CN103454373A - Method for detecting medicament for treating dysmenorrhea - Google Patents

Method for detecting medicament for treating dysmenorrhea Download PDF

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CN103454373A
CN103454373A CN2012101781860A CN201210178186A CN103454373A CN 103454373 A CN103454373 A CN 103454373A CN 2012101781860 A CN2012101781860 A CN 2012101781860A CN 201210178186 A CN201210178186 A CN 201210178186A CN 103454373 A CN103454373 A CN 103454373A
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solution
wogonin
tablet
medicinal material
adds
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CN103454373B (en
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夏文
安斯扬
蒋坤
吴春玲
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GUIZHOU BAILING GROUP PHARMACY CO Ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/539—Scutellaria (skullcap)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P15/00—Drugs for genital or sexual disorders; Contraceptives
    • A—HUMAN NECESSITIES
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    • A61K9/00—Medicinal preparations characterised by special physical form
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    • A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
    • A61K9/2054—Cellulose; Cellulose derivatives, e.g. hydroxypropyl methylcellulose
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract

The invention discloses a method for detecting a pharmaceutical composition for treating dysmenorrhea. The pharmaceutical composition is prepared from total flavonoid aglycone of Scutellaria baicalensis, microcrystalline cellulose, pregelatinized starch, carboxymethyl starch sodium, cross-linked polyvinylpyrrolidone, sodium dodecyl sulfate, polysorbate 80, talc and povidone K30. The detection method has the advantages of accurate determination, high sensitivity and good repeatability, and can effectively control the quality of the medicament for treating dysmenorrhea involved in the invention.

Description

A kind of detection method for the treatment of the medicine of dysmenorrhoea
Technical field
The present invention relates to a kind of detection method for the treatment of the medicine of dysmenorrhoea, belong to the field of medicine technology.
Background technology
Dysmenorrhoea is menstrual woman's common clinical, and frequently-occurring disease, particularly adolescent girls approximately have people more than half to be subject to this misery.Dysmenorrhoea mostly occurs at ovulatory cycle, and the uterine hemorrhage of anovulatory cycle is many without pain, this be due to after ovulation under the effect of progestational hormone, the uterine mucosa of secretory phase can synthesize more Prostaglandin PGF 2 α, it can stimulate the uterus contraction of muscle.Dysmenorrhoea patient uterus Prostaglandin PGF 2 αcontent increases, and acts on mesometrium and blood vessel, causes that strong contraction produces pain.Work as Prostaglandin PGF 2 αafter entering blood circulation, can also cause that gastrointestinal smooth muscle shrinks, and produces and feels sick, vomits and all diseases of suffering from diarrhoea.Along with endometrial, come off, the part Prostaglandin PGF 2 αalso by target cell, absorbed or destroy, symptom progressively alleviates to disappearance.China approximately has 1,000 ten thousand maidens to adolesce every year, and the dysmenorrhoea number of the infected will reach tens million of.As treatment means, doctor trained in Western medicine adopts the antispasmodic relief of symptoms such as atropine, compound belladonna tablet clinically usually, also can be with the medicine of antiprostaglandin effect as brufen, naproxen, indocin, and Ketoprofen, the pain of dispelling sheet etc. are treated.But above medicine is large to the pungency of stomach, and easily produce drug resistance and other bad reactions, a lot of patients can't stand its spinoff and less than effective treatment due to anti-.Chinese medicine is having certain advantage in treatment aspect dysmenorrhoea, wherein take temperature through stagnation resolvation person as many, as by stasis of blood wenjing decoction, gynaecology's pill for relaxing nerve, dysmenorrhoea treasured, TONGJINGLING CHONGJI, TONGJING WAN etc., the production of these medicines, for solution extensive patients sufferings, is played good effect.But above drug administration amount is large, and Time of Administration is longer.
