3:0.4) for developing solvent, launch, take out, dry; Inspect under putting ultra-violet lamp (254nm); In test sample chromatograph, on the position corresponding with reference substance chromatograph to control medicinal material chromatograph, the speckle of aobvious same color, quality conforms with the regulations.
(2) Radix Wikstroemae medical material detects: get tablet 2-3g, porphyrize, add methanol 20ml, supersound process 15 minutes, and filter, get filtrate 10ml, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution,
Get Radix Wikstroemae control medicinal material 1g, decoct with water 30 minutes, filter, filtrate evaporate to dryness, residue adds methanol 4ml makes dissolving, medical material solution in contrast,
According to thin layer chromatography (Chinese Pharmacopoeia version in 2010 annex VIB) test, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid (5:4:1) for developing solvent, launch, take out, dry.Inspect under putting ultra-violet lamp (365nm).In test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious same color, quality conforms with the regulations;
(3) Herba Oxalidis strictae medical material detects: get tablet 2-3g, porphyrize, add methanol 30ml, reflux 30 minutes, filters, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, 2 times are extracted, each 20ml, combined ethyl acetate with ethyl acetate jolting, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution
Separately get Herba Oxalidis strictae control medicinal material 1g, the 50ml that adds water decocts 30 minutes, and filter, filtrate is concentrated into 20ml, is made in the same way of control medicinal material solution,
Test according to thin layer chromatography (Chinese Pharmacopoeia version in 2010 annex VIB), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-formic acid (10: 4: 1) for developing solvent launches, take out, dry, inspect under putting ultra-violet lamp (365nm).In test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious same color, quality conforms with the regulations;
Effective property of medicine component content of medicine is sanatory most important product quality index, for being the upper den of monsters performance figure of guarantee, the invention provides a kind of method of quality control of 'Xiaoyanjiedu ', wherein assay:
(1) Herba Andrographis medical material content detection: measure according to high performance liquid chromatography standard operating procedure:
Chromatographic column: KromasilC
18(octadecylsilane chemically bonded silica); Methanol-water (55:45) is mobile phase; Determined wavelength is 250nm; Theoretical cam curve calculates should be not less than 4000 by dehydrorographolide peak;
Get dehydrorographolide reference substance, it is appropriate that precision takes dehydrorographolide reference substance, adds 60% methanol and make every 1ml containing 15 μ g; Get the tablet 4-6g under content uniformity item, accurately weighed, porphyrize, get about 0.5g, accurately weighed, put in 100ml measuring bottle, add 60% methanol 90ml, ultrasonic (power 250W, frequency 33kHz) process 30 minutes, let cool, add 60% methanol dilution to scale, microporous filter membrane (0.45 μm) filters, and gets subsequent filtrate and uses; Accurate absorption reference substance solution and each 20 μ l of need testing solution respectively, injection liquid chromatography, measures Determination of Dehydroandrographoliin, and in said preparation, every sheet in dehydrorographolide (C42H62O16), must not be less than 0.30mg containing Herba Andrographis.
(2) in preparation, rutin content detects:
According to spectrophotometry: get awns fourth reference substance, precision takes at 120 DEG C of drying under reduced pressure appropriate to the control substance of Rutin of constant weight, adds 60% ethanol and makes the solution of every 1ml containing 0.1mg;
Preparation standard curve: precision measures reference substance solution 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, put in 25ml measuring bottle respectively, respectively add 10% sodium nitrite solution 0.3ml, mixing, places 6 minutes, add 10% aluminum nitrate solution 0.3ml, mixing, places 6 minutes, add 4% sodium hydroxide solution 4ml, shake up, add 30% ethanol to scale, shake up, place 15 minutes; With corresponding solution for blank;
Measure trap at 510nm wavelength place, take trap as vertical coordinate, concentration is abscissa, drawing standard curve; Get the tablet 4-6g under content uniformity item, accurately weighed, porphyrize, gets 0.2g, put in round-bottomed flask, add methanol 25ml, shake up, reflux 1 hour, take out, be cooled to room temperature, filter, filter paper adds methanol 25ml again together with residue, reflux 1 hour, takes out, and cooling filters, merging filtrate, residue methanol 15ml gradation washing, washing liquid and filtrate merge, evaporate to dryness, residue adds 60% alcoholic solution makes dissolving, to be transferred in 50ml measuring bottle and to be diluted to scale, shaking up;
Precision measures 1ml, method under sighting target directrix curve preparation, from " putting respectively in 25ml measuring bottle ", measure trap in accordance with the law, read the weight of rutin in need testing solution from standard curve, calculate rutin content, in said preparation, every sheet in rutin (C27H30O16), must not be less than 10.0mg containing total flavones.
