CN104034839A - Quality detection method of hepatitis B treatment capsule - Google Patents
Quality detection method of hepatitis B treatment capsule Download PDFInfo
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- CN104034839A CN104034839A CN201310072533.6A CN201310072533A CN104034839A CN 104034839 A CN104034839 A CN 104034839A CN 201310072533 A CN201310072533 A CN 201310072533A CN 104034839 A CN104034839 A CN 104034839A
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Abstract
The invention provides a quality detection method of ahepatitis B treatment capsule. The method is a quality control method having the advantages of simplification, time and energy saving, and strong maneuverability, and is highly conducive to industrial production application.
Description
Technical field
The present invention relates to a kind of quality determining method of Chinese patent drug, be specifically related to the quality determining method of hepatitis B strengthening capsule.
Background technology
Hepatitis B strengthening capsule records in " Drug Standard of Ministry of Public Health of the Peoples Republic of China Traditional Chinese medicine historical preparation " first 1 page, and standard code is WS
3-B-0001-89, tool filling liver kidney, the function of qi and activate blood circulation.For hepatitis B, dialectical liver kidney two asthenic symptoms that belong to are waited.Clinical manifestation is: dull pain in liver discomfort, malaise, soreness and weakness of waist and knees, the palpitaition of breathing hard, spontaneous perspiration, dizzy, receive few, the light weak pulse of tongue.Hepatitis B strengthening capsule is applied for many years clinically, obtains more gratifying curative effect.Hepatitis B strengthening capsule prescription is made up of Chinese crude drug fleece-flower root 15g, giant knotweed 25g, rhizome of cyrtomium 50g, Chinese cassia tree 5g, alum 10g, granatum 6g, Radix Angelicae Sinensis 10g, red sage root 15g, semen astragali complanati 10g, ginseng 10g, Chinese ephedra 6g, make by following technique: above ten simply, Radix Angelicae Sinensis, Chinese cassia tree, the red sage root, alum are pulverized as fine powder, the seven taste boiling secondaries such as all the other fleece-flowers root, each 3 hours, 2 hours for the second time, collecting decoction, filtered, filtrate filters into thick paste, add above-mentioned powder, mix, dry in 70～80 DEG C, be ground into fine powder, sieve, encapsulated, to obtain final product.In prescription, the fleece-flower root is the dried root of polygonum multiflorum thunb Polygotum multi florum Thunb.; Giant knotweed is dry rhizome and the root of polygonaceae plant giant knotweed Polygonum cuspidatum Sieb.et Zucc.; Rhizome of cyrtomium is the dry root-like stock of osmund Pteridiaceae plant Osmunda Vachellii Hook Osmunda vachellii Hook., Blechnaceae plant blechnoid Blechnum orientale L. or Brainea insignis Brainea insignis (Hook.) J.Sm.; Chinese cassia tree is the dry bark of canella Chinese cassia tree Cinnamomum cassia Presl; Alum is that Sulfates mineral alunite refines and makes through processing, containing aqueous sulfuric acid aluminium potassium [AlK (SO
4)
212H
2o] be no less than 99.5%; Granatum is the dry pericarp of Punicaceae plant pomegranate Punica granatum L.; When being classified as the dry root of umbelliferae angelica Angelica sinensis (Oliv) Diels.; The red sage root is dry root and the rhizome of labiate red sage root Salvia miltiorrhiza Bge.; Semen astragali complanati is the dry mature seed of legume astragatus complanatus A stragalus complanatus R.Br.; Ginseng is dry root and the rhizome of Araliaceae ginseng Panax ginseng C.A.Mey.; Chinese ephedra is the dry herbaceous stem stem of Ephedraceae plant plait Chinese ephedra Ephedra sinica Stapf., epheday intermedia Ephedraintermedia Schrenk et C.A.Mey. or ephedra equisetina Ephedra equisetina Bge..
Hepatitis B strengthening capsule proper mass standard is only controlled product quality with micro-discriminating, therefore need study its method of quality control, formulates truly feasible method and ensures product quality and clinical efficacy.
Summary of the invention
The technical problem to be solved in the present invention is to provide the quality determining method of a kind of method simplification, hepatitis B strengthening capsule time-saving energy-saving, workable, is extremely conducive to the application of suitability for industrialized production.
The present invention solves the problems of the technologies described above with following technical scheme:
The quality determining method of hepatitis B strengthening capsule comprises one or more in following detection:
A, the giant knotweed in medicine is carried out to qualitative discriminating by thin-layered chromatography
Get this product content appropriate, add the ultrasonic processing of methyl alcohol, filter, filtrate evaporate to dryness, residue is dissolved in water, and extracts with ether jolting, gets ether extracted liquid, volatilizes, and residue adds acetic acid ethyl dissolution, as need testing solution; Separately get giant knotweed control medicinal material 0.1g, be made in the same way of control medicinal material solution; Get again archen reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast; Draw above-mentioned reference substance solution, control medicinal material solution, each 1～6 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking 60～90 DEG C-ethyl acetate-formic acid of sherwood oil 14～16: 2～4: 0.5～1.5 upper solution, as developping agent, is launched, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color; Put in ammonia steam smoked after, under daylight, inspect, spot becomes redness.