The root of large-flowered skullcap is one of conventional Chinese medicine of recording of Chinese Pharmacopoeia, is the dry root of labiate root of large-flowered skullcap Scutellaria baicalensis Georgi.Its bitter, cold in nature.Return lung, courage, spleen, large intestine, small intestinl channel, there is heat-clearing and damp-drying drug, purging intense heat and detonicating, hemostasis, antiabortive effect, for damp-warm syndrome, the heat temperature evil of vomitting uncomfortable in chest, damp and hot ruffian is full, rushes down dysentery, jaundice, the cough with lung heat, high hot polydipsia, blood-head is told nosebleed, carbuncle sore tumefacting virus, fetal irritability etc.Recent studies finds that the root of large-flowered skullcap generates and has a significant effect to the uterus smooth muscle contractile activity with to the uterus prostaglandin, and the single preparation of baikal skullcap root has obvious curative effects to primary dysmenorrhea.
The research discovery, in the root of large-flowered skullcap, contained Scullcap total-flavonoid aglycone is the main effective constituent for the treatment of dysmenorrhoea.The medicine that the Scullcap total-flavonoid aglycone of take is made as raw material, have the effect of clearing heat and expelling damp, regulating blood condition pain relieving, can be used for the primary dysmenorrhea syndrome of stagnant dampness-heat.In order to control better the quality of this product, guarantee clinical drug effect, the invention provides the detection method of the medicine of this treatment dysmenorrhoea.
Summary of the invention
Technical matters to be solved by this invention is, a kind of detection method for the treatment of the medicine of dysmenorrhoea is provided.Described detection method is accurate, highly sensitive, reproducible.
For solving the problems of the technologies described above, the present invention adopts following technical scheme to realize:
The medicine of described treatment dysmenorrhoea calculates according to composition by weight, by Scullcap total-flavonoid aglycone 150-170 part, microcrystalline cellulose 80-90 part, pregelatinized starch 60-70 part, sodium carboxymethyl starch 15-25 part, polyvinylpolypyrrolidone 1-10 part, lauryl sodium sulfate 0.1-5 part, polyoxyethylene sorbitan monoleate 0.5-5 part, talcum powder 3-5 part and 30 POVIDONE K 30 BP/USP 30prepared by 1-10 part: A, take lauryl sodium sulfate, polyoxyethylene sorbitan monoleate and 30 POVIDONE K 30 BP/USP by the following method 30be mixed with containing 30 POVIDONE K 30 BP/USP 30being 5% aqueous solution, is the A product; B, take the Scullcap total-flavonoid aglycone of 80-120 mesh sieve, added microcrystalline cellulose, pregelatinized starch and sodium carboxymethyl starch, mixed in mixer-granulator, obtained the B product; C, A product and B product are mixed, the water that adds B product 0.03-1 doubly to measure stirs, and granulates, and obtains particle, is the C product; D, get C product dry 2-4 hour at the temperature of 60-80 ℃, dried particle, with after the whole grain of 20-40 mesh sieve, adds polyvinylpolypyrrolidone and talcum powder to sieve and mixes, and trimmer is heavily 0.35g, and compressing tablet, obtain tablet of the present invention.
Specifically, the medicine of described treatment dysmenorrhoea calculates according to composition by weight, by 160 parts of Scullcap total-flavonoid aglycones, 84 parts of microcrystalline celluloses, 62.48 parts of pregelatinized starch, 21 parts of sodium carboxymethyl starches, 7 parts of polyvinylpolypyrrolidone, 1.75 parts of lauryl sodium sulfate, 1.22 parts of polyoxyethylene sorbitan monoleates, 4.55 parts of talcum powder and 30 POVIDONE K 30 BP/USP 308 parts of preparations by the following method: A, take lauryl sodium sulfate, polyoxyethylene sorbitan monoleate and 30 POVIDONE K 30 BP/USP 30be mixed with containing 30 POVIDONE K 30 BP/USP 30being 5% aqueous solution, is the A product; B, take the Scullcap total-flavonoid aglycone of 100 mesh sieves, added microcrystalline cellulose, pregelatinized starch and sodium carboxymethyl starch, mixed in mixer-granulator, obtained the B product; C, A product and B product being mixed, add the distilled water of 0.06 times of amount of B product to stir, granulate, obtain particle, is the C product; D, get the C product at the temperature of 70 ℃ dry 3 hours, dried particle, with after whole of 30 mesh sieves, adds polyvinylpolypyrrolidone and talcum powder to sieve and mixes, and trimmer is heavily 0.35g, and compressing tablet, obtain tablet of the present invention.
