CN1857620A - Quality control method for visual fatigue treating medicine preparation - Google Patents
Quality control method for visual fatigue treating medicine preparation Download PDFInfo
- Publication number
- CN1857620A CN1857620A CN 200610200321 CN200610200321A CN1857620A CN 1857620 A CN1857620 A CN 1857620A CN 200610200321 CN200610200321 CN 200610200321 CN 200610200321 A CN200610200321 A CN 200610200321A CN 1857620 A CN1857620 A CN 1857620A
- Authority
- CN
- China
- Prior art keywords
- solution
- preparation
- reference substance
- methanol
- adds
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The present invention relates to the quality control method for visual fatigue treating medicine preparation. The quality control method includes character checking, identification and content measurement. The identification is the thin layer identification of white peony root and cassia seed; and the content measurement includes measurement of white peony root. Compared with available technology, the present invention has the advantages of high precision, high stability, high repeatability, high recovery rate and accurate measurement result. The present invention can ensure the high quality and clinical curative effect of the visual fatigue treating medicine preparation.
Description
Technical field: the present invention relates to a kind of method of quality control for the treatment of asthenopic pharmaceutical preparation, belong to the technical field of medicine being carried out quality control.
Background technology: along with various electric equipments by the cathode ray tube assembling such as computer, television set, video recorder and electronic game machine enter society and family, people owing to these electronic equipments of life-time service, cause excess eye-using in working and learning.Studies show that excess eye-using, too much use computer terminal etc. can cause asthenopia, its cardinal symptom is: eye acid; ophthalmic bloated, eye is tired uncomfortable, and attention is difficult to concentrate; conjunctiva or keratitis, even visual deterioration, intraocular pressure raises; form myopia; usually also follow General Symptoms, ache the emotion agitation as shoulder, neck, the back of the body, waist etc.; autonomic nervous dysfunctions etc. have influenced people's life and healthy greatly.Tradition
Western medicine therapy is mainly adopted in asthenopic treatment, and its major measure is the replacement therapy of tear composition and the secretion that promotes tear, but curative effect is undesirable and have certain toxic and side effects.The applicant has researched and developed the asthenopic pharmaceutical preparation of a kind of treatment (application number is 200510200488.3), to asthenopic good effect and have no side effect.If but do not have the strict quality standard, the product quality reliability of producing would be not high, quality is unstable, thereby can influence the clinical efficacy of medicine.
Summary of the invention:
The objective of the invention is to: a kind of method of quality control for the treatment of asthenopic pharmaceutical preparation is provided, and said preparation comprises capsule, tablet, granule, drop pill, oral liquid, syrup or eye drop; The present invention has studied and defined feasible discriminating and content assaying method according to respectively distinguish the flavor of in the prescription content, characteristic and the preparation technology thereof of medical material, with the quality of the asthenopic pharmaceutical preparation of control treatment effectively, thereby guarantees the clinical efficacy of this preparation.
The asthenopic pharmaceutical preparation of treatment of the present invention is to constitute like this: according to listed as parts by weight, it adds suitable adjuvant for 4～9 parts by 6～15 parts of the Radix Paeoniae Albas, 5～12 parts of Herba Dendrobiis, 6～15 parts of Semen Cassiaes and Fructus Leonuri and is prepared from.
The preparation method for the treatment of asthenopic pharmaceutical preparation is: take by weighing the Radix Paeoniae Alba, Herba Dendrobii, Semen Cassiae and Fructus Leonuri four Chinese medicine material, decoct with water 1～3 time, add for the first time 8～12 times of water gagings, add for the second time 6～10 times of water gagings, each 0.5～2.5 hour, collecting decoction filters, and the survey relative density was 1.10～1.15 clear paste when filtrate was concentrated into 60 ℃, adding ethanol after cooling makes and contains alcohol amount and reach 60%～80%, left standstill 10～14 hours, and filtered, decompression filtrate recycling ethanol and to survey relative density when being concentrated into 60 ℃ be 1.25～1.30 thick paste, dry, pulverize, sieve, add suitable adjuvant then and make various dosage form.
Method of quality control of the present invention mainly comprise in character, inspection, discriminating, the assay project partly or entirely; Wherein character should meet the pertinent regulations under each preparation item; Discriminating is that the thin layer of the Radix Paeoniae Alba, Semen Cassiae is differentiated; Inspection should meet " the pertinent regulations under each preparation item of appendix of Chinese pharmacopoeia version in 2000; Assay is the assay to the Radix Paeoniae Alba in the preparation.
The discrimination method of the Radix Paeoniae Alba is to be contrast with the peoniflorin reference substance in this preparation, and with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is the thin layer discrimination method of developing solvent.
The discrimination method of Semen Cassiae is to be contrast with the chrysophanol reference substance in this preparation, and with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is the thin layer discrimination method of developing solvent.
Discrimination method comprises the part or all of of following project:
(1) get this preparation or its content, add ethanol, jolting filters, and filtrate evaporate to dryness, residue add ethanol makes dissolving, as need testing solution; It is an amount of that other gets the peoniflorin reference substance, adds ethanol and make solution, in contrast product solution; According to " appendix a VIB of Chinese pharmacopoeia version in 2000 thin layer chromatography test, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is developing solvent, launches, and takes out, dry, spray is with the vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;
(2) get this preparation or its content, add methanol, dipping filters, and filtrate evaporate to dryness, residue add water makes dissolving, adds hydrochloric acid again, puts in the water-bath and heats, and ether extraction is used in cooling immediately, merges ether solution, and evaporate to dryness, residue add chloroform makes dissolving, as need testing solution; It is an amount of that other gets the chrysophanol reference substance, adds methanol and make solution, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is developing solvent, launches, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
Discrimination method comprises the part or all of of following project more specifically:
(1) get this preparation or its content 0.2g, add ethanol 10ml, jolting 5min filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to " appendix a VIB of Chinese pharmacopoeia version in 2000 thin layer chromatography test, draw above-mentioned two kinds of each 10ml of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;
(2) get this preparation or its content 0.2g, add methanol 10ml, flooded 1 hour, filter, filtrate evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, put and heat 30min in the water-bath, immediately cooling, divide 2 extractions with ether, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution; Other gets the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to " appendix a VIB of Chinese pharmacopoeia version in 2000 thin layer chromatography test, draw above-mentioned two kinds of each 5ml of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
The content assaying method of the Radix Paeoniae Alba is to be contrast with the peoniflorin reference substance in this preparation, and with methanol: water=27: 73 is the high performance liquid chromatography of mobile phase.
