CN105004810A - Rheumatism bone pain tablet quality standard and test method thereof - Google Patents
Rheumatism bone pain tablet quality standard and test method thereof Download PDFInfo
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Abstract
The present invention discloses a rheumatism bone pain tablet quality standard and a test method thereof. The quality standard comprises a character indicator, a microscopic identification indicator, a thin-layer chromatography indicator, diester type alkaloid dose limited examination and a content determination indicator. The test method comprises: (1) adopting eye determining, nose smelling and mouth tasting to test the character; (2) adopting microscope observation to perform the microscopic identification; (3) adopting a thin-layer chromatography method to test the thin-layer chromatography indicator; (4) adopting a high-performance liquid chromatography method to test the liquid chromatography identification indicator; (5) adopting a high-performance liquid chromatography method to perform the diester type alkaloid dose limited examination; and (6) adopting a high-performance liquid chromatography method to test the content determination indicator. Compared with the existing standard, the quality standard and the test method of the present invention have the following advantages that the standard is completely stringent, and the effectiveness, the quality controllability and the stability of the rheumatism bone pain tablet can be effectively enhanced.
Description
Technical field
The present invention relates to medicine detection field, be specifically related to quality standard and the method for inspection thereof for the treatment of rheumatic ostealgia sheet.
Background technology
Treating rheumatic ostealgia sheet cures mainly warming channel and expelling cold, removes obstruction in channels to relieve pain.Sick for the numbness caused by cold-dampness impatency channels and collaterals, disease sees lumbar vertebrae pain, extremities joint crymodynia; Rheumatic arthritis is shown in above-mentioned patient.The prescription for the treatment of rheumatic ostealgia sheet is aconiti preparata,radix 103g, wild aconite root 103g, Chinese ephedra 103g, pawpaw 103 g, safflower 103g, Fructus Mume 103g, Radix Glycyrrhizae 103g, and method for making is: above seven tastes, gets aconiti preparata,radix, wild aconite root, licorice powder be broken into fine powder, sieve, mix; The four taste boiling secondaries such as all the other safflowers, each 2 hours, collecting decoction, filter, filtrate was condensed into paste, adds above-mentioned fine powder, and mixing, makes particle, dry, adds 0.5% dolomol mixing, is pressed into 1000, film coating, obtains final product.The test stone that treating rheumatic ostealgia sheet now performs is State Food and Drug Administration's standard (trying) YBZ04152005, this standard comprises: (1) characteristic index: this product is Film coated tablets, aobvious brown to sepia after removing film-coating, bitter; (2) thin-layer chromatography index: being that reference substance is differentiated Radix Glycyrrhizae with enoxolone in test sample chromatogram, is that reference substance is differentiated Chinese ephedra with ephedrine hydrochloride; (4) aconitine limit inspection: with every 1ml containing the contrast solution of aconitine 1mg, to sample by ripple once chromatography carry out aconitine limit inspection; The spot of reference substance should be less than with the spot that occurs in reference substance chromatogram same position or not occur spot in test sample chromatogram; (5) assay index: the every sheet of this product in aconitine, should be 0.25 ~ 0.80mg containing rhizome of Chinese monkshood total alkaloids.The shortcoming of this standard is: not comprehensively, poor, the poor accuracy of specificity, be unfavorable for that the quality of product accurately controls.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, and a kind for the treatment of rheumatic ostealgia tablet quality standard and the method for inspection thereof are provided, by determining quality standard and the method for inspection thereof, the validity of this medicine, quality controllability and stability can be strengthened.