The detection method of the medicine of described treatment dysmenorrhoea comprises the steps:
Differentiate: get 2, tablet of the present invention, be ground into fine powder, get 0.1g, the 40-60ml that adds diethyl ether, ultrasonic processing 10-20 minute, get ether solution 0.5-3ml, evaporate to dryness, residue adds methyl alcohol 0.5-3ml and dissolves, as need testing solution; Separately get root of large-flowered skullcap control medicinal material 0.2-1g, be made in the same way of control medicinal material solution; According to the Chinese Pharmacopoeia thin-layered chromatography, test, draw need testing solution and each 1-3 μ l of control medicinal material solution, put on same silica gel g thin-layer plate respectively, take chloroform: methyl alcohol: formic acid=90-100: 2-7: 0.5-2 is developping agent, pre-equilibration 20-35 minute, launch, take out, dry, put under visible ray and inspect, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the principal spot of aobvious same color.
The detection method of the medicine of aforesaid treatment dysmenorrhoea also comprises:
Assay: according to the Chinese Pharmacopoeia high effective liquid chromatography for measuring;
System suitability: be filling agent 3.9 * 150mm with octadecylsilane chemically bonded silica; Methyl alcohol: 5-10% acetic acid=10-20: 20-30 is mobile phase; Detect wavelength 255-300nm, column temperature 30-40 ℃, number of theoretical plate calculates and should be not less than 1500 by the wogonin peak;
The preparation of reference substance solution: precision takes the wogonin reference substance of 50-60 ℃ of drying under reduced pressure to constant weight, adds ethanol and makes the solution of every 1ml containing wogonin 30-35 μ g, shakes up, and obtains;
The preparation of need testing solution: get 5, tablet of the present invention, be ground into fine powder, get 0.1-0.3g, accurately weighed, put in the 25ml measuring bottle, add ethanol 15-25ml, ultrasonic processing 10-20 minute, let cool, and adds ethanol to scale, shake up, filter, the accurate subsequent filtrate 0.5-2ml that draws, put in the 10ml measuring bottle, add ethanol to scale, shake up, obtain;
Determination method: precision is drawn reference substance solution and each 3-7 μ l of need testing solution respectively, injects high performance liquid chromatograph, measures the wogonin peak area, calculates, and obtains.