Preparation method and the method for quality control that present invention also offers this 'Xiaoyanjiedu ' provided by the invention.Said preparation is made up of the extract of Herba Andrographis, Herb Polygoni Chinensis, Radix Wikstroemae, Herba Oxalidis strictae, Pericarpium Granati, Herba Plantaginis, Cortex Ilicis Rotundae seven taste Chinese crude drug, has eliminating inflammation and expelling toxin, clearing away heat-damp and promoting diuresis, convergence analgesic effect.Be mainly used in expectorant heat syndrome cough to breathe heavily, acute and chronic tonsillitis, pharyngolaryngitis, pneumonia, stomachache, diarrhoea, vomiting, acute gastroenteritis, acute bacillary dysentery has significant curative effect, and wherein " andrographis tablet " is on the books in Chinese Pharmacopoeia version one in 2010, but this product is single component, cannot play Chinese medical theory " monarch well, minister, assistant, make " effect, this preparation method, for the difference of medical material dissolubility, adopts alcohol extraction, water extraction combines, alcoholization process, belt decompression rapid draing adds the method for adjuvant pelletizing press sheet again, and the tablet made greatly remains active component content, has formulated and has comprised the detection of Herba Andrographis medical material thin layer, Radix Wikstroemae medical material thin layer detects, Herba Oxalidis strictae medical material thin layer detects and in Herba Andrographis medical material, Determination of Dehydroandrographoliin detects, in preparation, rutin content detects and tablet routine examination project, control effectively, can meet the needs of extensive patients, workinprocess cost and market brand effect also have stronger competitiveness, reduces cost, products quality guarantee tablet quality.
Detailed description of the invention
Be clearly and completely described the technical scheme in the embodiment of the present invention below in conjunction with the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The present invention proposes a kind of 'Xiaoyanjiedu ', this preparation mainly refers to tablet, calculate according to composition by weight, Herba Andrographis 1100 ~ 1300, Herb Polygoni Chinensis 900 ~ 1100, Radix Wikstroemae 700 ~ 900, Herba Oxalidis strictae 900 ~ 1100, Pericarpium Granati 300 ~ 360, Herba Plantaginis 300 ~ 360, Cortex Ilicis Rotundae 640 ~ 700.'Xiaoyanjiedu ' provided by the invention, breathes heavily at expectorant heat syndrome cough, acute and chronic tonsillitis, pharyngolaryngitis, pneumonia, and stomachache, diarrhoea, vomiting, acute gastroenteritis, acute bacillary dysentery has significant curative effect.The invention allows for a kind of preparation method of 'Xiaoyanjiedu ', the tablet active component purity that this preparation method is made is high, is easy to mechanization, automated production.The invention allows for a kind of method of quality control of 'Xiaoyanjiedu ', pure Chinese medicinal preparation, dosage is accurate, constant product quality, taking convenience, safe without toxic side effect workinprocess cost and market brand effect also have stronger competitiveness, reduce cost, products quality guarantee.
The invention provides a kind of 'Xiaoyanjiedu ', (unit: weight portion) composed of the following components:
Herba Andrographis 1100 ~ 1300
Herb Polygoni Chinensis 900 ~ 1100
Radix Wikstroemae 700 ~ 900
Herba Oxalidis strictae 900 ~ 1100
Pericarpium Granati 300 ~ 360
Herba Plantaginis 300 ~ 360
Cortex Ilicis Rotundae 640 ~ 700.
By above formula, the invention additionally provides a kind of preparation method of 'Xiaoyanjiedu ', (unit: weight portion):
Step 1, Herba Andrographis extracts: Herba Andrographis is broken into 40 order coarse powder, adding concentration is that 85% ethanol is heated to 70 ~ 80 DEG C, lixiviate secondary, each 2 hours, then extracting solution is condensed into the creat extract of relative density 1.30 ~ 1.40;
Step 2, Radix Wikstroemae extracts; By Radix Wikstroemae extracting in water secondary, each 5 hours, then Radix Wikstroemae extractum extracting solution being condensed into relative density 1.30 ~ 1.40;
Step 3, Herba Oxalidis strictae, Pericarpium Granati, Herba Plantaginis, Herb Polygoni Chinensis, Cortex Ilicis Rotundae extract; By Herba Oxalidis strictae, Pericarpium Granati, Herba Plantaginis, Herb Polygoni Chinensis, Cortex Ilicis Rotundae mixing, add water and extract secondary in right amount, each 2 hours, adding concentration is 65% ethanol, purification secondary, then mixing extractum extracting solution being condensed into relative density 1.30 ~ 1.40;
Step 4: creat extract, Radix Wikstroemae extractum and mixing extractum are blended in and put in band drier, drying under reduced pressure becomes dry extract at 50 DEG C ~ 70 DEG C;
Step 5: dry extract is broken into 100 ~ 120 object fine powders;
Step 6: fine powder 75% ethanol is made wet granular, then wet grain drying is become dry granule,
Add disintegrating agent and lubricant, dry granule, disintegrating agent, lubricant are pressed 100:1:5 mixing, tabletted, obtained 'Xiaoyanjiedu '.