Technical scheme of the present invention is as follows:
Treating rheumatic ostealgia tablet quality standard and the method for inspection thereof, it is characterized in that: the quality standard of this tablet comprises characteristic index, microscopical characters index, liquid chromatography identification beacon, thin-layer chromatography index, diester-type alkaloids limit examine and assay index, and described indices is as follows:
(1) characteristic index: this product is Film coated tablets, aobvious tawny after removing film-coating; Mildly bitter flavor, acid;
(2) microscopical characters index: microexamination has the microscopic features of aconiti preparata,radix, wild aconite root, licorice medicinal materials;
(3) indentification by TLC index: be control medicinal material and liquiritin with Radix Glycyrrhizae in test sample chromatogram for reference substance is differentiated Radix Glycyrrhizae;
(4) liquid chromatography identification beacon: in test sample chromatogram with ephedrine hydrochloride and pseudoephedrine hydrochloride for reference substance is differentiated Chinese ephedra;
(5) diester-type alkaloids limit examine: with the mixing contrast solution of every 1ml containing aconitine 0.3mg, Hypaconitine 0.18mg, mesaconine 1mg, limit examine is carried out to sample; The every sheet of this product contains diester-type alkaloids with aconitine (C
34h
47nO
11), Hypaconitine (C
33h
45nO
11) and mesaconine (C
33h
45nO
11) total amount, must not 0.072mg be crossed;
(6) assay index: the every sheet of this product contains aconiti preparata,radix, wild aconite root with benzoyl aconine (C
32h
45nO
10), benzoyl time aconine (C
31h
43nO
9) and benzoylmesaconine (C
31h
43nO
10) total amount, should be 0.081 ~ 0.198mg; The every sheet of this product contains Chinese ephedra with ephedrine hydrochloride (C
10h
15and pseudoephedrine hydrochloride (C NOHCl)
10h
15nOHCl) total amount, must not be less than 0.27mg; The every sheet of this product contains Radix Glycyrrhizae with ammonium glycyrrhetate (C
42h
42o10NH4) count, must not 0.70mg be less than.
The method of inspection of described index is as follows: (1) characteristic index: adopt range estimation, nasil and mouth to taste; (2) microscopical characters index: adopt microscopic examination; (3) thin-layer chromatography index: adopt thin-layered chromatography; (4) liquid chromatography identification beacon: adopt high performance liquid chromatography; (5) diester-type alkaloids limit examine: adopt high performance liquid chromatography; (5) assay index: adopt high performance liquid chromatography.
Described microscopical characters method is:
(1) instrument: microscope, micrometer, mortar, microslide, cover glass, spirit lamp
(2) reagent: chloral hydrate test solution
(3) method of inspection: measure with reference to medicinal material and prescribed preparation microscopical characters method.
In described indentification by TLC, the method for inspection of Radix Glycyrrhizae is:
(1) instrument: mortar, graduated cylinder, round-bottomed flask, straight cold finger, electric jacket, filtrator, counter balance, evaporating dish, sample applicator, silica gel g thin-layer plate, ultraviolet point sample analyser, chromatography cylinder, baking oven
(2) control medicinal material: Radix Glycyrrhizae control medicinal material, liquiritin reference substance
(3) reagent: methyl alcohol, hydrochloric acid, ethyl acetate, methenyl choloride, formic acid
(4) method of inspection: get this product 6, porphyrize, adds 50% methyl alcohol 40ml, ultrasonic process 30 minutes, filters, filtrate evaporate to dryness, the residue 30ml that adds water makes dissolving, salt adding acid for adjusting pH value to 2 ~ 3, extract 2 times with ethyl acetate jolting, every 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as need testing solution.Another extracting Radix Glycyrrhizae control medicinal material 0.5g, is made in the same way of control medicinal material solution.Extracting Radix Glycyrrhizae glycosides reference substance again, adds methyl alcohol and makes the solution of every 1ml containing 1mg, product solution in contrast.Test according to thin-layered chromatography Chinese Pharmacopoeia version in 2010 annex VI B, draw need testing solution and each 10 μ l of reference substance solution, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with methenyl choloride-methyl alcohol-formic acid (5:1:0.1) for developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear.In test sample chromatogram, on the position corresponding with reference substance chromatogram to control medicinal material, aobvious identical spot.
Described liquid chromatography differentiates that the method for inspection of epheday intermedia is: test sample chromatogram presents the chromatographic peak identical with pseudoephedrine control product retention time with ephedrine.