Content assaying method is:
According to " an appendix VI of Chinese pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
The system suitability test is a filler with the octadecylsilane chemically bonded silica; Methanol: water=27: 73 is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;
It is an amount of that the peoniflorin reference substance is got in the preparation of reference substance solution, adds methanol and make solution, shakes up, promptly;
This preparation or its content are got in the preparation of need testing solution, mix, and porphyrize, the accurate title, decide, and puts in the measuring bottle, adds methanol, and supersound process adds methanol to scale, shakes up, and filters, and gets filtrate, promptly;
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;
Every gram contains the Radix Paeoniae Alba with peoniflorin C in this preparation
23H
28O
11Meter must not be less than 10.28mg.
Content assaying method is more specifically:
According to " an appendix VI of Chinese pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
The system suitability test is a filler with the octadecylsilane chemically bonded silica; Methanol: water=27: 73 is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;
It is an amount of to the peoniflorin reference substance of constant weight that the preparation precision of reference substance solution takes by weighing 60 ℃ of drying under reduced pressure, adds 80% methanol and make the solution that every 1ml contains 0.2mg, shakes up, promptly;
This preparation or its content are got in the preparation of need testing solution, mix, and porphyrize is got 0.1g, and accurate the title decides, and puts in the 50ml measuring bottle, adds 80% methanol 45ml, and supersound process 20min adds 80% methanol to scale, shakes up, and filters, and gets filtrate, promptly;
Accurate respectively reference substance solution and each 5ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures, promptly;
Every gram contains the Radix Paeoniae Alba with peoniflorin C in this preparation
23H
28O
11Meter must not be less than 10.28mg.
Method of quality control of the present invention comprises:
Character:
For capsule: content is brown to chocolate brown powder, feeble QI, mildly bitter flavor;
For tablet: medicine is brown to brown color chips, feeble QI, mildly bitter flavor;
For granule: medicine is brown to brown granular, feeble QI, mildly bitter flavor;
For drop pill: medicine is brown to sepia drop pill, feeble QI, mildly bitter flavor;
For oral liquid: medicine is brown to the sepia supernatant liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For syrup: medicine is brown to the sepia thick liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For eye drop: medicine is brown to the sepia supernatant liquid;
Differentiate: (1) gets this preparation or its content, adds ethanol, and jolting filters, and filtrate evaporate to dryness, residue add ethanol makes dissolving, as need testing solution; It is an amount of that other gets the peoniflorin reference substance, adds ethanol and make solution, in contrast product solution; According to " appendix a VIB of Chinese pharmacopoeia version in 2000 thin layer chromatography test, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is developing solvent, launches, and takes out, dry, spray is with the vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;
(2) get this preparation or its content, add methanol, dipping filters, and filtrate evaporate to dryness, residue add water makes dissolving, adds hydrochloric acid again, puts in the water-bath and heats, and ether extraction is used in cooling immediately, merges ether solution, and evaporate to dryness, residue add chloroform makes dissolving, as need testing solution; It is an amount of that other gets the chrysophanol reference substance, adds methanol and make solution, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is developing solvent, launches, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Check: should meet " relevant every regulation under each preparation item of appendix of Chinese pharmacopoeia version in 2000;
Assay: according to " an appendix VI of Chinese pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
The system suitability test is a filler with the octadecylsilane chemically bonded silica; Methanol: water=27: 73 is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;
It is an amount of that the peoniflorin reference substance is got in the preparation of reference substance solution, adds methanol and make solution, shakes up, promptly;
This preparation or its content are got in the preparation of need testing solution, mix, and porphyrize, the accurate title, decide, and puts in the measuring bottle, adds methanol, and supersound process adds methanol to scale, shakes up, and filters, and gets filtrate, promptly;
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;
Every gram contains the Radix Paeoniae Alba with peoniflorin C in this preparation
23H
28O
11Meter must not be less than 10.28mg.
Described method of quality control also can comprise:
Character:
For capsule: content is brown to chocolate brown powder, feeble QI, mildly bitter flavor;
For tablet: medicine is brown to brown color chips, feeble QI, mildly bitter flavor;
For granule: medicine is brown to brown granular, feeble QI, mildly bitter flavor;
For drop pill: medicine is brown to sepia drop pill, feeble QI, mildly bitter flavor;
For oral liquid: medicine is brown to the sepia supernatant liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For syrup: medicine is brown to the sepia thick liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For eye drop: medicine is brown to the sepia supernatant liquid;
Differentiate: (1) gets this preparation or its content 0.2g, adds ethanol 10ml, and jolting 5min filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to " appendix a VIB of Chinese pharmacopoeia version in 2000 thin layer chromatography test, draw above-mentioned two kinds of each 10ml of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;
(2) get this preparation or its content 0.2g, add methanol 10ml, flooded 1 hour, filter, filtrate evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, put and heat 30min in the water-bath, immediately cooling, divide 2 extractions with ether, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution; Other gets the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to " appendix a VI of Chinese pharmacopoeia version in 2000 B thin layer chromatography test, draw above-mentioned two kinds of each 5ml of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Check: should meet " relevant every regulation under each preparation item of appendix of Chinese pharmacopoeia version in 2000;
Assay: according to " an appendix VI of Chinese pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
The system suitability test is a filler with the octadecylsilane chemically bonded silica; Methanol: water=27: 73 is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;
It is an amount of to the peoniflorin reference substance of constant weight that the preparation precision of reference substance solution takes by weighing 60 ℃ of drying under reduced pressure, adds 80% methanol and make the solution that every 1ml contains 0.2mg, shakes up, promptly;
This preparation or its content are got in the preparation of need testing solution, mix, and porphyrize is got 0.1g, and accurate the title decides, and puts in the 50ml measuring bottle, adds 80% methanol 45ml, and supersound process 20min adds 80% methanol to scale, shakes up, and filters, and gets filtrate, promptly;
Accurate respectively reference substance solution and each 5ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures, promptly;
Every gram contains the Radix Paeoniae Alba with peoniflorin C in this preparation
23H
28O
11Meter must not be less than 10.28mg.