Specifically, the detection method of the medicine of aforesaid treatment dysmenorrhoea is:
Proterties: be yellow sheet; Bitter;
Differentiate: get 2, tablet of the present invention, be ground into fine powder, get 0.1g, the 50ml that adds diethyl ether, ultrasonic processing 15 minutes, get ether solution 1ml, evaporate to dryness, residue adds methyl alcohol 1ml and dissolves, as need testing solution; Separately get root of large-flowered skullcap control medicinal material 0.5g, be made in the same way of control medicinal material solution; According to the Chinese Pharmacopoeia thin-layered chromatography, test, draw each 2 μ l of need testing solution and control medicinal material solution, put on same silica gel g thin-layer plate respectively, take chloroform: methyl alcohol: formic acid=be at 95: 5: 1 developping agent, pre-equilibration 30 minutes, launch, take out, dry, put under visible ray and inspect, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the principal spot of aobvious same color;
Check: should meet every regulation relevant under Chinese Pharmacopoeia tablet item;
Assay: according to the Chinese Pharmacopoeia high effective liquid chromatography for measuring;
System suitability: be filling agent 3.9 * 150mm with octadecylsilane chemically bonded silica; Methyl alcohol: 8% acetic acid=be at 16: 25 mobile phase; Detect wavelength 277.0nm, 35 ℃ of column temperatures, number of theoretical plate calculates and should be not less than 1500 by the wogonin peak;
The preparation of reference substance solution: precision takes the wogonin reference substance of 50-60 ℃ of drying under reduced pressure to constant weight, adds ethanol and makes the solution of every 1ml containing wogonin 32 μ g, shakes up, and obtains;
The preparation of need testing solution: get 5, tablet of the present invention, be ground into fine powder, get 0.1g, accurately weighed, put in the 25ml measuring bottle, add ethanol 20ml, ultrasonic processing 15 minutes, let cool, and adds ethanol to scale, shake up, filter, the accurate subsequent filtrate 1ml that draws, put in the 10ml measuring bottle, add ethanol to scale, shake up, obtain;
Determination method: precision is drawn reference substance solution and each 5 μ l of need testing solution respectively, injects high performance liquid chromatograph, measures the wogonin peak area, and calculating, obtain.
Every, tablet of the present invention contains wogonin (C 16h 12o 5) must not be less than 17.5mg.
Below the research of detection method of the present invention
Experimental example: quality determining method research
1, proterties: be yellow sheet; Bitter.Detect three batches all up to specification, in Table 1.
 
Three batches of examination and test of products results of table 1
Figure 540585DEST_PATH_IMAGE001
2, differentiate: get 2, tablet of the present invention, be ground into fine powder, get 0.1g, the 50ml that adds diethyl ether, ultrasonic processing 15 minutes, get ether solution 1ml, evaporate to dryness, residue adds methyl alcohol 1ml and dissolves, as need testing solution; Get the blank that blank auxiliary material 0.1g makes, be made in the same way of negative control product solution; Get root of large-flowered skullcap control medicinal material 0.5g, be made in the same way of control medicinal material solution.Separately take from baicalein reference substance processed appropriate, make reference substance solution.According to the test of Chinese Pharmacopoeia thin-layered chromatography, draw each 2 μ l of above-mentioned four kinds of solution, to put on same silica gel g thin-layer plate respectively, the chloroform-methanol-formic acid (95: 5: 1) of take is developping agent, pre-equilibration 30 minutes launches, and takes out, and dries, and puts under visible ray and inspects.In the test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, the principal spot of aobvious same color, longer or iodine colour developing standing time, spot is more clear.In negative control product solution chromatogram, on the position corresponding with control medicinal material and reference substance chromatogram, without obvious spot.Detect three batches, result is all up to specification in accordance with the law.
The purpose of this is to identify one of main effective constituent baicalein.Unstable because of baicalein, be difficult for making sterling, pharmacopeia is not also recorded, and determines to use root of large-flowered skullcap control medicinal material product in contrast, and with self-control baicalein reference substance, is illustrated in photo.Though baicalein prepared by our unit is purer, yield is lower, and a large amount of preparation costs are too high.
In research process, once used the developping agents such as chloroform-methanol-formic acid (96: 4: 1), chloroform-methanol (96: 4 and 98: 2), each spot all can separate preferably, and the baicalein spot is obvious.But the former contained formic acid corrosivity is strong, and the no acidic spot of the latter easily trails.
3, check
3.1 weight differential: measure 5 batches of pilot products according to Chinese Pharmacopoeia appendix weight differential determination method, all up to specification, in Table 2.
Table 2 tablet weight variation measurement result
Figure 2012101781860100002DEST_PATH_IMAGE002
3.2 disintegration time limited: measure 5 batches of pilot products according to Chinese Pharmacopoeia appendix disintegration time mensuration method, double, all up to specification, in Table 3.