Disintegrating agent described in step 6 is carboxymethyl starch sodium, and lubricant is magnesium stearate.
Wherein, step 1,2, the preparation process of 3 is preparation process arranged side by side.
Present invention also offers a kind of method of quality control of 'Xiaoyanjiedu ', effective property of medicine composition of medicine can effectively be identified and ensure to the method.
Comprise discriminating project to detect and content detection,
Discriminating project detects and comprises the detection of Herba Andrographis medical material, the detection of Radix Wikstroemae medical material and the detection of Herba Oxalidis strictae medical material,
Content detection comprises rutin content in Herba Andrographis medical material content detection and preparation and detects.
Particularly, (1) Herba Andrographis medical material detects: get tablet 2-3g, porphyrize, add chloroform 20ml, supersound process 15 minutes, and filter, filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution,
Get Herba Andrographis control medicinal material 1g, add methanol 10ml, supersound process 15 minutes, filter, filtrate is medical material solution in contrast,
Get dehydrorographolide reference substance appropriate, add methanol and make the solution of every 1ml containing 1mg, product solution in contrast,
Test according to thin layer chromatography (Chinese Pharmacopoeia version in 2010 annex VIB), draw above-mentioned need testing solution 4 ~ 10 μ l, control medicinal material solution 5 μ l, reference substance solution 4 μ l, put respectively on same silica GF254 lamellae, with chloroform-acetate-methanol (4:3:0.4) for developing solvent, launch, take out, dry; Inspect under putting ultra-violet lamp (254nm); In test sample chromatograph, on the position corresponding with reference substance chromatograph to control medicinal material chromatograph, the speckle of aobvious same color, quality conforms with the regulations.
(2) Radix Wikstroemae medical material detects: get tablet 2-3g, porphyrize, add methanol 20ml, supersound process 15 minutes, and filter, get filtrate 10ml, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution,
Get Radix Wikstroemae control medicinal material 1g, decoct with water 30 minutes, filter, filtrate evaporate to dryness, residue adds methanol 4ml makes dissolving, medical material solution in contrast,
According to thin layer chromatography (Chinese Pharmacopoeia version in 2010 annex VIB) test, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid (5:4:1) for developing solvent, launch, take out, dry.Inspect under putting ultra-violet lamp (365nm).In test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious same color, quality conforms with the regulations;
(3) Herba Oxalidis strictae medical material detects: get tablet 2-3g, porphyrize, add methanol 30ml, reflux 30 minutes, filters, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, 2 times are extracted, each 20ml, combined ethyl acetate with ethyl acetate jolting, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution
Separately get Herba Oxalidis strictae control medicinal material 1g, the 50ml that adds water decocts 30 minutes, and filter, filtrate is concentrated into 20ml, is made in the same way of control medicinal material solution,
Test according to thin layer chromatography (Chinese Pharmacopoeia version in 2010 annex VIB), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-formic acid (10: 4: 1) for developing solvent launches, take out, dry, inspect under putting ultra-violet lamp (365nm).In test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious same color, quality conforms with the regulations;
Effective property of medicine component content of medicine is sanatory most important product quality index, for being the upper den of monsters performance figure of guarantee, the invention provides a kind of method of quality control of 'Xiaoyanjiedu ', wherein assay:
(1) Herba Andrographis medical material content detection: measure according to high performance liquid chromatography standard operating procedure:
Chromatographic column: KromasilC
18(octadecylsilane chemically bonded silica); Methanol-water (55:45) is mobile phase; Determined wavelength is 250nm; Theoretical cam curve calculates should be not less than 4000 by dehydrorographolide peak;
Get dehydrorographolide reference substance, it is appropriate that precision takes dehydrorographolide reference substance, adds 60% methanol and make every 1ml containing 15 μ g; Get the tablet 4-6g under content uniformity item, accurately weighed, porphyrize, get about 0.5g, accurately weighed, put in 100ml measuring bottle, add 60% methanol 90ml, ultrasonic (power 250W, frequency 33kHz) process 30 minutes, let cool, add 60% methanol dilution to scale, microporous filter membrane (0.45 μm) filters, and gets subsequent filtrate and uses; Accurate absorption reference substance solution and each 20 μ l of need testing solution respectively, injection liquid chromatography, measures Determination of Dehydroandrographoliin, and in said preparation, every sheet in dehydrorographolide (C42H62O16), must not be less than 0.30mg containing Herba Andrographis.