The applicant has carried out a series of experimental study, and to determine best method of quality control, its result is as follows:
One, differentiates
This preparation is made up of four flavor Chinese crude drugs, forms through extracting, making with extra care, and composition is complicated.We had once carried out the experimental study of discrimination method to each flavor Chinese crude drug composition separately, had set up the discrimination method of the Radix Paeoniae Alba, Semen Cassiae.The discrimination method of other each flavor, through repetition test, all the content because of composition is low excessively, fails well to be differentiated, so exclude quality standard of the present invention.
(1) this preparation or its content 0.2g are got in the discriminating of the Radix Paeoniae Alba, add ethanol 10ml, and jolting 5min filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Get the feminine gender simulation preparation that lacks the Radix Paeoniae Alba, be equipped with negative controls with legal system.Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.According to " Chinese pharmacopoeia thin layer chromatography of version in 2000 (appendix VIB) test, draw above-mentioned three kinds of each 10ml of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, (10: 4: 6: 1) be developing solvent, expansion was taken out with chloroform-ethyl acetate-methanol-acetic acid, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, negative control is noiseless.
(2) this preparation or its content 0.2g are got in the discriminating of Semen Cassiae, add methanol 10ml, flood 1 hour, filter, filtrate evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, put and heat 30min in the water-bath, immediately cooling, divide 2 extractions with ether, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.Get the feminine gender simulation preparation that lacks Semen Cassiae, be equipped with negative controls with legal system.Other gets the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.According to " Chinese pharmacopoeia thin layer chromatography of version in 2000 (appendix VIB) test, draw above-mentioned three kinds of each 2ml of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃)-ethyl acetate-formic acid (20: 2: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color, negative control is noiseless.
(3) research of the discrimination test of Herba Dendrobii and Fructus Leonuri is also unmatchful according to medical material because of no reference substance, so exclude corresponding discrimination test in the quality standard, remains further to be studied.
Two, check
The applicant is according to " pertinent regulations under each preparation item of appendix of Chinese pharmacopoeia version in 2000 are checked.Check moisture, content uniformity, disintegration, microbial limit respectively, wherein:
Moisture is by " " oven drying method " measured in aquametry of Chinese pharmacopoeia version in 2000.
Content uniformity is by " the regulation inspection under each preparation item of appendix of Chinese pharmacopoeia version in 2000.
Disintegration is by " the regulation inspection under each preparation item of appendix of Chinese pharmacopoeia version in 2000.
Microbial limit is by " Chinese pharmacopoeia appendix of version in 2000 " microbial limit method " is checked.
Every check result shows, preparation of the present invention meets that " pertinent regulations under each preparation item of appendix of Chinese pharmacopoeia version in 2000 the results are shown in Table 1.
Table 1 preparation check result of the present invention (n=2)
| The sample lot number | 040102 | 040106 | 040112 |
| Moisture (%) content uniformity (%) disintegration time limited (min) microbial limit is (individual/g) the bacterial population fungi count pathogenic bacteria mite that lives | 4.12 up to specification 19＜10＜10 do not detect | 4.73 17＜l0 up to specification＜10 do not detect | 5.22 up to specification 19＜10＜10 do not detect |
Three, assay
According to the documents and materials of square Chinese crude drug ingredient, the applicant has carried out assay research to the peoniflorin in the Radix Paeoniae Alba, chrysophanol in the Semen Cassiae.Result of the test shows, in the Semen Cassiae medical material chrysophanol content lower (＜0.1%, make in the preparation content of chrysophanol be lower than ten thousand/, bigger with the error of chrysophanol quantitative assay, do not reach the purpose of control product quality, so do not list quality standard of the present invention in.Main effective ingredient is a peoniflorin in the Radix Paeoniae Alba, the assay of chemical constituent in the Radix Paeoniae Alba, and what bibliographical information was more is that content of paeoniflorin is measured, method for measuring has thin layer chromatography scanning, high performance liquid chromatography etc.We study content of paeoniflorin assay method in the Radix Paeoniae Alba, adopt content of paeoniflorin in the high effective liquid chromatography for measuring Radix Paeoniae Alba.Paeoniflorin content assay method and content of paeoniflorin limit have been drafted in the quality standard, with the quality of control preparation.
1, instrument: the HP1100 of U.S. Hewlett-Packard type high performance liquid chromatograph (comprising vacuum degassing machine, quaternary pump, automatic sampler, DAD detector, column oven), HP1100/WIND-3D chem workstation; KQ-250 type ultrasonic cleaner (city of Kunshan's ultrasonic instrument factory).
2, reagent: methanol is chromatographically pure; Water is redistilled water; Other reagent are analytical pure; Peoniflorin reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number 0736-200219).Medical material is identified through Guizhou Prov. Traditional Chinese Medical Research Inst Chen Deyuan researcher.
3, chromatographic condition: chromatographic column: Hypersil C
18(5 μ m, ID4.6 * 250mm, Dalian Yi Lite scientific instrument company limited); Mobile phase: methanol-water (23: 73); Flow velocity: 1.0mlmin
-130 ℃ of column temperatures; Detect wavelength 230nm.
4, system suitability test: get peoniflorin reference substance solution, need testing solution respectively, lack the negative need testing solution injection of Radix Paeoniae Alba chromatograph of liquid, record chromatograph.Under this experimental condition, need testing solution peoniflorin peak and other compositions can reach baseline separation, and it is noiseless that negative need testing solution goes out the place, peak at peoniflorin.Theoretical cam curve should be not less than 1500 in the peoniflorin peak.
5, peoniflorin reference substance purity test: it is an amount of to the peoniflorin reference substance of constant weight that precision takes by weighing drying under reduced pressure, prepares to such an extent that concentration is the solution of 0.1484mg/ml with 80% dissolve with methanol, in contrast product solution.Accurate each 15mL of solvent that draws this reference substance solution and preparation reference substance solution injects chromatograph of liquid, measures by above-mentioned chromatographic condition, and calculating peoniflorin purity with peak area normalization is 99.8%.