Table 3 disintegration time mensuration result
Lot number Disintegration time is measured for the 1st time Disintegration time is measured for the 2nd time Conclusion
010615 1 minute 15 seconds 1 minute 19 seconds Up to specification
010618 1 minute 25 seconds 1 minute 09 second Up to specification
010620 1 minute 18 seconds 1 minute 17 seconds Up to specification
010623 1 minute 11 seconds 1 minute 15 seconds Up to specification
010625 1 minute 25 seconds 1 minute 25 seconds Up to specification
3.3 microbial limit: according to Chinese Pharmacopoeia appendix microbial limit detection method, check, up to specification.
3.4 heavy metal inspection: get tablet 5.0g of the present invention, accurately weighed, check 5 batch samples according to Chinese Pharmacopoeia appendix " heavy metal inspection technique " the second method, all up to specification, in Table 4.
Table 4 heavy metal check result
Lot number Sample size g Solution colour Plumbous total content μ g Every gram lead content μ g
010615 5.0000 Water white transparency ＜10 ＜2
010615 5.0000 Water white transparency ＜10 ＜2
010618 5.0008 Water white transparency ＜10 ＜2
010618 5.0002 Water white transparency ＜10 ＜2
010620 5.0004 Water white transparency ＜10 ＜2
010620 5.0003 Water white transparency ＜10 ＜2
010623 5.0007 Water white transparency ＜10 ＜2
010623 5.0010 Water white transparency ＜10 ＜2
010625 5.0001 Water white transparency ＜10 ＜2
010625 5.0003 Water white transparency ＜10 ＜2
Standard lead solution 1 10ppm Muddiness is arranged / /
Standard lead solution 2 20ppm Obviously muddy / /
Above result shows, the leaded every 1g of tablet of the present invention is lower than 2 μ g.
Because the compositions such as baicalein in tablet of the present invention contain more carbonyl and hydroxyl, easy and lead ion generation complex reaction, and the sample intrinsic colour is darker, easily produces and disturbs, therefore do not adopt non-organic destroy method inspection heavy metal.
3.5 arsenic salt checks: precision takes tablet 2.0g of the present invention, according to Chinese Pharmacopoeia appendix " arsenic salt inspection technique " first method, checks 5 batch samples, result is as table 5.
Table 5 arsenic salt check result
Lot number Sample size g Arsenic spot color Arsenic total content μ g Every gram arsenic content μ g
010615 2.0000 Without obvious color ＜2 ＜1
010615 2.0003 Without obvious color ＜2 ＜1
010618 2.0005 Without obvious color ＜2 ＜1
010618 2.0009 Without obvious color ＜2 ＜1
010620 2.0012 Without obvious color ＜2 ＜1
010620 2.0004 Without obvious color ＜2 ＜1
010623 2.0011 Without obvious color ＜2 ＜1
010623 2.0001 Without obvious color ＜2 ＜1
010625 2.0002 Without obvious color ＜2 ＜1
010625 2.0006 Without obvious color ＜2 ＜1
Positive control solution 2ml standard arsenic solution Obviously yellow =2 /
Above result shows, tablet of the present invention containing the every 1g of arsenic lower than 1 μ g.
Because flavone compound in tablet of the present invention is ring texture, easily with arsenic, to be combined, impact detects.Therefore adopting dry method destroys.
4, assay
4.1 content assaying method: according to the Chinese Pharmacopoeia high effective liquid chromatography for measuring.
System suitability: be filling agent (3.9 * 150mm) with octadecylsilane chemically bonded silica; Methyl alcohol-8% acetic acid (16: 25) is mobile phase; Detect wavelength 277.0nm, 35 ℃ of column temperatures.Number of theoretical plate calculates and should be not less than 1500 by the wogonin peak.
The preparation of reference substance solution: it is appropriate that precision takes wogonin reference substance (50 ~ 60 ℃ of drying under reduced pressure are to constant weight), adds ethanol and make the solution of every 1ml containing wogonin 32 μ g, shakes up, and obtains.