The method of inspection of described diester-type alkaloids limit examine is:
(1) instrument: high performance liquid chromatograph, analytical balance, transfer pipet, ultrasonic cleaner, tool plug conical flask, brown measuring bottle, 0.45 μm of miillpore filter;
(2) reagent: hydrochloric acid, acetonitrile, ammonia, methyl alcohol;
(3) reference substance: aconitine reference substance, Hypaconitine reference substance, mesaconine reference substance;
(4) method of inspection: measure with reference to high performance liquid chromatography (Chinese Pharmacopoeia version in 2010 annex VI D), specific as follows:
chromatographic condition and system suitabilitytake octadecylsilane chemically bonded silica as filling agent; With acetonitrile-tetrahydrofuran (25:15) for mobile phase A, with 0.1mol/L ammonium acetate solution (every 1000ml adds glacial acetic acid 0.5ml) for Mobile phase B, the regulation according to the form below carries out gradient elution; Determined wavelength is 235nm; Number of theoretical plate calculates should be not less than 2000 by mesaconine peak;
the preparation of reference substance solutionget aconitine reference substance, Hypaconitine reference substance, mesaconine reference substance in right amount, accurately weighed, add mobile phase and make the mixed solution of every 1ml containing aconitine 0.3mg, Hypaconitine 0.18mg, mesaconine 1mg respectively, to obtain final product;
the preparation of need testing solutionget this product 10, accurately weighed, porphyrize, get 2g, accurately weighed, put in tool plug conical flask, precision adds 0.1mol/L hydrochloric acid solution 25ml, close plug, weighed weight, ultrasonic process (power 400W, frequency 40kHz) 40 minutes and time jolting, let cool, weighed weight again, the weight of less loss is supplied with 0.1mol/L hydrochloric acid solution, shake up, centrifugal, precision measures supernatant 10ml, be added in solid-phase extraction column (with the agent of mixed type cation exchange reverse phase absorption for filling agent, 150mg or 200mg, capacity is 6ml, use acetonitrile successively in advance, the each 6ml wash-out of water) on, successively with water 3ml, ammonia solution (5 → 100), water, methyl alcohol, the each 5ml wash-out of acetonitrile, after eluent flows to end, place 5 minutes, continue with the mixed solution 10ml wash-out of acetonitrile-strong ammonia solution (90:10), collect eluent, in less than 40 DEG C recovered under reduced pressure to dry, precision adds mobile phase 3ml makes dissolving, filter, obtain,
determination methodaccurate absorption reference substance solution and each 10 μ 1 of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
The assay method of inspection of described aconiti preparata,radix and wild aconite root is except reference substance solution preparation, all identical with the method for inspection of above-mentioned diester-type alkaloids limit examine; Being prepared as follows of described reference substance solution: get benzoyl aconine reference substance, benzoyl time aconine reference substance, benzoylmesaconine reference substance are appropriate, accurately weighed, add mobile phase and make the mixed solution of every 1ml containing benzoyl aconine 20 μ g, benzoyl time aconine 0.1mg, benzoylmesaconine 80 μ g, to obtain final product.
The assay method of inspection of described Chinese ephedra is carried out according to high performance liquid chromatography (annex VI D):
chromatographic condition and system suitabilitytake octadecylsilane chemically bonded silica as filling agent; With acetonitrile-0.1% phosphoric acid (with triethylamine adjust pH to 3.0) (5:95) for mobile phase; Determined wavelength is 207nm; Number of theoretical plate calculates should be not less than 4000 by ephedrine hydrochloride peak;
the preparation of reference substance solutionget ephedrine hydrochloride reference substance, pseudoephedrine hydrochloride reference substance thermophilic, accurately weighed, add methyl alcohol and make every 1ml respectively respectively containing the mixed solution of 10 μ g, to obtain final product;
the preparation of need testing solutionprecision measures the need testing solution 1ml described in claim 7, adds mobile phase and is diluted to 10ml, to obtain final product;
determination methodaccurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
The assay method of inspection of described Radix Glycyrrhizae is carried out according to high performance liquid chromatography (annex VI D):
chromatographic condition and system suitabilitytake octadecylsilane chemically bonded silica as filling agent; With methanol-water-glacial acetic acid-triethylamine (62:38:1:0.3) for mobile phase; Determined wavelength is 270nm; Number of theoretical plate calculates should be not less than 3000 by glycyrrhizic acid peak;
the preparation of reference substance solutionextracting Radix Glycyrrhizae acid ammonium reference substance thermophilic, accurately weighed, add 50% methyl alcohol and make every 1ml respectively respectively containing the mixed solution of 30 μ g, to obtain final product;