(2) in preparation, rutin content detects:
According to spectrophotometry: get awns fourth reference substance, precision takes at 120 DEG C of drying under reduced pressure appropriate to the control substance of Rutin of constant weight, adds 60% ethanol and makes the solution of every 1ml containing 0.1mg;
Preparation standard curve: precision measures reference substance solution 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, put in 25ml measuring bottle respectively, respectively add 10% sodium nitrite solution 0.3ml, mixing, places 6 minutes, add 10% aluminum nitrate solution 0.3ml, mixing, places 6 minutes, add 4% sodium hydroxide solution 4ml, shake up, add 30% ethanol to scale, shake up, place 15 minutes; With corresponding solution for blank;
Measure trap at 510nm wavelength place, take trap as vertical coordinate, concentration is abscissa, drawing standard curve; Get the tablet 4-6g under content uniformity item, accurately weighed, porphyrize, gets 0.2g, put in round-bottomed flask, add methanol 25ml, shake up, reflux 1 hour, take out, be cooled to room temperature, filter, filter paper adds methanol 25ml again together with residue, reflux 1 hour, takes out, and cooling filters, merging filtrate, residue methanol 15ml gradation washing, washing liquid and filtrate merge, evaporate to dryness, residue adds 60% alcoholic solution makes dissolving, to be transferred in 50ml measuring bottle and to be diluted to scale, shaking up;
Precision measures 1ml, method under sighting target directrix curve preparation, from " putting respectively in 25ml measuring bottle ", measure trap in accordance with the law, read the weight of rutin in need testing solution from standard curve, calculate rutin content, in said preparation, every sheet in rutin (C27H30O16), must not be less than 10.0mg containing total flavones.
Applicant carries out pilot scale three batches of process certifications to preparation method of the present invention, and has carried out methodology experimentation to quality standard Herba Andrographis medical material dehydrorographolide and rutin respectively containing reason assay method, and concrete condition is as follows:
one, process certification
In above-mentioned medical material prescription ratio, expand 10 times amount and take above-mentioned medical material totally three parts, verify above-mentioned process conditions, the result sees the following form:
The above results shows: acquired results is consistent with actual production, shows this stable preparation process, quality controllable, and the available above method of large production is produced.
two, Herba Andrographis medical material glue Determination of Andrographolide assay method
2.1 choice of experimental conditions
Adopt the content of joining in rp-hplc determination dehydration Herba Andrographis herein.
2.2 methodological studies and sample tests
2.2.1 instrument: Laballiance high performance liquid chromatograph: LaballianceModel201 type UV-detector; AC-120, AE-163; Electronic balance
2.2.2 reagent: methanol is chromatograph alcohol; Other reagent is analytical pure;
Dehydrorographolide (Nat'l Pharmaceutical & Biological Products Control Institute 0854-9601).
2.2.3 chromatographic condition
Chromatographic column: KromasilC18 (octadecylsilane chemically bonded silica); Mobile phase: methanol-water (55:45); Determined wavelength: 250nm; Column temperature: 35 DEG C; Flow velocity: 1.0ml/min.Under this chromatographic condition, dehydrorographolide and other component all can reach good separation, and negative control chromatograph does not disturb the mensuration of dehydrorographolide.
2.2.4 the preparation of reference substance solution
Get dehydrorographolide reference substance, it is appropriate that precision takes dehydrorographolide reference substance, adds 60% methanol and make every 1ml containing 15 μ g, to obtain final product.
2.2.5 the preparation of need testing solution
Selection mobile phase extracts, and has investigated extraction time, extract 10 respectively, 20,30,45,60min, find to extract 30min.Get tablet 4-6g sheet, porphyrize, get powder 1g, accurately weighed, in 50ml volumetric flask, add mobile phase to nearly scale, supersound extraction 30min, cooling, is diluted to scale with mobile phase, filters, and filtrate filters through microporous filter membrane (0.45 μm) again, gets subsequent filtrate, to obtain final product.
2.2.6 the selection of wavelength
Select 250nm as determined wavelength.
2.2.7 linear relationship
Get reference substance 10mg, accurately weighed, put in 50ml volumetric flask, be diluted to scale with mobile phase.The above-mentioned solution of accurate absorption is mixed with concentration in right amount for being respectively 4.705,9.410,18.82,37.64,56.46,94.10 μ g/ml reference substance solution, each sample introduction 20 μ l, measures peak area, the results are shown in Table 1 by above-mentioned chromatographic condition.Make abscissa (X) with reference substance concentration, peak area obtains equation of linear regression: Y=as vertical coordinate (Y)
-6.78 × 10
3+ 2.272 × 10
4xr=0.9999 shows that dehydrorographolide has good linear relation within the scope of 0.0941 ~ 1.882 μ g, the results are shown in Table 1.