The preparation of need testing solution: get 5, tablet of the present invention, be ground into fine powder.Get 0.1g, accurately weighed, put in the 25ml measuring bottle, add ethanol 20ml, ultrasonic processing 15 minutes, let cool, and adds ethanol to scale, shakes up, and filters.The accurate subsequent filtrate 1ml that draws, put in the 10ml measuring bottle, adds ethanol to scale, shakes up, and obtains.
Determination method: precision is drawn reference substance solution and each 5 μ l of need testing solution respectively, injects high performance liquid chromatograph, measures the wogonin peak area, and calculating, obtain.
Every, tablet of the present invention contains wogonin (C 16h 12o 5) must not be less than 17.5mg.
4.2 research data
4.2.1 instrument, medicine and reagent: high performance liquid chromatograph: Waters600 type pump, Waters600 controller, Shen, river chromatogram working software, Waters486 type UV-detector; Ultrasonic washing instrument (city of Kunshan ultrasonic process instrumentation company limited).Methyl alcohol is chromatographically pure, and water is ultrapure water, and it is pure that other reagent is analysis.
Wogonin reference substance pharmaceutical technology center in river provides.
4.2.2 chromatographic condition: Nova-pak C18 chromatographic column (150mm * 3.9mm), mobile phase: methyl alcohol-8% acetic acid (16: 25).Detect wavelength: 277.0nm, 35 ℃ of column temperatures.Number of theoretical plate calculates with wogonin, must not be lower than 1500.Under this condition, continuous three pins of the test liquid of tablet of the present invention (210930,210951,211021) (accompanying drawing 1) all went out peak fully in 20 minutes, and fully overlapping, and wogonin peak separation case meets the requirements.
In research process, once used acetonitrile-water-phosphoric acid, acetonitrile-water-acetic acid, methanol-water-phosphoric acid system, separating effect is better.But phosphoric acid acidity is stronger, acetonitrile is more expensive and toxicity is larger, therefore exclude text.
4.2.3 the selection of reference substance: the active component of tablet material medicine of the present invention is flavone aglycone, take baicalein, wogonin as main.Baicalein is containing three vicinal phenolic hydroxyl groups, very unstable, is difficult for making; And wogonin content is higher, stable chemical nature, and be one of main effective constituent, therefore the selection wogonin is reference substance.Use high performance liquid chromatograph, adopt area normalization method, the purity that records homemade wogonin reference substance reaches more than 99.64%.
4.2.4 the selection of extraction conditions: in tablet material medicine of the present invention, active component is that to take the flavone aglycone such as baicalein be main potpourri, and polarity is less, is dissolved in ethanol.Research shows, sample and reference substance are difficult for dissolve complete under heating condition, and ultrasonic processing solute effect is good.Once comparative studies sample ultrasonic process the difference (in Table 6) of 15 minutes and 30 minutes, result shows, the ultrasonic processing of tablet of the present invention can be extracted fully in 15 minutes, so to select the ultrasonic processing of ethanol 15 minutes be extraction conditions.
Table 6 equivalent sample ultrasonic is processed and is extracted result
Sequence number The ultrasonic processing time (minute) Peak area
1 15 1221148
2 15 1211623
3 15 1252328
4 30 1195596
5 30 1190786
6 30 1210875
4.2.5 measure the selection of wavelength: under acid condition, the wogonin reference substance has maximum absorption band at 277.5nm, but identical with the absorbance log at 277.0nm wavelength place, and tablet of the present invention also has maximum absorption band (276.5 is identical with 277.0nm place absorbance log) near 277.0nm, therefore select 277.0nm for measuring wavelength.