6, the peoniflorin linear relationship is investigated: the accurate respectively reference substance solution of drawing under " peoniflorin reference substance purity test " item 0.5,1,2,3,4,5ml puts in the 5ml measuring bottle, be diluted to scale successively with 80% methanol, shake up, the accurate 5ml that draws, inject chromatograph of liquid, measure the peoniflorin peak area by above-mentioned chromatographic condition.With peoniflorin peak area integrated value is vertical coordinate (Y), and paeoniflorin content is abscissa (X), gets regression equation: Y=1354.10734X+0.25894, r=0.99995, and peoniflorin is good in 0.07405～0.7405 μ g scope internal linear relation, the results are shown in Table 2.
Table 2 peoniflorin linear relationship is investigated
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 |
| Peak area integrated value (mAus) | 103.43 | 203.76 | 397.05 | 596.99 | 801.58 | 1007.43 |
| Peoniflorin contains heavily (μ g) | 0.07405 | 0.1481 | 0.2962 | 0.4443 | 0.5924 | 0.7405 |
7, the investigation of test sample peoniflorin extracting method:
7.1 extract the investigation of solvent: precision takes by weighing this preparation or its content 0.1g, puts in the 50ml measuring bottle, adds each 45ml of different solvents respectively, supersound process 10min, put and use the coordinative solvent standardize solution respectively after cold, shake up, filter, get the subsequent filtrate sample introduction, measure paeoniflorin content, the results are shown in Table 3.
The different comparisons (n=2) of extracting solvent of table 3
| Extract solvent | 40% methanol | 50% methanol | 80% methanol | Methanol | Ethanol |
| Peoniflorin contains heavily (mg/g) | 18.24 | 18.28 | 18.69 | 18.67 | 16.35 |
Above result shows that the paeoniflorin content of 80% ethanol extraction is the highest, so adopt 80% methanol for extracting solvent.
7.2 the investigation of extraction time: precision takes by weighing this preparation or its content 0.1g, puts in the 50ml measuring bottle, adds 80% methanol 45ml, respectively the supersound process different time, put cold back with 80% methanol constant volume, shake up, filter, get the subsequent filtrate sample introduction, measure paeoniflorin content, the results are shown in Table 4.
The comparison (n=2) of different supersound process times of table 4
| Ultrasonic time (min) | 5 | 10 | 20 | 30 |
| Peoniflorin contains heavily (mg/g) | 18.43 | 18.48 | 19.08 | 18.52 |
Show in the table that institute is in the investigation time, supersound process 20min, content no longer increases, so determine that the supersound process time is 20min.
7.3 the investigation of extracting method: precision takes by weighing this preparation or its content 0.1g, and solvent extracts 20min with different extracting method respectively with 80% methanol of 50ml, it is heavy with 80% methanol benefit that extracting solution is put cold back, shakes up, and filters, get the subsequent filtrate sample introduction, measure paeoniflorin content, the results are shown in Table 5.
The comparison of table 5 Different Extraction Method (n=2)
| Extracting method | Ultrasonic | Reflux | Jolting is extracted |
| Peoniflorin contains heavily (mg/g) | 19.08 | 19.16 | 18.35 |
The result shows, supersound process method peoniflorin is carried to such an extent that amount is equivalent to reflux extraction 99.6%, though the test sample content that reflux extraction extracts than supersound process method is high slightly, but the two is more or less the same, and ultrasonic processing method is simple and easy to do relatively, test sample liquid has solids to become the agglomerate phenomenon in the reflux, extract, simultaneously, so determine that extracting method is a supersound process.
7.4 conclusion: draw from above-mentioned result of the test, it is comparatively suitable as the extracting method of test sample with 80% methanol supersound process 20min to select.
8, the preparation of need testing solution: get preparation or its content under the content uniformity item, mixing, porphyrize are got about 0.1g, and accurate the title decides, put in the 50ml measuring bottle, add the about 45ml of 80% methanol, supersound process 20min adds 80% methanol to scale, shake up, filter with the 0.45mm filter membrane, promptly.
9, the preparation of negative control product solution: other gets the group's medicine that does not contain the Radix Paeoniae Alba, prepares the negative control sample by preparation technology.It is an amount of to get the negative control sample, prepares negative controls by the preparation method of need testing solution.
10, precision test: the accurate peoniflorin reference substance solution (0.4341mg/ml) of drawing, repeat sample introduction 5 times, each 5ml measures the peoniflorin peak area, and RSD is 0.7%, the results are shown in Table 6.
Table 6 Precision test result
| Sequence number | 1 | 2 | 3 | 4 | 5 | On average | RSD(％) |
| The peoniflorin peak area | 549.62 | 559.37 | 558.04 | 555.11 | 559.45 | 556.32 | 0.74 |
11, stability test: the same need testing solution 5ml of accurate absorption, measured the peoniflorin peak area every 2 hours, the results are shown in Table 7, show that peoniflorin is good at 8 hours internal stabilities in the need testing solution.
Peoniflorin stability test in table 7 test sample
| Sample injection time (h) | 0 | 2 | 4 | 6 | 8 | On average | RSD(％) |
| The peoniflorin peak area | 544.97 | 541.53 | 546.44 | 554.29 | 563.64 | 550.17 | 1.61 |
12, replica test: precision takes by weighing this preparation or its content 0.1g, presses 5 parts of need testing solutions of the parallel preparation of preparation method of need testing solution, and equal chromatographic condition is measured the peoniflorin peak area, the results are shown in Table 8, average content 38.16mg/g, RSD=1.1%.
The replica test of peoniflorin in table 8 test sample
| Measure number of times | 1 | 2 | 3 | 4 | 5 | On average | RSD(％) |
| Content (mg/g) | 18.77 | 18.66 | 18.78 | 19.99 | 19.20 | 19.08 | 2.88 |
13, recovery test: get preparation or its content (average content 19.08mg/g) of measuring content, it is an amount of to add the peoniflorin reference substance respectively, press 5 parts of test liquids of preparation method preparation of need testing solution, the difference sample introduction, measure the peoniflorin peak area, the results are shown in Table 9, the average recovery rate of peoniflorin is 100.7%, RSD=2.1%.