Table 1: linearity curve measurement result
2.2.8 precision test
Get above-mentioned reference substance solution (37.64 μ g/ml), repeat sample introduction 6 times, measure peak area value, RSD < 2%, the results are shown in Table 2.
Table 2: Precision test result
2.2.9 stability test
To get with a collection of need testing solution (lot number: the 1st batch) respectively at 0,1,2,3,4,8,24h sample introduction 20 μ l, measure peak area value, the results are shown in Table 3, RSD < 2%, visible test sample is stable in 24h.
Table 3 stability experiment result
2.2.10 repeatability test
Get with a collection of test sample (lot number: the 1st batch), parallelly take 6 parts, under product assay item, method measures in the same old way, the results are shown in Table 4, RSD% < 2%, and repeatability is good, and method is feasible.
Table 4 repeatability experimental result
2.2.11 recovery test
Adopt application of sample absorption method, get the tablet samples (lot number: the 1st batch) with a collection of known content, add a certain amount of dehydrorographolide reference substance respectively, measure by above-mentioned chromatographic condition, calculate the response rate, the results are shown in Table 5, result shows, this law has the good response rate.
Table 5 determination of recovery rates result
The assay of dehydrorographolide in Herba Andrographis medical material
Get Herba Andrographis medical material 1g, accurately weighed, be placed in 50ml volumetric flask, add the close scale of flowing, supersound process 30min, cooling, is diluted to scale with mobile phase, filters, and filtrate filters through microporous filter membrane (0.45 μm) again, gets subsequent filtrate, to obtain final product.
Measure by above-mentioned chromatographic condition, result is 1.73mg/g.
2.2.12 sample determination
By above-mentioned same totally 10 batches, legal system available test product sample, get reference substance solution and need testing solution 20 μ l respectively, measure peak area by above-mentioned chromatographic condition, calculate content, ten batch sample measurement results are in table 6.
Table 6 sample determination result
Working out of content limit
Herba Andrographis crude drug measurement result Determination of Dehydroandrographoliin is 1.73mg/g, and according to ten batches of measured results, limit is worked out temporarily as the every sheet of this product contains Herba Andrographis in dehydrorographolide (C42H62O16), must not be less than 0.30mg
three, Assaying of Rutin technique study in preparation
The selection of 3.1 experiment conditions
Measure containing the preparation of rutin and the content assaying method of Chinese crude drug with reference to " Chinese Pharmacopoeia " version one in 2010.
3.2 methodological studies and sample tests
Instrument, sample
Ultraviolet-visible spectrophotometer (Shimadzu UV-2550) work station: UVProbe2.33
Sample: a point lot number is the 1st batch, the 2nd batch, the 3rd batch
The preparation precision of reference substance solution takes at 120 DEG C of drying under reduced pressure appropriate to the control substance of Rutin of constant weight, adds 60% ethanol and makes the solution of every 1ml containing 0.1mg, to obtain final product.
The preparation precision of standard curve measures reference substance solution 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, put in 25ml measuring bottle respectively, respectively add 10% sodium nitrite solution 0.3ml, mixing, places 6 minutes, add 10% aluminum nitrate solution 0.3ml, mixing, places 6 minutes, add 4% sodium hydroxide solution 4ml, shake up, add 30% ethanol to scale, shake up, place 15 minutes; With corresponding solution for blank.According to spectrophotography (Chinese Pharmacopoeia version in 2010 annex V A) test, measure trap at 510nm wavelength place, take trap as vertical coordinate, concentration is abscissa, drawing standard curve.Algoscopy.
Get this product under weight differential item, removing coating, porphyrize, gets 0.2g, accurately weighed, put in round-bottomed flask, add methanol 25ml, shake up, reflux 1 hour, takes out, is cooled to room temperature, filters, filter paper adds methanol 25ml again together with residue, reflux 1 hour, takes out, cooling, filter, merging filtrate, residue methanol 15ml gradation washing, washing liquid and filtrate merge, evaporate to dryness, residue adds 60% alcoholic solution makes dissolving, to be transferred in 50ml measuring bottle and to be diluted to scale, shaking up.Precision measures 1ml, method under sighting target directrix curve preparation, from " putting respectively in 25ml measuring bottle ", measures trap in accordance with the law, reads the weight of rutin in need testing solution from standard curve, calculates, to obtain final product.