4.2.6 linear relationship and regression equation:
The preparation of typical curve: get reference substance 8mg, accurately weighed, put in the 100ml measuring bottle, add ethanol 90ml, ultrasonic processing 15 minutes, let cool, and adds ethanol to scale, shakes up.Accurate 0.0,1.0,2.0,3.0,4.0,5.0,7.0,9.0, the 10.0ml that draws, put in the 10ml measuring bottle, adds ethanol to scale, shakes up.The accurate 5 μ l that draw, inject high performance liquid chromatograph, take 277.0nm as detecting wavelength, measures peak area, the results are shown in Table 7.Take sample size as ordinate, and peak area is horizontal ordinate, and the drawing standard curve calculates regression equation: m=4.365375 * 10 -8a-0.001983, r=0.9998.Show that wogonin has good linear relationship in 0.0 ~ 0.4 μ g/ml scope, and typical curve is by initial point, as shown in Figure 1.
Table 7 HPLC standard curve determination result
Sequence number Sample size (μ g) Peak area (n=3)
1 0 0
2 0.04 9277340
3 0.08 1885226.0
4 0.12 2840686.0
5 0.16 3719543.0
6 0.20 4669386.0
7 0.28 6537937.0
8 0.36 8194791.0
9 0.40 9201962.0
4.2.7 precision test
Accurate reference substance solution (40 μ g/ml) the 5 μ l that draw, inject high performance liquid chromatograph, measures peak area, and continuous 6 times, result is as table 8.
Table 8 Precision test result
Figure 2012101781860100002DEST_PATH_IMAGE003
Above result shows, this method precision is good, and relative standard deviation is less than 2%.
4.2.8 stability test
At regular intervals, accurate need testing solution (800 μ g/ml) the 5 μ l that draw, inject high performance liquid chromatograph, measures peak area, and result is as table 9.
Table 9 stability test result
Figure 2012101781860100002DEST_PATH_IMAGE004
Above result shows, stable in need testing solution 7 hours, this method has good stability.
4.2.9 reappearance test
5 parts of sample thiefs (lot number 010521), measure according to " assay " lower method, and result is as table 10.
Table 10 reproducible test results
Figure 2012101781860100002DEST_PATH_IMAGE005
Above result shows, this method reappearance is good, and relative standard deviation is less than 2%.
4.2.10 recovery test
Get 5, tablet of the present invention (lot number 010521), porphyrize, get 50mg, accurately weighed, and totally 5 parts, it is appropriate that precision adds the wogonin reference substance solution respectively, waves most solvent, presses the lower method test of text " assay " item, and calculate recovery rate, the results are shown in Table 11.
Table 11 recovery test result
Figure 2012101781860100002DEST_PATH_IMAGE006
Above result shows, this method recovery is good, and relative standard deviation is less than 2%.
4.2.11 negative interference test
Get the sheet of blank auxiliary material compacting, by " assay " lower method, measure wogonin content, result is noiseless.
4.2.12 sample wogonin cubage formula
Content with one point external standard method calculation sample wogonin
250NA s
Figure 2012101781860100002DEST_PATH_IMAGE007
wogonin %(mg/mg)=* 100%
wA o
Annotate: in formula, N is reference substance concentration (mg/ml);
W is that test sample takes weight mg;
A sfor the test sample peak area;
A ofor the reference substance peak area.
4.2.13 sample determination
Get five batches of tablet pilot products of the present invention, measure by " assay " lower method, the results are shown in Table 12.
Table 12 sample determination result
Figure 2012101781860100002DEST_PATH_IMAGE008
According to above result, every, tentative tablet of the present invention is not less than 17.5mg containing wogonin.
Beneficial effect of the present invention is: the present invention adopts the content of high effective liquid chromatography for measuring wogonin, and adopt thin-layered chromatography to be measured radix scutellariae medicinal materials, described detection method is measured accurately, highly sensitive, reproducible, can effectively control the quality of the medicine for the treatment of dysmenorrhoea of the present invention, reach goal of the invention.