B, the Radix Angelicae Sinensis in medicine is carried out to qualitative discriminating by thin-layered chromatography
Get this product content 2.5g, add ethanol 10ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, and residue adds ethanol 1ml to be made to dissolve, as need testing solution; Separately get Radix Angelicae Sinensis control medicinal material 0.5g, be made in the same way of control medicinal material solution; Draw the each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane-ethyl acetate 9: 1 as developping agent, launch, take out, dry, put in ammonia steam smoked after, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
C, the red sage root in medicine is carried out to qualitative discriminating by thin-layered chromatography
Get the ultrasonic processing that adds diethyl ether of this product content, filter, discard filtrate, the dregs of a decoction volatilize ether, add the ultrasonic processing of methyl alcohol, filter, filtrate evaporate to dryness, residue adds 1% hydrochloric acid solution to be made to dissolve, with ether jolting extraction, get ether solution, volatilize, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution; Separately get red sage root control medicinal material and be made in the same way of control medicinal material solution; Get again tanshin polyphenolic acid B reference substance, add Methanol and become reference substance solution; Draw above-mentioned control medicinal material solution, reference substance solution, each 1～6 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking toluene-methenyl choloride-ethyl acetate-methyl alcohol-formic acid 2: 3: 4: 0.5: 2 as developping agent, launch, take out, dry; Spray, with 1% liquor ferri trichloridi and the 1% potassium ferricyanide solution mixed solution of 1: 1, mixes before use, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color.D, with the content of red sage root characteristic component tanshin polyphenolic acid B in this medicine of high effective liquid chromatography for measuring
Chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking methyl alcohol-acetonitrile-formic acid-water 24～28: 7～9: 0.8～1.2: 62～68 as mobile phase; Detect wavelength 280～290nm;
It is appropriate that tanshin polyphenolic acid B reference substance is got in the preparation of reference substance solution, accurately weighed, adds 75% methyl alcohol and make the solution of every 1ml containing 30～80 μ g, to obtain final product;
This product content is got in the preparation of need testing solution, and porphyrize is got 0.1～1g, accurately weighed, to put in tool plug conical flask, precision adds 75% methyl alcohol 30～100ml, close plug, weighed weight, adds hot reflux 0.5～3 hour, let cool, more weighed weight, supply the weight of less loss with 75% methyl alcohol, shake up, centrifugal, get supernatant, to obtain final product;
Determination method is accurate reference substance solution and each 10～20 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and to obtain final product.
The quality determining method of hepatitis B strengthening capsule comprises one or more in following detection:
A, the giant knotweed in medicine is carried out to qualitative discriminating by thin-layered chromatography
Get this product content 1g, add methyl alcohol 30ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, the residue 20ml gradation that adds water makes to dissolve, and extracts 2 times each 20ml with ether jolting, merge ether extracted liquid, volatilize, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution; Separately get giant knotweed control medicinal material 0.1g, be made in the same way of control medicinal material solution; Get again archen reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast; Draw above-mentioned reference substance solution 1 μ l, control medicinal material solution, each 3～6 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking 60～90 DEG C-ethyl acetate-formic acid of sherwood oil upper solution of 15: 3: 1 as developping agent, launches, and takes out, and dries; Put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color; Put in ammonia steam smoked after, under daylight, inspect, spot becomes redness.
B, the Radix Angelicae Sinensis in medicine is carried out to qualitative discriminating by thin-layered chromatography
Get this product content 2.5g, add ethanol 10ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, and residue adds ethanol 1ml to be made to dissolve, as need testing solution; Separately get Radix Angelicae Sinensis control medicinal material 0.5g, be made in the same way of control medicinal material solution; Draw the each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane-ethyl acetate 9: 1 as developping agent, launch, take out, dry, put in ammonia steam smoked after, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
C, the red sage root in medicine is carried out to qualitative discriminating by thin-layered chromatography
Get this product content 3g, the 40ml that adds diethyl ether, ultrasonic processing 10 minutes, filter, discard filtrate, the dregs of a decoction volatilize ether, add methyl alcohol 40ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, residue adds 1% hydrochloric acid solution 15ml to be made to dissolve, with ether jolting extraction 2 times, each 20ml, merges ether solution, volatilizes, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution; Separately get red sage root control medicinal material 1g, be made in the same way of control medicinal material solution; Get again tanshin polyphenolic acid B reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast; Draw above-mentioned control medicinal material solution 1 μ l, reference substance solution, each 3～6 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking toluene-methenyl choloride-ethyl acetate-methyl alcohol-formic acid 2: 3: 4: 0.5: 2 as developping agent, launches, and takes out, and dries; Spray, with 1% liquor ferri trichloridi and the 1% potassium ferricyanide solution mixed solution of 1: 1, mixes before use, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color.D, with the content of red sage root characteristic component tanshin polyphenolic acid B in this medicine of high effective liquid chromatography for measuring
Chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking methyl alcohol-acetonitrile-formic acid-water 26: 8: 1: 65 as mobile phase; Detect wavelength 286nm;
It is appropriate that tanshin polyphenolic acid B reference substance is got in the preparation of reference substance solution, accurately weighed, adds 75% methyl alcohol and make the solution of every 1ml containing 50 μ g, to obtain final product;
This product content is got in the preparation of need testing solution, and porphyrize is got about 0.3g, accurately weighed, to put in tool plug conical flask, precision adds 75% methyl alcohol 50ml, close plug, weighed weight, adds hot reflux 1 hour, let cool, more weighed weight, supply the weight of less loss with 75% methyl alcohol, shake up, get centrifugal 10 minutes of the rotating speed that 10ml turns with per minute 3000, get supernatant, to obtain final product;
Determination method is accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and to obtain final product.