3.3 linear relationships are investigated precision and are measured reference substance solution 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, put in 25ml measuring bottle respectively, respectively add 10% sodium nitrite solution 0.3ml, mixing, places 6 minutes, add 10% aluminum nitrate solution 0.3ml, mixing, places 6 minutes, add 4% sodium hydroxide solution 4ml, shake up, add 30% ethanol to scale, shake up, place 15 minutes; With corresponding solution for blank.According to spectrophotography (Chinese Pharmacopoeia version in 2010 annex V A) test, measure trap at 510nm wavelength place, take trap as vertical coordinate, concentration is abscissa, drawing standard curve, and measurement result sees the following form 1.
Table 1 linear test result table
Result shows, rutin has good linear relationship at concentration 4.2 μ g/ml ~ 21.0 μ g/ml and trap.
It is appropriate that 3.4 precision test precisions take control substance of Rutin, adds methanol and make every 1ml about containing the solution of 20 μ g, prepare need testing solution, METHOD FOR CONTINUOUS DETERMINATION 6 times, calculate RSD(% by rutin trap by the method under assay item).Measurement result sees the following form 2:
Table 2 Precision test result table
Result shows, precision test RSD is 0.22%, and method precision is good.
It is appropriate that 130401 batch samples are got in 3.5 repeatability tests, prepares need testing solution by the method under assay item, substitutes into linear equation calculate content by trap, and by cubage RSD(%).Measurement result is as following table 3:
Table 3 reproducible test results table
Measurement result, 6 parts of sample sizes are 36.2mg/ sheet ~ 36.6mg/ sheet, and average content is 36.4mg/ sheet, and its RSD is 0.40%, and method repeatability is good.
3.6 method stability test sample thiefs are appropriate, and make need testing solution by method below assay item, separated in time measures its trap, and calculates RSD(%), result is as following table 4:
Table 4 method stability test result table
Result shows, need testing solution recorded trap and stablizes in 4 hours, recording trap and obviously declined, showing that need testing solution should face with now joining after 6 hours.
3.7 recovery tests adopt application of sample absorption method.It is appropriate that precision takes the sample (130401 batches) measuring content, adds control substance of Rutin solution 1ml (1.05mg/ml), add methanol 24ml, reflux 1 hour, take out, be cooled to room temperature, filter, filter paper adds methanol 25ml again together with residue, reflux 1 hour, takes out, cooling, filters, merging filtrate, residue methanol 15ml gradation washing, washing liquid and filtrate merge, evaporate to dryness, residue adds 60% ethanol makes dissolving, to be transferred in 50ml measuring bottle and to be diluted to scale, shaking up.Precision measures 1ml, method under sighting target directrix curve preparation, from " putting respectively in 25ml measuring bottle ", measures trap in accordance with the law, substitutes into linear equation, and calculate the content of rutin in need testing solution, and calculate the response rate, measurement result sees the following form 5:
Table 5 recovery test result table
Result shows, this Assay recovery is 97.71% ~ 100.86%, and average recovery rate is 99.54%, RSD is 1.28%, and the response rate is good.
3.8 negative interference tests get scarce Herba Oxalidis strictae negative control sample, extract by the method under need testing solution preparation, measure.Result negative control sample goes out peak position without absworption peak rutin, and show that in prescription, other compositions are noiseless to mensuration, analysis condition specificity is strong.
3.9, the assay of sample gets this product under weight differential item, removing coating, porphyrize, get 0.2g, accurately weighed, put in round-bottomed flask, add methanol 25ml, shake up, reflux 1 hour, take out, be cooled to room temperature, filter, filter paper adds methanol 25ml again together with residue, reflux 1 hour, takes out, cooling, filter, merging filtrate, residue methanol 15ml gradation washing, washing liquid and filtrate merge, evaporate to dryness, residue adds 60% alcoholic solution makes dissolving, to be transferred in 50ml measuring bottle and to be diluted to scale, shaking up.Precision measures 1ml, method under sighting target directrix curve preparation, from " putting respectively in 25ml measuring bottle ", measures trap in accordance with the law, reads the weight of rutin in need testing solution from standard curve, calculates, to obtain final product.Measurement result sees the following form 6:
Table 6 sample size measurement result
As a result, the every sheet of three batch samples contains total flavones in rutin (C27H30O16) content at 36.2mg/ sheet ~ 36.5mg/ sheet, and determining standard limits is: the every sheet of this product in rutin (C27H30O16), must not be less than 10.0mg containing total flavones.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. a 'Xiaoyanjiedu ', is characterized in that, (unit: weight portion) composed of the following components:
Herba Andrographis 1100 ~ 1300
Herb Polygoni Chinensis 900 ~ 1100
Radix Wikstroemae 700 ~ 900
Herba Oxalidis strictae 900 ~ 1100
Pericarpium Granati 300 ~ 360
Herba Plantaginis 300 ~ 360
Cortex Ilicis Rotundae 640 ~ 700.