the preparation of need testing solutionget this product 10, accurately weighed, porphyrize, gets about 0.2g, accurately weighed, puts in 50ml measuring bottle, adds 50% methyl alcohol 40ml, and ultrasonic process (power 400W, frequency 40kHz) 30 minutes, lets cool, and with 5% methanol dilution to scale, shakes up, and filters, to obtain final product;
determination methodaccurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
The invention has the advantages that:
The present invention, relative to act.std, adds microscopical characters index; Be control medicinal material and liquiritin respectively with Radix Glycyrrhizae in thin-layer chromatography index for reference substance is differentiated Radix Glycyrrhizae, with ephedrine hydrochloride and pseudoephedrine hydrochloride for reference substance is differentiated Chinese ephedra, reference substance arranges more diversified, and identification result is comprehensively more scientific, and accuracy is high; Adopt diester-type alkaloids limit examine to replace traditional aconitine limit inspection, and inspection method becomes high performance liquid chromatography from thin-layered chromatography, becomes quantitative check from qualitative examination, accuracy is higher; In assay index, be different from and traditional only measure rhizome of Chinese monkshood total alkaloid content with aconitine, quality standard of the present invention directly measures the aconiti preparata,radix in medicinal material and wild aconite root content, and have selected reference substance in 3, and result more accurately comprehensively; Further comprises the assay of Chinese ephedra and Radix Glycyrrhizae simultaneously in assay index, effectively accomplished all to carry out assay to several compositions main in treating rheumatic ostealgia sheet.To sum up, quality standard of the present invention and the relative existing standard of the method for inspection more comprehensive strict, effectively can strengthen the validity for the treatment of rheumatic ostealgia sheet, quality controllability and stability.
Embodiment
The present invention will be further described below.
Technical scheme of the present invention is as follows:
Treating rheumatic ostealgia tablet quality standard and the method for inspection thereof, it is characterized in that: the quality standard of this tablet comprises characteristic index, microscopical characters index, liquid chromatography identification beacon, thin-layer chromatography index, diester-type alkaloids limit examine and assay index, and described indices is as follows:
(1) characteristic index: this product is Film coated tablets, aobvious tawny after removing film-coating; Mildly bitter flavor, acid;
(2) microscopical characters index: microexamination has the microscopic features of aconiti preparata,radix, wild aconite root, licorice medicinal materials;
(3) indentification by TLC index: be control medicinal material and liquiritin with Radix Glycyrrhizae in test sample chromatogram for reference substance is differentiated Radix Glycyrrhizae;
(4) liquid chromatography identification beacon: in test sample chromatogram with ephedrine hydrochloride and pseudoephedrine hydrochloride for reference substance is differentiated Chinese ephedra;
(5) diester-type alkaloids limit examine: with the mixing contrast solution of every 1ml containing aconitine 0.3mg, Hypaconitine 0.18mg, mesaconine 1mg, limit examine is carried out to sample; The every sheet of this product contains diester-type alkaloids with aconitine (C
34h
47nO
11), Hypaconitine (C
33h
45nO
11) and mesaconine (C
33h
45nO
11) total amount, must not 0.072mg be crossed;
(6) assay index: the every sheet of this product contains aconiti preparata,radix, wild aconite root with benzoyl aconine (C
32h
45nO
10), benzoyl time aconine (C
31h
43nO
9) and benzoylmesaconine (C
31h
43nO
10) total amount, should be 0.081 ~ 0.198mg; The every sheet of this product contains Chinese ephedra with ephedrine hydrochloride (C
10h
15and pseudoephedrine hydrochloride (C NOHCl)
10h
15nOHCl) total amount, must not be less than 0.27mg; The every sheet of this product contains Radix Glycyrrhizae with ammonium glycyrrhetate (C
42h
42o10NH4) count, must not 0.70mg be less than.
The method of inspection of described index is as follows: (1) characteristic index: adopt range estimation, nasil and mouth to taste; (2) microscopical characters index: adopt microscopic examination; (3) thin-layer chromatography index: adopt thin-layered chromatography; (4) liquid chromatography identification beacon: adopt high performance liquid chromatography; (5) diester-type alkaloids limit examine: adopt high performance liquid chromatography; (5) assay index: adopt high performance liquid chromatography.
Described microscopical characters method is:
(1) instrument: microscope, micrometer, mortar, microslide, cover glass, spirit lamp
(2) reagent: chloral hydrate test solution
(3) method of inspection: measure with reference to medicinal material and prescribed preparation microscopical characters method.