The quality determining method of hepatitis B strengthening capsule of the present invention, draws by lot of experiments investigation and comparison, is that a kind of method is simplified, the quality determining method of hepatitis B strengthening capsule time-saving energy-saving, workable, is extremely conducive to the application of suitability for industrialized production.
Embodiment
Although this instructions by particularly pointing out and knowing that claimed claims of the present invention draw a conclusion, should be believed following explanation and will understand better the present invention.
Except as otherwise noted, the ratio of related developping agent and mobile phase is volume ratio herein.
" 1% hydrochloric acid solution " refers to mass volume ratio herein, and 1g hydrochloric acid is mixed with 100ml.
Described in " 1% liquor ferri trichloridi and the 1% potassium ferricyanide solution mixed solution of 1: 1 " 1% all refers to the ratio of weight herein, refers to the ratio of volume at 1: 1.
" 75% methyl alcohol " is volume ratio herein.
As used herein, word " preferably " and variant refer to embodiment of the present invention that specific beneficial effect can be provided under specific environment.But other embodiment can be also preferred under identical or other environment.In addition, the detailed description of one or more preferred embodiments does not represent that other embodiment is useless, and is not intended to get rid of from category of the present invention other embodiment.
Quality determining method of the present invention is to obtain through a large amount of experiment sievings, below experimental study be preferred process of the present invention.
One, the thin-layer chromatography of giant knotweed is differentiated
The preparation method of need testing solution, except the inventive method, has also compared following two kinds of methods:
1. get this product content 2.5g, add absolute ethyl alcohol 10ml, put in water-bath warm 10 minutes, filter, filtrate is concentrated into about 1ml, as need testing solution.
2. get this product content 1g, add methyl alcohol 20ml, ultrasonic processing 15 minutes, filter, filtrate evaporate to dryness, residue adds 2.5mol/L sulfuric acid solution 20ml to be made to dissolve, put in water-bath and heat 30 minutes, let cool, with methenyl choloride jolting extraction 2 times, each 20ml, merge methenyl choloride liquid, evaporate to dryness, residue adds methenyl choloride 1ml to be made to dissolve, as need testing solution.
Test findings: 1. spot is clear not, 2. separating effect and the inventive method are suitable, but its preparation method is more complicated.
Separately try out different development systems: 1. sherwood oil (60～90 DEG C)-ethyl acetate (8: 2); 2. sherwood oil (30～60 DEG C)-ethyl formate-formic acid (15: 5: 1) upper strata liquid; 3. normal hexane-toluene-ethyl acetate-glacial acetic acid (18: 2: 2: 0.5); 4. toluene-ethyl acetate-formic acid (10: 1: 0.3); 5. normal hexane-ethyl acetate-formic acid (15: 5: 1).Result 1. Rf value is on the low side, and spot is clear not, the 2. 3. 4. 5. inadequate rounding of spot, and separating effect is bad, and the present invention records system and launches effectively, Rf value is moderate, clear spot, favorable reproducibility.
Investigate the separating effect of the different proportionings of 60～90 DEG C of developping agent sherwood oils-ethyl acetate-formic acid, for obtaining good Rf value and spot rounding property, developping agent is preferably 60～90 DEG C-ethyl acetate-formic acid of sherwood oil 14～16: 2～4: 0.5～1.5, more preferably 60～90 DEG C-ethyl acetate-formic acid of sherwood oil 15: 3: 1.
Two, the thin-layer chromatography of Radix Angelicae Sinensis is differentiated
The preparation method of need testing solution, except the inventive method, has also compared following two kinds of methods:
1. get this product content 2.5g, the 10ml that adds diethyl ether, ultrasonic processing 10 minutes, filters, and filtrate volatilizes, and residue adds ethanol 1ml to be made to dissolve, as need testing solution.
2. get this product content 2.5g, add absolute ethyl alcohol 10ml, put in water-bath warm 10 minutes, filter, filtrate is concentrated into about 1ml, as need testing solution.
Result result method 1. 2. in test sample chromatogram feature spot all not obviously clear, impurity disturbs large, therefore do not adopt.