2. the preparation method of a kind of 'Xiaoyanjiedu ' according to claim 1, is characterized in that (unit: weight portion):
Step 1, Herba Andrographis extracts: 1100 ~ 1300 parts of Herba Andrographis are broken into 40 order coarse powder, and adding concentration is that 85% ethanol is heated to 70 ~ 80 DEG C, lixiviate secondary, each 2 hours, then extracting solution is condensed into the creat extract of relative density 1.30 ~ 1.40;
Step 2, Radix Wikstroemae extracts; By 700 ~ 900 parts of Radix Wikstroemae extracting in water secondaries, each 5 hours, then Radix Wikstroemae extractum extracting solution being condensed into relative density 1.30 ~ 1.40;
Step 3, Herba Oxalidis strictae, Pericarpium Granati, Herba Plantaginis, Herb Polygoni Chinensis, Cortex Ilicis Rotundae extract; By Herba Oxalidis strictae 900 ~ 1100 parts, Pericarpium Granati 300 ~ 360 parts, Herba Plantaginis 300 ~ 360 parts, Herb Polygoni Chinensis 900 ~ 1100 parts, Cortex Ilicis Rotundae 640 ~ 700 parts mixing, add water and extract secondary in right amount, each 2 hours, adding concentration is 65% ethanol, purification secondary, then mixing extractum extracting solution being condensed into relative density 1.30 ~ 1.40;
Step 4: creat extract, Radix Wikstroemae extractum and mixing extractum are blended in and put in band drier, drying under reduced pressure becomes dry extract at 50 DEG C ~ 70 DEG C;
Step 5: dry extract is broken into 100 ~ 120 object fine powders;
Step 6: fine powder 75% ethanol is made wet granular, then wet grain drying is become dry granule,
Add disintegrating agent and lubricant, dry granule, disintegrating agent, lubricant are pressed 100:1:5 mixing, tabletted, obtained 'Xiaoyanjiedu '.
3. the preparation method of a kind of 'Xiaoyanjiedu ' according to claim 2, is characterized in that:
Disintegrating agent described in step 6 is carboxymethyl starch sodium, and lubricant is magnesium stearate.
4. the preparation method of a kind of 'Xiaoyanjiedu ' according to claim 1, is characterized in that:
Step 1,2, the preparation process of 3 is preparation process arranged side by side.
5. a method of quality control for eliminating inflammation and expelling toxin, is characterized in that:
Comprise discriminating project to detect and content detection,
Discriminating project detects and comprises the detection of Herba Andrographis medical material, the detection of Radix Wikstroemae medical material and the detection of Herba Oxalidis strictae medical material,
Content detection comprises rutin content in Herba Andrographis medical material content detection and preparation and detects.
6. the method for quality control of a kind of 'Xiaoyanjiedu ' according to claim 5, is characterized in that:
Differentiate: (1) Herba Andrographis medical material detects: get tablet 2-3g, porphyrize, add chloroform 20ml, supersound process 15 minutes, filter, filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution,
Get Herba Andrographis control medicinal material 1g, add methanol 10ml, supersound process 15 minutes, filter, filtrate is medical material solution in contrast,
Get dehydrorographolide reference substance appropriate, add methanol and make the solution of every 1ml containing 1mg, product solution in contrast,
Test according to thin layer chromatography (Chinese Pharmacopoeia version in 2010 annex VIB), draw above-mentioned need testing solution 4 ~ 10 μ l, control medicinal material solution 5 μ l, reference substance solution 4 μ l, put respectively on same silica GF254 lamellae, with chloroform-acetate-methanol (4:3:0.4) for developing solvent, launch, take out, dry; Inspect under putting ultra-violet lamp (254nm); In test sample chromatograph, on the position corresponding with reference substance chromatograph to control medicinal material chromatograph, the speckle of aobvious same color, quality conforms with the regulations,
(2) Radix Wikstroemae medical material detects: get tablet 2-3g, porphyrize, add methanol 20ml, supersound process 15 minutes, and filter, get filtrate 10ml, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution,
Get Radix Wikstroemae control medicinal material 1g, decoct with water 30 minutes, filter, filtrate evaporate to dryness, residue adds methanol 4ml makes dissolving, medical material solution in contrast, tests according to thin layer chromatography (Chinese Pharmacopoeia version in 2010 annex VIB), draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid (5:4:1) for developing solvent, launch, take out, dry; Inspect under putting ultra-violet lamp (365nm); In test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious same color, quality conforms with the regulations;
(3) Herba Oxalidis strictae medical material detects: get tablet 2-3g, porphyrize, add methanol 30ml, reflux 30 minutes, filter, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, 2 times are extracted with ethyl acetate jolting, each 20ml, combined ethyl acetate, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution, separately get Herba Oxalidis strictae control medicinal material 1g, the 50ml that adds water decocts 30 minutes, filter, filtrate is concentrated into 20ml, be made in the same way of control medicinal material solution, test according to thin layer chromatography (Chinese Pharmacopoeia version in 2010 annex VIB), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-formic acid (10: 4: 1) for developing solvent launches, take out, dry, inspect under putting ultra-violet lamp (365nm), in test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious same color, quality conforms with the regulations.