In described indentification by TLC, the method for inspection of Radix Glycyrrhizae is:
(1) instrument: mortar, graduated cylinder, round-bottomed flask, straight cold finger, electric jacket, filtrator, counter balance, evaporating dish, sample applicator, silica gel g thin-layer plate, ultraviolet point sample analyser, chromatography cylinder, baking oven
(2) control medicinal material: Radix Glycyrrhizae control medicinal material, liquiritin reference substance
(3) reagent: methyl alcohol, hydrochloric acid, ethyl acetate, methenyl choloride, formic acid
(4) method of inspection: get this product 6, porphyrize, adds 50% methyl alcohol 40ml, ultrasonic process 30 minutes, filters, filtrate evaporate to dryness, the residue 30ml that adds water makes dissolving, salt adding acid for adjusting pH value to 2 ~ 3, extract 2 times with ethyl acetate jolting, every 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as need testing solution.Another extracting Radix Glycyrrhizae control medicinal material 0.5g, is made in the same way of control medicinal material solution.Extracting Radix Glycyrrhizae glycosides reference substance again, adds methyl alcohol and makes the solution of every 1ml containing 1mg, product solution in contrast.Test according to thin-layered chromatography Chinese Pharmacopoeia version in 2010 annex VI B, draw need testing solution and each 10 μ l of reference substance solution, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with methenyl choloride-methyl alcohol-formic acid (5:1:0.1) for developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear.In test sample chromatogram, on the position corresponding with reference substance chromatogram to control medicinal material, aobvious identical spot.
Described liquid chromatography differentiates that the method for inspection of epheday intermedia is: test sample chromatogram presents the chromatographic peak identical with pseudoephedrine control product retention time with ephedrine.
The method of inspection of described diester-type alkaloids limit examine is:
(1) instrument: high performance liquid chromatograph, analytical balance, transfer pipet, ultrasonic cleaner, tool plug conical flask, brown measuring bottle, 0.45 μm of miillpore filter;
(2) reagent: hydrochloric acid, acetonitrile, ammonia, methyl alcohol;
(3) reference substance: aconitine reference substance, Hypaconitine reference substance, mesaconine reference substance;
(4) method of inspection: measure with reference to high performance liquid chromatography (Chinese Pharmacopoeia version in 2010 annex VI D), specific as follows:
chromatographic condition and system suitabilitytake octadecylsilane chemically bonded silica as filling agent; With acetonitrile-tetrahydrofuran (25:15) for mobile phase A, with 0.1mol/L ammonium acetate solution (every 1000ml adds glacial acetic acid 0.5ml) for Mobile phase B, the regulation according to the form below carries out gradient elution; Determined wavelength is 235nm; Number of theoretical plate calculates should be not less than 2000 by mesaconine peak;
the preparation of reference substance solutionget aconitine reference substance, Hypaconitine reference substance, mesaconine reference substance in right amount, accurately weighed, add mobile phase and make the mixed solution of every 1ml containing aconitine 0.3mg, Hypaconitine 0.18mg, mesaconine 1mg respectively, to obtain final product;
the preparation of need testing solutionget this product 10, accurately weighed, porphyrize, get 2g, accurately weighed, put in tool plug conical flask, precision adds 0.1mol/L hydrochloric acid solution 25ml, close plug, weighed weight, ultrasonic process (power 400W, frequency 40kHz) 40 minutes and time jolting, let cool, weighed weight again, the weight of less loss is supplied with 0.1mol/L hydrochloric acid solution, shake up, centrifugal, precision measures supernatant 10ml, be added in solid-phase extraction column (with the agent of mixed type cation exchange reverse phase absorption for filling agent, 150mg or 200mg, capacity is 6ml, use acetonitrile successively in advance, the each 6ml wash-out of water) on, successively with water 3ml, ammonia solution (5 → 100), water, methyl alcohol, the each 5ml wash-out of acetonitrile, after eluent flows to end, place 5 minutes, continue with the mixed solution 10ml wash-out of acetonitrile-strong ammonia solution (90:10), collect eluent, in less than 40 DEG C recovered under reduced pressure to dry, precision adds mobile phase 3ml makes dissolving, filter, obtain,
determination methodaccurate absorption reference substance solution and each 10 μ 1 of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
The assay method of inspection of described aconiti preparata,radix and wild aconite root is except reference substance solution preparation, all identical with the method for inspection of above-mentioned diester-type alkaloids limit examine; Being prepared as follows of described reference substance solution: get benzoyl aconine reference substance, benzoyl time aconine reference substance, benzoylmesaconine reference substance are appropriate, accurately weighed, add mobile phase and make the mixed solution of every 1ml containing benzoyl aconine 20 μ g, benzoyl time aconine 0.1mg, benzoylmesaconine 80 μ g, to obtain final product.