Inspection method had once been tried out directly and had been inspected under ultraviolet lamp (365nm), and the negative test sample of result is equipped with impurity in control medicinal material principal spot corresponding positions and disturbs, and adopts after ammonia fumigating, can eliminate well impurity and disturb.
Three, the thin-layer chromatography of the red sage root and red sage root characteristic component tanshin polyphenolic acid B is differentiated
The preparation method of need testing solution, except the inventive method, has also compared following two kinds of methods:
1. get this product content 4.0g, the 20ml that adds diethyl ether, jolting, places 1 hour, filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution.
2. get this product content 1.0g, add 75% methyl alcohol 50ml, add hot reflux 1 hour, filter, filtrate is concentrated into 1ml, as need testing solution.
Feature spot in result test sample chromatogram is all not obvious.And that the present invention records method separating effect is better, spot is more clear.
Developping agent, except the inventive method, has also been investigated following developping agent: 1. toluene-ethyl acetate-formic acid (5: 3: 1); 2. toluene-ethyl acetate-acetone-formic acid (5: 2: 1: 1); 3. toluene-ethyl acetate-acetone-formic acid (4: 3: 2: 1).1. 2. Rf value is less than normal for result development system, the inadequate rounding of spot, the 3. inadequate rounding of spot.
Inspection knowledge method is also on probation: 1. put under ultraviolet lamp (254nm) and inspect; 2. put under ultraviolet lamp (365nm) and inspect; 3. spray with inspection under daylight after 5% liquor ferri trichloridi and know.Result: 1. chromatogram background is darker, impurity spot is more, and separating effect is bad, and 2. feature spot is not obvious, and 3. spot is clear not; With the inventive method for well.
Also another feature composition tanshinone IIA of the red sage root is differentiated test sample preparation: 1. get this product content 4.0g, the 20ml that adds diethyl ether, jolting, places 1 hour, filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution; 2. get this product content 3.5g, the 40ml that adds diethyl ether, ultrasonic 10 minutes, filter, filtrate volatilizes, and residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution.Development system has been tried out 1. sherwood oil (60～90 DEG C)-ethyl acetate (4: 1); 2. toluene-ethyl acetate-acetone-formic acid (10: 2: 4: 2); 3. normal hexane-ethyl acetate-formic acid (6: 2: 0.1); 4. toluene-methyl alcohol (10: 1).Result feature spot is all not obvious.
It is effective that the present invention records method expansion, and Rf value is moderate, thin layer separator well, clear spot, favorable reproducibility.
Four, the content assaying method of red sage root characteristic component tanshin polyphenolic acid B is learned test
1 need testing solution preparation method selects
The preparation of 1.1 reference substance solution: precision takes tanshin polyphenolic acid B reference substance, adds 75% methyl alcohol and is mixed with the reference substance solution of debita spissitudo, shakes up, and to obtain final product.
Suitable reference substance solution concentration can be saved reference substance, and has the mensuration precision conforming with the regulations, and its concentration is preferably every 1ml containing 30～80 μ g, and more preferably every 1ml is containing 50 μ g.
The preparation of 1.2 need testing solutions: get this product content, porphyrize, gets appropriate, accurately weighed, to put in tool plug conical flask, precision adds 75% methyl alcohol appropriate, close plug, weighed weight, adds hot reflux, let cool, more weighed weight, supply the weight of less loss with 75% methyl alcohol, shake up, centrifugal, get supernatant, to obtain final product.
Get appropriate sample and be conducive to accurately detect sample, its sampling amount is preferably 0.1～1g, more preferably 0.3g.
Extraction solvent 75% methyl alcohol adds in right amount and is conducive to accurately detect sample, and its addition is preferably 30～100ml, more preferably 50ml.
Add hot reflux appropriate time and be conducive to extracts active ingredients out, its heating return time is preferably 0.5～3 hour, more preferably 1 hour.
The negative sample solution of preparing of 1.3 negative sample solution is to get the negative sample solution that does not contain the red sage root containing the negative sample of the red sage root by the preparation of above-mentioned " preparation of need testing solution " method.
2 chromatographic conditions and system suitability
Chromatographic column: octadecyl silane chromatographic column (Thermo C18250 × 4.6mm), Phenomenex C184 × 3.0mm guard column; Taking methyl alcohol-acetonitrile-formic acid-water (26: 8: 1: 65) as mobile phase; Flow velocity: 1.0ml/min, column temperature: 30 DEG C; Detect wavelength: 286nm.
Suitable mobile phase can be saved proving time, and obtains good separating effect, and mobile phase is preferably methyl alcohol-acetonitrile-formic acid-water 24～28: 7～9: 0.8～1.2: 62～68, and more preferably methyl alcohol-acetonitrile-formic acid-water 26: 8: 1: 65.
Suitable detection wavelength can make to detect has good sensitivity, detects wavelength and is preferably 280～290nm, more preferably 286nm.