7. the method for quality control of a kind of 'Xiaoyanjiedu ' according to claim 5, is characterized in that:
Assay: (1) Herba Andrographis medical material content detection: measure according to high performance liquid chromatography standard operating procedure:
Chromatographic column: KromasilC
18(octadecylsilane chemically bonded silica); Methanol-water (55:45) is mobile phase; Determined wavelength is 250nm; Theoretical cam curve calculates should be not less than 4000 by dehydrorographolide peak;
Get dehydrorographolide reference substance, it is appropriate that precision takes dehydrorographolide reference substance, adds 60% methanol and make every 1ml containing 15 μ g; Get the tablet 4-6g under content uniformity item, accurately weighed, porphyrize, get about 0.5g, accurately weighed, put in 100ml measuring bottle, add 60% methanol 90ml, ultrasonic (power 250W, frequency 33kHz) process 30 minutes, let cool, add 60% methanol dilution to scale, microporous filter membrane (0.45 μm) filters, and gets subsequent filtrate and uses; Accurate absorption reference substance solution and each 20 μ l of need testing solution respectively, injection liquid chromatography, measures Determination of Dehydroandrographoliin, and in said preparation, every sheet in dehydrorographolide (C42H62O16), must not be less than 0.30mg containing Herba Andrographis;
(2) in preparation, rutin content detects:
According to spectrophotometry: get awns fourth reference substance, precision takes at 120 DEG C of drying under reduced pressure appropriate to the control substance of Rutin of constant weight, adds 60% ethanol and makes the solution of every 1ml containing 0.1mg;
Preparation standard curve: precision measures reference substance solution 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, put in 25ml measuring bottle respectively, respectively add 10% sodium nitrite solution 0.3ml, mixing, places 6 minutes, add 10% aluminum nitrate solution 0.3ml, mixing, places 6 minutes, add 4% sodium hydroxide solution 4ml, shake up, add 30% ethanol to scale, shake up, place 15 minutes; With corresponding solution for blank;
Measure trap at 510nm wavelength place, take trap as vertical coordinate, concentration is abscissa, drawing standard curve; Get the tablet 4-6g under content uniformity item, accurately weighed, porphyrize, gets 0.2g, put in round-bottomed flask, add methanol 25ml, shake up, reflux 1 hour, take out, be cooled to room temperature, filter, filter paper adds methanol 25ml again together with residue, reflux 1 hour, takes out, and cooling filters, merging filtrate, residue methanol 15ml gradation washing, washing liquid and filtrate merge, evaporate to dryness, residue adds 60% alcoholic solution makes dissolving, to be transferred in 50ml measuring bottle and to be diluted to scale, shaking up;
Precision measures 1ml, method under sighting target directrix curve preparation, from " putting respectively in 25ml measuring bottle ", measure trap in accordance with the law, read the weight of rutin in need testing solution from standard curve, calculate rutin content, in said preparation, every sheet in rutin (C27H30O16), must not be less than 10.0mg containing total flavones.
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| CN105954396A (en) * | 2016-04-25 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for detecting content of dehydroandrographoline in andrographis tablet by using HPLC |
| CN110221015A (en) * | 2019-06-11 | 2019-09-10 | 浙江金大康动物保健品有限公司 | A kind of gradient full information thin-layer identification method of granatum medicinal material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105954396A (en) * | 2016-04-25 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for detecting content of dehydroandrographoline in andrographis tablet by using HPLC |
| CN110221015A (en) * | 2019-06-11 | 2019-09-10 | 浙江金大康动物保健品有限公司 | A kind of gradient full information thin-layer identification method of granatum medicinal material |
| CN110221015B (en) * | 2019-06-11 | 2021-04-27 | 浙江金大康动物保健品有限公司 | Gradient full-information thin-layer identification method for pomegranate bark medicinal material |
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