The assay method of inspection of described Chinese ephedra is carried out according to high performance liquid chromatography (annex VI D):
chromatographic condition and system suitabilitytake octadecylsilane chemically bonded silica as filling agent; With acetonitrile-0.1% phosphoric acid (with triethylamine adjust pH to 3.0) (5:95) for mobile phase; Determined wavelength is 207nm; Number of theoretical plate calculates should be not less than 4000 by ephedrine hydrochloride peak;
the preparation of reference substance solutionget ephedrine hydrochloride reference substance, pseudoephedrine hydrochloride reference substance thermophilic, accurately weighed, add methyl alcohol and make every 1ml respectively respectively containing the mixed solution of 10 μ g, to obtain final product;
the preparation of need testing solutionprecision measures the need testing solution 1ml described in claim 7, adds mobile phase and is diluted to 10ml, to obtain final product;
determination methodaccurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
The assay method of inspection of described Radix Glycyrrhizae is carried out according to high performance liquid chromatography (annex VI D):
chromatographic condition and system suitabilitytake octadecylsilane chemically bonded silica as filling agent; With methanol-water-glacial acetic acid-triethylamine (62:38:1:0.3) for mobile phase; Determined wavelength is 270nm; Number of theoretical plate calculates should be not less than 3000 by glycyrrhizic acid peak;
the preparation of reference substance solutionextracting Radix Glycyrrhizae acid ammonium reference substance thermophilic, accurately weighed, add 50% methyl alcohol and make every 1ml respectively respectively containing the mixed solution of 30 μ g, to obtain final product;
the preparation of need testing solutionget this product 10, accurately weighed, porphyrize, gets about 0.2g, accurately weighed, puts in 50ml measuring bottle, adds 50% methyl alcohol 40ml, and ultrasonic process (power 400W, frequency 40kHz) 30 minutes, lets cool, and with 5% methanol dilution to scale, shakes up, and filters, to obtain final product;
determination methodaccurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
Claims (9)
1. treating rheumatic ostealgia tablet quality standard and the method for inspection thereof, it is characterized in that: the quality standard of this tablet comprises characteristic index, microscopical characters index, liquid chromatography identification beacon, thin-layer chromatography index, diester-type alkaloids limit examine and assay index, and described indices is as follows:
(1) characteristic index: this product is Film coated tablets, aobvious tawny after removing film-coating; Mildly bitter flavor, acid;
(2) microscopical characters index: microexamination has the microscopic features of aconiti preparata,radix, wild aconite root, licorice medicinal materials;
(3) indentification by TLC index: be control medicinal material and liquiritin with Radix Glycyrrhizae in test sample chromatogram for reference substance is differentiated Radix Glycyrrhizae;
(4) liquid chromatography identification beacon: in test sample chromatogram with ephedrine hydrochloride and pseudoephedrine hydrochloride for reference substance is differentiated Chinese ephedra;
(5) diester-type alkaloids limit examine: with the mixing contrast solution of every 1ml containing aconitine 0.3mg, Hypaconitine 0.18mg, mesaconine 1mg, limit examine is carried out to sample; The every sheet of this product contains diester-type alkaloids with aconitine (C
34h
47nO
11), Hypaconitine (C
33h
45nO
11) and mesaconine (C
33h
45nO
11) total amount, must not 0.072mg be crossed;
(6) assay index: the every sheet of this product contains aconiti preparata,radix, wild aconite root with benzoyl aconine (C
32h
45nO
10), benzoyl time aconine (C
31h
43nO
9) and benzoylmesaconine (C
31h
43nO
10) total amount, should be 0.081 ~ 0.198mg; The every sheet of this product contains Chinese ephedra with ephedrine hydrochloride (C
10h
15and pseudoephedrine hydrochloride (C NOHCl)
10h
15nOHCl) total amount, must not be less than 0.27mg; The every sheet of this product contains Radix Glycyrrhizae with ammonium glycyrrhetate (C
42h
42o10NH4) count, must not 0.70mg be less than.