Draw respectively tanshin polyphenolic acid B reference substance solution, need testing solution and not containing the each 10 μ l of negative sample solution of the red sage root, injection liquid chromatography, color rendering spectrogram.Under this condition, tanshin polyphenolic acid B and other component reach baseline separation, degree of separation R > 1.5, and theoretical cam curve is calculated and is greater than 2000 by tanshin polyphenolic acid B, and tanshin polyphenolic acid B retention time is about 13 minutes, in table 1.Negative sample solution is in reference substance chromatogram relevant position without absorption peak, and visible feminine gender is noiseless.
Table 1 theoretical cam curve, degree of separation, retention time data
2.3 linear relationships are investigated
Precision takes tanshin polyphenolic acid B reference substance, adds 75% methyl alcohol and be mixed with respectively the reference substance solution of 12.77 μ g/ml, 25.54 μ g/ml, 51.07 μ g/ml, 95.76 μ g/ml, 191.52 μ g/ml.By above-mentioned chromatographic condition, sample introduction 10 μ l respectively, measure, and with peak area integration A, to tanshin polyphenolic acid B sample size C, (μ g) carries out regretional analysis, obtains regression equation: A=1.19 × 10
3c-53.72, r=0.9995.Show that tanshin polyphenolic acid B sample size is good in 0.1277 μ g～1.9152 μ g scope internal linear relation, and straight-line pass initial point, available single-point external standard method is carried out measurement and calculation, and linear relationship data is in table 2.
Table 2 linear relationship is investigated data
2.4 precision test
Get tanshin polyphenolic acid B reference substance solution (51.07 μ g/ml), by above-mentioned chromatographic condition, measure in accordance with the law, repeat sample introduction 5 times, calculate the relative standard deviation of tanshin polyphenolic acid B peak area A, the results are shown in Table 3, show that precision is better.
Table 3 precision test
2.5 stability test
Get need testing solution (lot number: 8610001), after placement 0,2,4,6,8 and 24h, measure tanshin polyphenolic acid B peak area A respectively in accordance with the law, calculate relative standard deviation, the results are shown in Table 4, show that 24 hours internal stabilities of need testing solution are better.
Table 4 stability test
2.6 replica test
Get same sample (lot number: 8610001), by preparation method's test of need testing solution, prepare 6 parts of need testing solutions, measure in accordance with the law, calculate content and the relative standard deviation of tanshin polyphenolic acid B, the results are shown in Table 5, show method repeatability better.
Table 5 replica test
2.7 average recovery tests
Get this product (lot number: 8610001) content, porphyrize, gets about 0.15g, accurately weighed, put in tool plug conical flask, it is the tanshin polyphenolic acid B reference substance solution 0.8ml of 1.596mg/g that precision adds concentration, volatilizes solvent, standby with legal system, measure in accordance with the law, calculate recovery rate, the results are shown in Table 6, shows that the method recovery is better.
The test of table 6 average recovery
2.8 sample determination
By measure 4 batch samples under text assay item in accordance with the law, with the content of tanshin polyphenolic acid B in peak area external standard method calculation sample, the results are shown in Table 7.
Table 7 sample determination result
Above-mentioned projects checking procedure need to not carried out according to sequencing, and can also carry out other conventional sense simultaneously, and as proterties, this product is capsule, and content is tan powder; Bitter.
Embodiment 1:
The quality determining method of hepatitis B strengthening capsule is as follows:
1, by thin-layered chromatography, the giant knotweed in this product is carried out to qualitative discriminating:
Get this product content 1g, add methyl alcohol 30ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, the residue 20ml gradation that adds water makes to dissolve, and extracts 2 times each 20ml with ether jolting, merge ether extracted liquid, volatilize, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution.Separately get giant knotweed control medicinal material 0.1g, be made in the same way of control medicinal material solution.Get again archen reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast.According to annex VIB thin-layered chromatography test of Chinese Pharmacopoeia version in 2010, draw above-mentioned reference substance solution 1 μ l, control medicinal material solution, each 3～6 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking 15: 3: 1 upper solution of 60～90 DEG C-ethyl acetate-formic acid of sherwood oil as developping agent, launch, take out, dry.Put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color; Put in ammonia steam smoked after, under daylight, inspect, spot becomes redness.
2, by thin-layered chromatography, the Radix Angelicae Sinensis in medicine is carried out to qualitative discriminating:
Get this product content 2.5g, add ethanol 10ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, and residue adds ethanol 1ml to be made to dissolve, as need testing solution.Separately get Radix Angelicae Sinensis control medicinal material 0.5g, be made in the same way of control medicinal material solution.According to annex VIB thin-layered chromatography test of Chinese Pharmacopoeia version in 2010, draw the each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane-ethyl acetate 9: 1 as developping agent, launch, take out, dry, put in ammonia steam smoked after, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
3, by thin-layered chromatography, the red sage root in medicine is carried out to qualitative discriminating:
Get this product content 3g, the 40ml that adds diethyl ether, ultrasonic processing 10 minutes, filter, discard filtrate, the dregs of a decoction volatilize ether, add methyl alcohol 40ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, residue adds 1% hydrochloric acid solution 15ml to be made to dissolve, with ether jolting extraction 2 times, each 20ml, merges ether solution, volatilizes, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution.Separately get red sage root control medicinal material 1g, be made in the same way of control medicinal material solution.Get again tanshin polyphenolic acid B reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast.According to annex VIB thin-layered chromatography test of Chinese Pharmacopoeia version in 2010, draw above-mentioned control medicinal material solution 1 μ l, reference substance solution, each 3～6 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking toluene-methenyl choloride-ethyl acetate-methyl alcohol-formic acid 2: 3: 4: 0.5: 2 as developping agent, launch, take out, dry.Spray is with 1% liquor ferri trichloridi and the 1% potassium ferricyanide solution mixed solution of 1: 1, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color.