The recovery test of peoniflorin in table 9 test sample
| Experiment number | Sample size (g) | Contain peoniflorin amount (mg) | Add peoniflorin amount (mg) | The amount of recording (mg) | The response rate (%) | Average recovery rate (%) | RSD(％) |
| 1 | 0.05050 | 0.963 | 0.955 | 1.912 | 99.37 | ||
| 2 | 0.05030 | 0.960 | 0.955 | 1.914 | 99.90 | ||
| 3 | 0.05170 | 0.986 | 0.955 | 1.926 | 98.43 | 100.42 | 3.7 |
| 4 | 0.05180 | 0.988 | 0.955 | 2.010 | 107.02 | ||
| 5 | 0.05066 | 0.966 | 0.955 | 1.896 | 97.38 |
14, sample size is measured and the peoniflorin yield: get test agent in 3 batches, prepare test liquid respectively by the preparation method of need testing solution, measure with method, external standard method is calculated paeoniflorin content, the results are shown in Table 10.
The content and the yield of paeoniflorin in table 10 preparation of the present invention
| Lot number | Content (mg/g) | Average content (mg/g) | Dried cream yield (%) | Paeoniflorin content in the Radix Paeoniae Alba (mg/g) | Peoniflorin yield (%) | |
| 1 | 2 | |||||
| 040102 040106 040112 | l6.83 16.64 17.06 | 17.28 16.85 16.57 | 17.05 16.75 16.82 | 8.53 8.60 8.63 | 9.21 9.40 9.13 | 52.3 52.2 52.1 |
15, sample paeoniflorin content limit is calculated: from 3 crowdes of pilot scale sample determination results as seen, each lot number peoniflorin extraction ratio is all more than 50%, thus in the preparation peoniflorin extraction ratio by being not less than 50%.The paeoniflorin content limit is calculated as follows in the sample: paeoniflorin content limit=preparation contains white Peony Root (g/g) * medical material and contains peoniflorin limit * peoniflorin extraction ratio * 100%=900/350 * 0.8% * 50% * 100%=1.028%.Paeoniflorin content: 1.028% * 1 * 1000=10.28mg/g in every 1g finished product.
So the tentative every gram of this preparation contains the Radix Paeoniae Alba with peoniflorin (C
23H
28O
11) meter, must not be less than 10.28mg.
Compared with prior art, method of quality control precision height of the present invention, good stability, favorable reproducibility, response rate height, measurement result is accurate, can control the quality of the asthenopic pharmaceutical preparation of treatment effectively, thereby has guaranteed the clinical efficacy of said preparation.
The specific embodiment:
Embodiments of the invention 1:
Character:
For capsule: content is brown to chocolate brown powder, feeble QI, mildly bitter flavor;
For tablet: medicine is brown to brown color chips, feeble QI, mildly bitter flavor;
For granule: medicine is brown to brown granular, feeble QI, mildly bitter flavor;
For drop pill: medicine is brown to sepia drop pill, feeble QI, mildly bitter flavor;
For oral liquid: medicine is brown to the sepia supernatant liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For syrup: medicine is brown to the sepia thick liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For eye drop: medicine is brown to the sepia supernatant liquid;
Differentiate: (1) gets this preparation or its content 0.2g, adds ethanol 10ml, and jolting 5min filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to " appendix a VIB of Chinese pharmacopoeia version in 2000 thin layer chromatography test, draw above-mentioned two kinds of each 10ml of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;
(2) get this preparation or its content 0.2g, add methanol 10ml, flooded 1 hour, filter, filtrate evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, put and heat 30min in the water-bath, immediately cooling, divide 2 extractions with ether, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution; Other gets the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to " appendix a VI of Chinese pharmacopoeia version in 2000 B thin layer chromatography test, draw above-mentioned two kinds of each 5ml of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Check: should meet " relevant every regulation under each preparation item of appendix of Chinese pharmacopoeia version in 2000;
Assay: according to " an appendix VI of Chinese pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
The system suitability test is a filler with the octadecylsilane chemically bonded silica; Methanol: water=27: 73 is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;
It is an amount of to the peoniflorin reference substance of constant weight that the preparation precision of reference substance solution takes by weighing 60 ℃ of drying under reduced pressure, adds 80% methanol and make the solution that every 1ml contains 0.2mg, shakes up, promptly;
This preparation or its content are got in the preparation of need testing solution, mix, and porphyrize is got 0.1g, and accurate the title decides, and puts in the 50ml measuring bottle, adds 80% methanol 45ml, and supersound process 20min adds 80% methanol to scale, shakes up, and filters, and gets filtrate, promptly;
Accurate respectively reference substance solution and each 5ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures, promptly;
Every gram contains the Radix Paeoniae Alba with peoniflorin C in this preparation
23H
28O
11Meter must not be less than 10.28mg.
Embodiments of the invention 2:
Character:
For capsule: content is brown to chocolate brown powder, feeble QI, mildly bitter flavor;
For tablet: medicine is brown to brown color chips, feeble QI, mildly bitter flavor;
For granule: medicine is brown to brown granular, feeble QI, mildly bitter flavor;
For drop pill: medicine is brown to sepia drop pill, feeble QI, mildly bitter flavor;
For oral liquid: medicine is brown to the sepia supernatant liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For syrup: medicine is brown to the sepia thick liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For eye drop: medicine is brown to the sepia supernatant liquid;
Differentiate: get this preparation or its content 0.2g, add ethanol 10ml, jolting 5min filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to " appendix a VIB of Chinese pharmacopoeia version in 2000 thin layer chromatography test, draw above-mentioned two kinds of each 10ml of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;
Assay: according to " an appendix VI of Chinese pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
The system suitability test is a filler with the octadecylsilane chemically bonded silica; Methanol: water=27: 73 is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;
It is an amount of to the peoniflorin reference substance of constant weight that the preparation precision of reference substance solution takes by weighing 60 ℃ of drying under reduced pressure, adds 80% methanol and make the solution that every 1ml contains 0.2mg, shakes up, promptly;
This preparation or its content are got in the preparation of need testing solution, mix, and porphyrize is got 0.1g, and accurate the title decides, and puts in the 50ml measuring bottle, adds 80% methanol 45ml, and supersound process 20min adds 80% methanol to scale, shakes up, and filters, and gets filtrate, promptly;
Accurate respectively reference substance solution and each 5ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures, promptly;
Every gram contains the Radix Paeoniae Alba with peoniflorin C in this preparation
23H
28O
11Meter must not be less than 10.28mg.