2. treating rheumatic ostealgia tablet quality standard according to claim 1 and the method for inspection thereof, is characterized in that, the method for inspection of described index is as follows: (1) characteristic index: adopt range estimation, nasil and mouth to taste; (2) microscopical characters index: adopt microscopic examination; (3) thin-layer chromatography index: adopt thin-layered chromatography; (4) liquid chromatography identification beacon: adopt high performance liquid chromatography; (5) diester-type alkaloids limit examine: adopt high performance liquid chromatography; (5) assay index: adopt high performance liquid chromatography.
3. treating rheumatic ostealgia tablet quality standard according to claim 1 and the method for inspection thereof, is characterized in that, described microscopical characters method is:
(1) instrument: microscope, micrometer, mortar, microslide, cover glass, spirit lamp
(2) reagent: chloral hydrate test solution
(3) method of inspection: measure with reference to medicinal material and prescribed preparation microscopical characters method.
4. treating rheumatic ostealgia tablet quality standard according to claim 1 and the method for inspection thereof, is characterized in that, in described indentification by TLC, the method for inspection of Radix Glycyrrhizae is:
(1) instrument: mortar, graduated cylinder, round-bottomed flask, straight cold finger, electric jacket, filtrator, counter balance, evaporating dish, sample applicator, silica gel g thin-layer plate, ultraviolet point sample analyser, chromatography cylinder, baking oven
(2) control medicinal material: Radix Glycyrrhizae control medicinal material, liquiritin reference substance
(3) reagent: methyl alcohol, hydrochloric acid, ethyl acetate, methenyl choloride, formic acid
(4) method of inspection: get this product 6, porphyrize, adds 50% methyl alcohol 40ml, ultrasonic process 30 minutes, filters, filtrate evaporate to dryness, the residue 30ml that adds water makes dissolving, salt adding acid for adjusting pH value to 2 ~ 3, extract 2 times with ethyl acetate jolting, every 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Another extracting Radix Glycyrrhizae control medicinal material 0.5g, is made in the same way of control medicinal material solution; Extracting Radix Glycyrrhizae glycosides reference substance again, adds methyl alcohol and makes the solution of every 1ml containing 1mg, product solution in contrast; Test according to thin-layered chromatography Chinese Pharmacopoeia version in 2010 annex VI B, draw need testing solution and each 10 μ l of reference substance solution, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with methenyl choloride-methyl alcohol-formic acid (5:1:0.1) for developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear; In test sample chromatogram, on the position corresponding with reference substance chromatogram to control medicinal material, aobvious identical spot.
5. treating rheumatic ostealgia tablet quality standard according to claim 1 and the method for inspection thereof, is characterized in that, described liquid chromatography differentiates that the method for inspection of epheday intermedia is: test sample chromatogram presents the chromatographic peak identical with pseudoephedrine control product retention time with ephedrine.