4, with the content of red sage root characteristic component tanshin polyphenolic acid B in this medicine of high effective liquid chromatography for measuring:
Chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking methyl alcohol-acetonitrile-formic acid-water 26: 8: 1: 65 as mobile phase; Detect wavelength 286nm; Theoretical cam curve is calculated and should be not less than 2000 by tanshin polyphenolic acid B peak.
It is appropriate that tanshin polyphenolic acid B reference substance is got in the preparation of reference substance solution, accurately weighed, adds 75% methyl alcohol and make the solution of every 1ml containing 50 μ g, to obtain final product.
This product content is got in the preparation of need testing solution, and porphyrize is got about 0.3g, accurately weighed, to put in tool plug conical flask, precision adds 75% methyl alcohol 50ml, close plug, weighed weight, adds hot reflux 1 hour, let cool, more weighed weight, supply the weight of less loss with 75% methyl alcohol, shake up, get centrifugal 10 minutes of 10ml (3000 revs/min), get supernatant, to obtain final product.
Determination method is accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and to obtain final product.
Embodiment 2:
The quality determining method of hepatitis B strengthening capsule is as follows:
1, by thin-layered chromatography, the giant knotweed in this product is carried out to qualitative discriminating:
Get this product content 0.2g, add methyl alcohol 20ml, ultrasonic processing 15 minutes, filters, filtrate evaporate to dryness, the residue 15ml gradation that adds water makes to dissolve, and extracts 3 times each 15ml with ether jolting, merge ether extracted liquid, volatilize, residue adds ethyl acetate 0.5ml to be made to dissolve, as need testing solution.Separately get giant knotweed control medicinal material 0.1g, be made in the same way of control medicinal material solution.Get again archen reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast.According to annex VIB thin-layered chromatography test of Chinese Pharmacopoeia version in 2010, draw above-mentioned reference substance solution, control medicinal material solution, each 4～6 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking 14: 4: 1.5 upper solution of 60～90 DEG C-ethyl acetate-formic acid of sherwood oil as developping agent, launch, take out, dry.Put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color; Put in ammonia steam smoked after, under daylight, inspect, spot becomes redness.
2, by thin-layered chromatography, the Radix Angelicae Sinensis in medicine is carried out to qualitative discriminating:
Get this product content 2.5g, add ethanol 10ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, and residue adds ethanol 1ml to be made to dissolve, as need testing solution.Separately get Radix Angelicae Sinensis control medicinal material 0.5g, be made in the same way of control medicinal material solution.According to annex VIB thin-layered chromatography test of Chinese Pharmacopoeia version in 2010, draw the each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane-ethyl acetate 9: 1 as developping agent, launch, take out, dry, put in ammonia steam smoked after, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
3, by thin-layered chromatography, the red sage root in medicine is carried out to qualitative discriminating:
Get this product content 1g, the 20ml that adds diethyl ether, ultrasonic processing 30 minutes, filter, discard filtrate, the dregs of a decoction volatilize ether, add methyl alcohol 20ml, ultrasonic processing 10 minutes, filters, filtrate evaporate to dryness, residue adds 1% hydrochloric acid solution 10ml to be made to dissolve, with ether jolting extraction 2 times, each 15ml, merges ether solution, volatilizes, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution.Separately get red sage root control medicinal material 0.5g, be made in the same way of control medicinal material solution.Get again tanshin polyphenolic acid B reference substance, add methyl alcohol and make the solution of every 1ml containing 0.5mg, product solution in contrast.According to annex VIB thin-layered chromatography test of Chinese Pharmacopoeia version in 2010, draw above-mentioned control medicinal material solution 1 μ l, reference substance solution, each 1～3 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking toluene-methenyl choloride-ethyl acetate-methyl alcohol-formic acid 2: 3: 4: 0.5: 2 as developping agent, launch, take out, dry.Spray is with 1% liquor ferri trichloridi and the 1% potassium ferricyanide solution mixed solution of 1: 1, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color.
4, with the content of red sage root characteristic component tanshin polyphenolic acid B in this medicine of high effective liquid chromatography for measuring:
Chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking methyl alcohol-acetonitrile-formic acid-water 24: 7: 1.2: 68 as mobile phase; Detect wavelength 280nm; Theoretical cam curve is calculated and should be not less than 2000 by tanshin polyphenolic acid B peak.