Embodiments of the invention 3:
Character:
For capsule: content is brown to chocolate brown powder, feeble QI, mildly bitter flavor;
For tablet: medicine is brown to brown color chips, feeble QI, mildly bitter flavor;
For granule: medicine is brown to brown granular, feeble QI, mildly bitter flavor;
For drop pill: medicine is brown to sepia drop pill, feeble QI, mildly bitter flavor;
For oral liquid: medicine is brown to the sepia supernatant liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For syrup: medicine is brown to the sepia thick liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For eye drop: medicine is brown to the sepia supernatant liquid;
Differentiate: (1) gets this preparation or its content 0.2g, adds ethanol 10ml, and jolting 5min filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to " appendix a VIB of Chinese pharmacopoeia version in 2000 thin layer chromatography test, draw above-mentioned two kinds of each 10ml of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;
(2) get this preparation or its content 0.2g, add methanol 10ml, flooded 1 hour, filter, filtrate evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, put and heat 30min in the water-bath, immediately cooling, divide 2 extractions with ether, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution; Other gets the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to " appendix a VI of Chinese pharmacopoeia version in 2000 B thin layer chromatography test, draw above-mentioned two kinds of each 5ml of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Check: should meet " relevant every regulation under each preparation item of appendix of Chinese pharmacopoeia version in 2000.
Embodiments of the invention 4:
Character:
For capsule: content is brown to chocolate brown powder, feeble QI, mildly bitter flavor;
For tablet: medicine is brown to brown color chips, feeble QI, mildly bitter flavor;
For granule: medicine is brown to brown granular, feeble QI, mildly bitter flavor;
For drop pill: medicine is brown to sepia drop pill, feeble QI, mildly bitter flavor;
For oral liquid: medicine is brown to the sepia supernatant liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For syrup: medicine is brown to the sepia thick liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;
For eye drop: medicine is brown to the sepia supernatant liquid;
Check: should meet " relevant every regulation under each preparation item of appendix of Chinese pharmacopoeia version in 2000;
Assay: according to " an appendix VI of Chinese pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
The system suitability test is a filler with the octadecylsilane chemically bonded silica; Methanol: water=27: 73 is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;
It is an amount of to the peoniflorin reference substance of constant weight that the preparation precision of reference substance solution takes by weighing 60 ℃ of drying under reduced pressure, adds 80% methanol and make the solution that every 1ml contains 0.2mg, shakes up, promptly;
This preparation or its content are got in the preparation of need testing solution, mix, and porphyrize is got 0.1g, and accurate the title decides, and puts in the 50ml measuring bottle, adds 80% methanol 45ml, and supersound process 20min adds 80% methanol to scale, shakes up, and filters, and gets filtrate, promptly;
Accurate respectively reference substance solution and each 5ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures, promptly;
Every gram contains the Radix Paeoniae Alba with peoniflorin C in this preparation
23H
28O
11Meter must not be less than 10.28mg.
Claims (10)
- One kind the treatment asthenopic pharmaceutical preparation method of quality control, said preparation comprises capsule, tablet, granule, drop pill, oral liquid, syrup or eye drop, described method of quality control mainly comprise in character, inspection, discriminating, the assay project partly or entirely; It is characterized in that: character should meet the pertinent regulations under each preparation item; Discriminating is that the thin layer of the Radix Paeoniae Alba, Semen Cassiae is differentiated; Inspection should meet the pertinent regulations under each preparation item of appendix of Chinese Pharmacopoeia version in 2000; Assay is the assay to the Radix Paeoniae Alba in the preparation.
- 2. according to the method for quality control of the asthenopic pharmaceutical preparation of the described treatment of claim 1, it is characterized in that: the discrimination method of the Radix Paeoniae Alba is to be contrast with the peoniflorin reference substance in this preparation, and with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is the thin layer discrimination method of developing solvent.
- 3. according to the method for quality control of the asthenopic pharmaceutical preparation of the described treatment of claim 1, it is characterized in that: the discrimination method of Semen Cassiae is to be contrast with the chrysophanol reference substance in this preparation, and with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is the thin layer discrimination method of developing solvent.
- 4. according to the method for quality control of claim 1, the asthenopic pharmaceutical preparation of 2 or 3 described treatments, it is characterized in that: discrimination method comprises the part or all of of following project:(1) get this preparation or its content, add ethanol, jolting filters, and filtrate evaporate to dryness, residue add ethanol makes dissolving, as need testing solution; It is an amount of that other gets the peoniflorin reference substance, adds ethanol and make solution, in contrast product solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2000 thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is developing solvent, launches, and takes out, dry, spray is with the vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;(2) get this preparation or its content, add methanol, dipping filters, and filtrate evaporate to dryness, residue add water makes dissolving, adds hydrochloric acid again, puts in the water-bath and heats, and ether extraction is used in cooling immediately, merges ether solution, and evaporate to dryness, residue add chloroform makes dissolving, as need testing solution; It is an amount of that other gets the chrysophanol reference substance, adds methanol and make solution, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is developing solvent, launches, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
- 5. according to the method for quality control of the asthenopic pharmaceutical preparation of the described treatment of claim 4, it is characterized in that: discrimination method comprises the part or all of of following project more specifically:(1) get this preparation or its content 0.2g, add ethanol 10ml, jolting 5min filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2000 thin layer chromatography, draw above-mentioned two kinds of each 10ml of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;(2) get this preparation or its content 0.2g, add methanol 10ml, flooded 1 hour, filter, filtrate evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, put and heat 30min in the water-bath, immediately cooling, divide 2 extractions with ether, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution; Other gets the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw above-mentioned two kinds of each 5ml of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
- 6. according to the method for quality control of the asthenopic pharmaceutical preparation of the described treatment of claim 1, it is characterized in that: the content assaying method of the Radix Paeoniae Alba is to be contrast with the peoniflorin reference substance in this preparation, and with methanol: water=27: 73 is the high performance liquid chromatography of mobile phase.