6. treating rheumatic ostealgia tablet quality standard according to claim 1 and the method for inspection thereof, is characterized in that, the method for inspection of described diester-type alkaloids limit examine is:
(1) instrument: high performance liquid chromatograph, analytical balance, transfer pipet, ultrasonic cleaner, tool plug conical flask, brown measuring bottle, 0.45 μm of miillpore filter;
(2) reagent: hydrochloric acid, acetonitrile, ammonia, methyl alcohol;
(3) reference substance: aconitine reference substance, Hypaconitine reference substance, mesaconine reference substance;
(4) method of inspection: measure with reference to high performance liquid chromatography (Chinese Pharmacopoeia version in 2010 annex VI D), specific as follows:
chromatographic condition and system suitabilitytake octadecylsilane chemically bonded silica as filling agent; With acetonitrile-tetrahydrofuran (25:15) for mobile phase A, with 0.1mol/L ammonium acetate solution (every 1000ml adds glacial acetic acid 0.5ml) for Mobile phase B, the regulation according to the form below carries out gradient elution; Determined wavelength is 235nm; Number of theoretical plate calculates should be not less than 2000 by mesaconine peak;
the preparation of reference substance solutionget aconitine reference substance, Hypaconitine reference substance, mesaconine reference substance in right amount, accurately weighed, add mobile phase and make the mixed solution of every 1ml containing aconitine 0.3mg, Hypaconitine 0.18mg, mesaconine 1mg respectively, to obtain final product;
the preparation of need testing solutionget this product 10, accurately weighed, porphyrize, get 2g, accurately weighed, put in tool plug conical flask, precision adds 0.1mol/L hydrochloric acid solution 25ml, close plug, weighed weight, ultrasonic process (power 400W, frequency 40kHz) 40 minutes and time jolting, let cool, weighed weight again, the weight of less loss is supplied with 0.1mol/L hydrochloric acid solution, shake up, centrifugal, precision measures supernatant 10ml, be added in solid-phase extraction column (with the agent of mixed type cation exchange reverse phase absorption for filling agent, 150mg or 200mg, capacity is 6ml, use acetonitrile successively in advance, the each 6ml wash-out of water) on, successively with water 3ml, ammonia solution (5 → 100), water, methyl alcohol, the each 5ml wash-out of acetonitrile, after eluent flows to end, place 5 minutes, continue with the mixed solution 10ml wash-out of acetonitrile-strong ammonia solution (90:10), collect eluent, in less than 40 DEG C recovered under reduced pressure to dry, precision adds mobile phase 3ml makes dissolving, filter, obtain,
determination methodaccurate absorption reference substance solution and each 10 μ 1 of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
7. treating rheumatic ostealgia tablet quality standard according to claim 1 and the method for inspection thereof, it is characterized in that, the assay method of inspection of described aconiti preparata,radix and wild aconite root is except reference substance solution preparation, all identical with the method for inspection of above-mentioned diester-type alkaloids limit examine; Being prepared as follows of described reference substance solution: get benzoyl aconine reference substance, benzoyl time aconine reference substance, benzoylmesaconine reference substance are appropriate, accurately weighed, add mobile phase and make the mixed solution of every 1ml containing benzoyl aconine 20 μ g, benzoyl time aconine 0.1mg, benzoylmesaconine 80 μ g, to obtain final product.
8. treating rheumatic ostealgia tablet quality standard according to claim 1 and the method for inspection thereof, is characterized in that, the assay method of inspection of described Chinese ephedra is carried out according to high performance liquid chromatography (annex VI D):
chromatographic condition and system suitabilitytake octadecylsilane chemically bonded silica as filling agent; With acetonitrile-0.1% phosphoric acid (with triethylamine adjust pH to 3.0) (5:95) for mobile phase; Determined wavelength is 207nm; Number of theoretical plate calculates should be not less than 4000 by ephedrine hydrochloride peak;
the preparation of reference substance solutionget ephedrine hydrochloride reference substance, pseudoephedrine hydrochloride reference substance thermophilic, accurately weighed, add methyl alcohol and make every 1ml respectively respectively containing the mixed solution of 10 μ g, to obtain final product;
the preparation of need testing solutionprecision measures the need testing solution 1ml described in claim 7, adds mobile phase and is diluted to 10ml, to obtain final product;
determination methodaccurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
9. treating rheumatic ostealgia tablet quality standard according to claim 1 and the method for inspection thereof, is characterized in that, the assay method of inspection of described Radix Glycyrrhizae is carried out according to high performance liquid chromatography (annex VI D):
chromatographic condition and system suitabilitytake octadecylsilane chemically bonded silica as filling agent; With methanol-water-glacial acetic acid-triethylamine (62:38:1:0.3) for mobile phase; Determined wavelength is 270nm; Number of theoretical plate calculates should be not less than 3000 by glycyrrhizic acid peak;
the preparation of reference substance solutionextracting Radix Glycyrrhizae acid ammonium reference substance thermophilic, accurately weighed, add 50% methyl alcohol and make every 1ml respectively respectively containing the mixed solution of 30 μ g, to obtain final product;
the preparation of need testing solutionget this product 10, accurately weighed, porphyrize, gets about 0.2g, accurately weighed, puts in 50ml measuring bottle, adds 50% methyl alcohol 40ml, and ultrasonic process (power 400W, frequency 40kHz) 30 minutes, lets cool, and with 5% methanol dilution to scale, shakes up, and filters, to obtain final product;
determination methodaccurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
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