It is appropriate that tanshin polyphenolic acid B reference substance is got in the preparation of reference substance solution, accurately weighed, adds 75% methyl alcohol and make the solution of every 1ml containing 30 μ g, to obtain final product.
This product content is got in the preparation of need testing solution, and porphyrize is got about 0.1g, accurately weighed, to put in tool plug conical flask, precision adds 75% methyl alcohol 30ml, close plug, weighed weight, adds hot reflux 0.5 hour, let cool, more weighed weight, supply the weight of less loss with 75% methyl alcohol, shake up, get centrifugal 20 minutes of 5ml (4000 revs/min), get supernatant, to obtain final product.
Determination method is accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and to obtain final product.
Embodiment 3:
The quality determining method of hepatitis B strengthening capsule is as follows:
1, by thin-layered chromatography, the giant knotweed in this product is carried out to qualitative discriminating:
Get this product content 3g, add methyl alcohol 50ml, ultrasonic processing 50 minutes, filters, filtrate evaporate to dryness, the residue 50ml gradation that adds water makes to dissolve, and extracts 3 times each 30ml with ether jolting, merge ether extracted liquid, volatilize, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution.Separately get giant knotweed control medicinal material 0.1g, be made in the same way of control medicinal material solution.Get again archen reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast.According to annex VIB thin-layered chromatography test of Chinese Pharmacopoeia version in 2010, draw above-mentioned reference substance solution, control medicinal material solution, each 2～4 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking 16: 2: 0.5 upper solution of 60～90 DEG C-ethyl acetate-formic acid of sherwood oil as developping agent, launch, take out, dry.Put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color; Put in ammonia steam smoked after, under daylight, inspect, spot becomes redness.
2, by thin-layered chromatography, the Radix Angelicae Sinensis in medicine is carried out to qualitative discriminating:
Get this product content 2.5g, add ethanol 10ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, and residue adds ethanol 1ml to be made to dissolve, as need testing solution.Separately get Radix Angelicae Sinensis control medicinal material 0.5g, be made in the same way of control medicinal material solution.According to annex VIB thin-layered chromatography test of Chinese Pharmacopoeia version in 2010, draw the each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane-ethyl acetate 9: 1 as developping agent, launch, take out, dry, put in ammonia steam smoked after, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
3, by thin-layered chromatography, the red sage root in medicine is carried out to qualitative discriminating:
Get this product content 5g, the 60ml that adds diethyl ether, ultrasonic processing 40 minutes, filter, discard filtrate, the dregs of a decoction volatilize ether, add methyl alcohol 60ml, ultrasonic processing 50 minutes, filters, filtrate evaporate to dryness, residue adds 1% hydrochloric acid solution 20ml to be made to dissolve, with ether jolting extraction 2 times, each 25ml, merges ether solution, volatilizes, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution.Separately get red sage root control medicinal material 2g, be made in the same way of control medicinal material solution.Get again tanshin polyphenolic acid B reference substance, add methyl alcohol and make the solution of every 1ml containing 2mg, product solution in contrast.According to annex VIB thin-layered chromatography test of Chinese Pharmacopoeia version in 2010, draw above-mentioned control medicinal material solution 1 μ l, reference substance solution, each 2～5 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking toluene-methenyl choloride-ethyl acetate-methyl alcohol-formic acid 2: 3: 4: 0.5: 2 as developping agent, launch, take out, dry.Spray is with 1% liquor ferri trichloridi and the 1% potassium ferricyanide solution mixed solution of 1: 1, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color.
4, with the content of red sage root characteristic component tanshin polyphenolic acid B in this medicine of high effective liquid chromatography for measuring:
Chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking methyl alcohol-acetonitrile-formic acid-water 28: 9: 0.8: 62 as mobile phase; Detect wavelength 290nm; Theoretical cam curve is calculated and should be not less than 2000 by tanshin polyphenolic acid B peak.
It is appropriate that tanshin polyphenolic acid B reference substance is got in the preparation of reference substance solution, accurately weighed, adds 75% methyl alcohol and make the solution of every 1ml containing 80 μ g, to obtain final product.
This product content is got in the preparation of need testing solution, and porphyrize is got about 1g, accurately weighed, to put in tool plug conical flask, precision adds 75% methyl alcohol 100ml, close plug, weighed weight, adds hot reflux 3 hours, let cool, more weighed weight, supply the weight of less loss with 75% methyl alcohol, shake up, get centrifugal 50 minutes of 30ml (2000 revs/min), get supernatant, to obtain final product.
Determination method is accurate reference substance solution and the each 20 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and to obtain final product.