- 7. according to the method for quality control of claim 1 or the asthenopic pharmaceutical preparation of 6 described treatments, it is characterized in that: content assaying method is:According to an appendix VI of Chinese Pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:The system suitability test is a filler with the octadecylsilane chemically bonded silica; Methanol: water=27: 73 is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;It is an amount of that the peoniflorin reference substance is got in the preparation of reference substance solution, adds methanol and make solution, shakes up, promptly;This preparation or its content are got in the preparation of need testing solution, mix, and porphyrize, the accurate title, decide, and puts in the measuring bottle, adds methanol, and supersound process adds methanol to scale, shakes up, and filters, and gets filtrate, promptly;Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;Every gram contains the Radix Paeoniae Alba in peoniflorin C23H28O11 in this preparation, must not be less than 10.28mg.
- 8. according to the method for quality control of the asthenopic pharmaceutical preparation of the described treatment of claim 7, it is characterized in that: content assaying method is more specifically:According to an appendix VI of Chinese Pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:The system suitability test is a filler with the octadecylsilane chemically bonded silica; Methanol: water=27: 73 is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;It is an amount of to the peoniflorin reference substance of constant weight that the preparation precision of reference substance solution takes by weighing 60 ℃ of drying under reduced pressure, adds 80% methanol and make the solution that every 1ml contains 0.2mg, shakes up, promptly;This preparation or its content are got in the preparation of need testing solution, mix, and porphyrize is got 0.1g, and accurate the title decides, and puts in the 50ml measuring bottle, adds 80% methanol 45ml, and supersound process 20min adds 80% methanol to scale, shakes up, and filters, and gets filtrate, promptly;Accurate respectively reference substance solution and each 5ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures, promptly;Every gram contains the Radix Paeoniae Alba in peoniflorin C23H28O11 in this preparation, must not be less than 10.28mg.
- 9. according to the method for quality control of the asthenopic pharmaceutical preparation of the described treatment of claim 1, it is characterized in that: described method of quality control comprises:Character:For capsule: content is brown to chocolate brown powder, feeble QI, mildly bitter flavor;For tablet: medicine is brown to brown color chips, feeble QI, mildly bitter flavor;For granule: medicine is brown to brown granular, feeble QI, mildly bitter flavor;For drop pill: medicine is brown to sepia drop pill, feeble QI, mildly bitter flavor;For oral liquid: medicine is brown to the sepia supernatant liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;For syrup: medicine is brown to the sepia thick liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;For eye drop: medicine is brown to the sepia supernatant liquid;Differentiate: (1) gets this preparation or its content, adds ethanol, and jolting filters, and filtrate evaporate to dryness, residue add ethanol makes dissolving, as need testing solution; It is an amount of that other gets the peoniflorin reference substance, adds ethanol and make solution, in contrast product solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2000 thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is developing solvent, launches, and takes out, dry, spray is with the vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;(2) get this preparation or its content, add methanol, dipping filters, and filtrate evaporate to dryness, residue add water makes dissolving, adds hydrochloric acid again, puts in the water-bath and heats, and ether extraction is used in cooling immediately, merges ether solution, and evaporate to dryness, residue add chloroform makes dissolving, as need testing solution; It is an amount of that other gets the chrysophanol reference substance, adds methanol and make solution, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is developing solvent, launches, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;Check: should meet relevant every regulation under each preparation item of appendix of Chinese Pharmacopoeia version in 2000;Assay: shine an appendix VI of Chinese Pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:The system suitability test is a filler with the octadecylsilane chemically bonded silica; Methanol: water=27: 73 is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;It is an amount of that the peoniflorin reference substance is got in the preparation of reference substance solution, adds methanol and make solution, shakes up, promptly;This preparation or its content are got in the preparation of need testing solution, mix, and porphyrize, the accurate title, decide, and puts in the measuring bottle, adds methanol, and supersound process adds methanol to scale, shakes up, and filters, and gets filtrate, promptly;Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;Every gram contains the Radix Paeoniae Alba in peoniflorin C23H28O11 in this preparation, must not be less than 10.28mg.