Claims (1)
1. one kind has filling liver kidney, the quality determining method of the hepatitis B strengthening capsule of qi and activate blood circulation, wherein this capsule is by Chinese crude drug fleece-flower root 15g, giant knotweed 25g, rhizome of cyrtomium 50g, Chinese cassia tree 5g, alum 10g, granatum 6g, Radix Angelicae Sinensis 10g, red sage root 15g, semen astragali complanati 10g, ginseng 10g, Chinese ephedra 6g composition, this capsule is made by following technique: above ten simply, Radix Angelicae Sinensis, Chinese cassia tree, the red sage root, alum is pulverized as fine powder, the seven taste boiling secondaries such as all the other fleece-flowers root, each 3 hours, 2 hours for the second time, collecting decoction, filter, filtrate filters into thick paste shape, add above-mentioned powder, mix, dry in 70～80 DEG C, be ground into fine powder, sieve, encapsulated, obtain.The quality determining method of this medicine is characterized in that: the method comprises following all or part of content: the qualitative discriminating of thin-layer chromatography of the qualitative discriminating of thin-layer chromatography of giant knotweed, the qualitative discriminating of thin-layer chromatography of Radix Angelicae Sinensis, the red sage root, the assay of red sage root characteristic component tanshin polyphenolic acid B.
The qualitative discriminating of thin-layer chromatography of a, giant knotweed:
Get this drug substance contents 1g, add methyl alcohol 30ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, the residue 20ml gradation that adds water makes to dissolve, and extracts 2 times each 20ml with ether jolting, merge ether extracted liquid, volatilize, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution.Separately get giant knotweed control medicinal material 0.1g, be made in the same way of control medicinal material solution.Get again archen reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast.Test according to thin-layered chromatography (annex VIB of " Chinese Pharmacopoeia " version in 2010), draw above-mentioned reference substance solution 1 μ l, control medicinal material solution, each 3～6 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil (60～90 DEG C)-ethyl acetate-formic acid (15: 3: 1) upper solution as developping agent, launch, take out, dry.Put under ultraviolet lamp (365nm) and inspect, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color; Put in ammonia steam smoked after, under daylight, inspect, spot becomes redness.
The qualitative discriminating of thin-layer chromatography of b, Radix Angelicae Sinensis:
Get this drug substance contents 2.5g, add ethanol 10ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, and residue adds ethanol 1ml to be made to dissolve, as need testing solution.Separately get Radix Angelicae Sinensis control medicinal material 0.5g, be made in the same way of control medicinal material solution.Test according to thin-layered chromatography (annex VIB of " Chinese Pharmacopoeia " version in 2010), draw the each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane-ethyl acetate (9: 1) as developping agent, launch, take out, dry, put in ammonia steam smoked after, put under ultraviolet lamp (365nm) and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
The qualitative discriminating of thin-layer chromatography of c, the red sage root:
Get this drug substance contents 3g, the 40ml that adds diethyl ether, ultrasonic processing 10 minutes, filter, discard filtrate, the dregs of a decoction volatilize ether, add methyl alcohol 40ml, ultrasonic processing 30 minutes, filters, filtrate evaporate to dryness, residue adds 1% hydrochloric acid solution 15ml to be made to dissolve, with ether jolting extraction 2 times, each 20ml, merges ether solution, volatilizes, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution.Separately get red sage root control medicinal material 1g, be made in the same way of control medicinal material solution.Get again tanshin polyphenolic acid B reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast.Test according to thin-layered chromatography (annex VIB of " Chinese Pharmacopoeia " version in 2010), draw above-mentioned control medicinal material solution 1 μ l, reference substance solution, each 3～6 μ l of need testing solution, put respectively on same silica gel g thin-layer plate, taking toluene-methenyl choloride-ethyl acetate-methyl alcohol-formic acid (2: 3: 4: 0.5: 2) as developping agent, launch, take out, dry.Spray is the mixed solution (mixing before use) with 1% potassium ferricyanide solution (1: 1) with 1% liquor ferri trichloridi, in test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color.
The assay of D, red sage root characteristic component tanshin polyphenolic acid B:
Measure according to high performance liquid chromatography (annex VI D of " Chinese Pharmacopoeia " version in 2010).
Chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking methyl alcohol-acetonitrile-formic acid-water (26: 8: 1: 65) as mobile phase; Detect wavelength 286nm; Theoretical cam curve is calculated and should be not less than 2000 by tanshin polyphenolic acid B peak.
It is appropriate that tanshin polyphenolic acid B reference substance is got in the preparation of reference substance solution, accurately weighed, adds 75% methyl alcohol and make the solution of every 1ml containing 50 μ g, to obtain final product.
This drug substance contents is got in the preparation of need testing solution, and porphyrize is got about 0.3g, accurately weighed, to put in tool plug conical flask, precision adds 75% methyl alcohol 50ml, close plug, weighed weight, adds hot reflux 1 hour, let cool, more weighed weight, supply the weight of less loss with 75% methyl alcohol, shake up, get centrifugal 10 minutes of 10ml (3000 revs/min), get supernatant, to obtain final product.
Determination method is accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and to obtain final product.
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| CN104792916A (en) * | 2015-04-24 | 2015-07-22 | 四川逢春制药有限公司 | Detection method of hepatitis B treating capsule as traditional Chinese medicine preparation |
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