- 10. according to the method for quality control of the asthenopic pharmaceutical preparation of the described treatment of claim 9, it is characterized in that: described method of quality control comprises:Character:For capsule: content is brown to chocolate brown powder, feeble QI, mildly bitter flavor;For tablet: medicine is brown to brown color chips, feeble QI, mildly bitter flavor;For granule: medicine is brown to brown granular, feeble QI, mildly bitter flavor;For drop pill: medicine is brown to sepia drop pill, feeble QI, mildly bitter flavor;For oral liquid: medicine is brown to the sepia supernatant liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;For syrup: medicine is brown to the sepia thick liquid, feeble QI, and it is sweet to distinguish the flavor of, little hardship;For eye drop: medicine is brown to the sepia supernatant liquid;Differentiate: (1) gets this preparation or its content 0.2g, adds ethanol 10ml, and jolting 5min filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2000 thin layer chromatography, draw above-mentioned two kinds of each 10ml of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methanol: acetic acid=10: 4: 6: 1 is developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, puts under the daylight and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;(2) get this preparation or its content 0.2g, add methanol 10ml, flooded 1 hour, filter, filtrate evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, put and heat 30min in the water-bath, immediately cooling, divide 2 extractions with ether, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution; Other gets the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw above-mentioned two kinds of each 5ml of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, with 60 ℃～90 ℃ petroleum ether: ethyl acetate: formic acid=20: 2: 1 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;Check: should meet relevant every regulation under each preparation item of appendix of Chinese Pharmacopoeia version in 2000;Assay: shine an appendix VI of Chinese Pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:The system suitability test is a filler with the octadecylsilane chemically bonded silica; Methanol: water=27: 73 is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;It is an amount of to the peoniflorin reference substance of constant weight that the preparation precision of reference substance solution takes by weighing 60 ℃ of drying under reduced pressure, adds 80% methanol and make the solution that every 1ml contains 0.2mg, shakes up, promptly;This preparation or its content are got in the preparation of need testing solution, mix, and porphyrize is got 0.1g, and accurate the title decides, and puts in the 50ml measuring bottle, adds 80% methanol 45ml, and supersound process 20min adds 80% methanol to scale, shakes up, and filters, and gets filtrate, promptly;Accurate respectively reference substance solution and each 5ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures, promptly;Every gram contains the Radix Paeoniae Alba in peoniflorin C23H28O11 in this preparation, must not be less than 10.28mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006102003211A CN100570358C (en) | 2006-04-06 | 2006-04-06 | Treat the detection method of asthenopic pharmaceutical preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006102003211A CN100570358C (en) | 2006-04-06 | 2006-04-06 | Treat the detection method of asthenopic pharmaceutical preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1857620A true CN1857620A (en) | 2006-11-08 |
| CN100570358C CN100570358C (en) | 2009-12-16 |
Family
ID=37296608
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006102003211A Active CN100570358C (en) | 2006-04-06 | 2006-04-06 | Treat the detection method of asthenopic pharmaceutical preparation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100570358C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101377482B (en) * | 2007-08-27 | 2012-04-25 | 中国人民解放军总医院 | Quality control method of Fengdima eye drops |
| CN102520113A (en) * | 2011-12-16 | 2012-06-27 | 西藏奇正藏药股份有限公司 | Detection method for fifteen Rupeng preparation |
| CN111849880A (en) * | 2020-06-23 | 2020-10-30 | 和携科技有限公司 | Recovery method of human adipose mesenchymal stem cells after ultralow-temperature cryopreservation |
| CN115814024A (en) * | 2023-01-05 | 2023-03-21 | 深圳梵活生命科学股份有限公司 | Eye care eye lotion and preparation method thereof |
-
2006
- 2006-04-06 CN CNB2006102003211A patent/CN100570358C/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101377482B (en) * | 2007-08-27 | 2012-04-25 | 中国人民解放军总医院 | Quality control method of Fengdima eye drops |
| CN102520113A (en) * | 2011-12-16 | 2012-06-27 | 西藏奇正藏药股份有限公司 | Detection method for fifteen Rupeng preparation |
| CN102520113B (en) * | 2011-12-16 | 2014-05-07 | 西藏奇正藏药股份有限公司 | Detection method for fifteen Rupeng preparation |
| CN111849880A (en) * | 2020-06-23 | 2020-10-30 | 和携科技有限公司 | Recovery method of human adipose mesenchymal stem cells after ultralow-temperature cryopreservation |
| CN115814024A (en) * | 2023-01-05 | 2023-03-21 | 深圳梵活生命科学股份有限公司 | Eye care eye lotion and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100570358C (en) | 2009-12-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101036748A (en) | Quality control method of the Yixinshu Chinese traditional medicine for supplementing qi and for promoting blood circulation by removing blood stasis | |
| CN1895617A (en) | Kidney-warming and heart-nourishing Chinese-medicinal preparation, its making method and quality control | |
| CN1712051A (en) | Quality control of Gongyanping preparation | |
| CN1876040A (en) | Pharmaceutical composition for treating hepatitis, its preparation process and quality control method | |
| CN1785380A (en) | Quality control method of Chinese medicinal preparation | |
| CN1621836A (en) | Quality controlling method for pulse restoring injection | |
| CN1857620A (en) | Quality control method for visual fatigue treating medicine preparation | |
| CN1255678C (en) | Method for measuring content of active constitutent of 'Siji-Sanhuang' capsule | |
| CN1824238A (en) | Quality control method of medicinal preparation for treating lypemania | |
| CN1305512C (en) | Traditional Chinese medicine compound recipe for treating hyperplasia of mammary glands and preparation method thereof | |
| CN1903325A (en) | Blood-sugar lowering A prepn. for treating diabetes, its prepn. method and quality-control method | |
| CN1843424A (en) | Cassia twig tuckahoe effervescence tablet and preparation method and its quality control method | |
| CN1857551A (en) | Quality control method for Chinese medicine preparation | |
| CN100344321C (en) | Medicinal composition, its preparation process and quality control method | |
| CN1911427A (en) | Medicine for treating chronic diarrhoea | |
| CN1785295A (en) | Quality control method of cbinese medicinal preparation | |
| CN1857435A (en) | Quality control method for Huganning preparation | |
| CN1785347A (en) | Quality control method of Chinese medicinal preparation for treating child hyperpyrexia | |
| CN1840118A (en) | Compound preparation for treating bronchitis, its preparation method and quality control method | |
| CN1291734C (en) | Method for preparing and controlling the quality of Chinese medicinal soft capsule | |
| CN101066437A (en) | Quality control method for compound cantharis oral liquid | |
| CN1857588A (en) | Quality control method for Xianlinggubao preparation | |
| CN1823887A (en) | Quality control method of injection preparation used for treating tumour | |
| CN1857422A (en) | Quality control method for Chinese medicine preparation | |
| CN1827147A (en) | Dispersible tablet with gastrodia tuber for treating headache, its preparation and quality control method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: SINOPHARM GROUP TONGJITANG (GUIZHOU) PHARMACEUTICA Free format text: FORMER NAME: GUIZHOU TONGJITANG PHARMACEUTICAL CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: 550001 No. 35, Xinjie new street, Guizhou, Guiyang Patentee after: Sinopharm group (Guizhou) Pharmaceutical Co., Ltd. Address before: 550001 No. 35, Xinjie new street, Guizhou, Guiyang Patentee before: Guizhou Tongjitang Pharmaceutical Co., Ltd. |
|
| C56 | Change in the name or address of the patentee | ||
| CP02 | Change in the address of a patent holder |
Address after: 550009 No. 296 Southwest Ring Road, Xiaohe District, Guizhou, Guiyang Patentee after: Sinopharm group (Guizhou) Pharmaceutical Co., Ltd. Address before: 550001 No. 35, Xinjie new street, Guizhou, Guiyang Patentee before: Sinopharm group (Guizhou) Pharmaceutical Co., Ltd. |