The accompanying drawing explanation
Fig. 1 is the wogonin canonical plotting
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment
Embodiment 1:
Prepared by tablet of the present invention: take Scullcap total-flavonoid aglycone 160g, microcrystalline cellulose 84g, pregelatinized starch 62.48g, sodium carboxymethyl starch 21g, polyvinylpolypyrrolidone 7g, lauryl sodium sulfate 1.75g, polyoxyethylene sorbitan monoleate 1.22g, talcum powder 4.55g and 30 POVIDONE K 30 BP/USP like this 30prepared by 8g: A, take lauryl sodium sulfate, polyoxyethylene sorbitan monoleate and 30 POVIDONE K 30 BP/USP by the following method 30be mixed with containing 30 POVIDONE K 30 BP/USP 30being 5% aqueous solution, is the A product; B, take the Scullcap total-flavonoid aglycone of 100 mesh sieves, added microcrystalline cellulose, pregelatinized starch and sodium carboxymethyl starch, mixed in mixer-granulator, obtained the B product; C, A product and B product being mixed, add the distilled water of 0.06 times of amount of B product to stir, granulate, obtain particle, is the C product; D, get the C product at the temperature of 70 ℃ dry 3 hours, dried particle, with after whole of 30 mesh sieves, adds polyvinylpolypyrrolidone and talcum powder to sieve and mixes, and trimmer is heavily 0.35g, and compressing tablet, obtain.
Described detection method is:
Proterties: be yellow sheet; Bitter;
Differentiate: get 2, tablet of the present invention, be ground into fine powder, get 0.1g, the 50ml that adds diethyl ether, ultrasonic processing 15 minutes, get ether solution 1ml, evaporate to dryness, residue adds methyl alcohol 1ml and dissolves, as need testing solution; Separately get root of large-flowered skullcap control medicinal material 0.5g, be made in the same way of control medicinal material solution; According to the Chinese Pharmacopoeia thin-layered chromatography, test, draw each 2 μ l of need testing solution and control medicinal material solution, put on same silica gel g thin-layer plate respectively, take chloroform: methyl alcohol: formic acid=be at 95: 5: 1 developping agent, pre-equilibration 30 minutes, launch, take out, dry, put under visible ray and inspect, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the principal spot of aobvious same color;
Check: should meet every regulation relevant under Chinese Pharmacopoeia tablet item;
Assay: according to the Chinese Pharmacopoeia high effective liquid chromatography for measuring;
System suitability: be filling agent 3.9 * 150mm with octadecylsilane chemically bonded silica; Methyl alcohol: 8% acetic acid=be at 16: 25 mobile phase; Detect wavelength 277.0nm, 35 ℃ of column temperatures, number of theoretical plate calculates and should be not less than 1500 by the wogonin peak;
The preparation of reference substance solution: precision takes the wogonin reference substance of 50-60 ℃ of drying under reduced pressure to constant weight, adds ethanol and makes the solution of every 1ml containing wogonin 32 μ g, shakes up, and obtains;
The preparation of need testing solution: get 5, tablet of the present invention, be ground into fine powder, get 0.1g, accurately weighed, put in the 25ml measuring bottle, add ethanol 20ml, ultrasonic processing 15 minutes, let cool, and adds ethanol to scale, shake up, filter, the accurate subsequent filtrate 1ml that draws, put in the 10ml measuring bottle, add ethanol to scale, shake up, obtain;
Determination method: precision is drawn reference substance solution and each 5 μ l of need testing solution respectively, injects high performance liquid chromatograph, measures the wogonin peak area, and calculating, obtain.
Embodiment 2:
Prepared by tablet of the present invention: take Scullcap total-flavonoid aglycone 170g, microcrystalline cellulose 90g, pregelatinized starch 70g, sodium carboxymethyl starch 25g, polyvinylpolypyrrolidone 10g, lauryl sodium sulfate 5g, polyoxyethylene sorbitan monoleate 5g, talcum powder 5g and 30 POVIDONE K 30 BP/USP like this 30prepared by 10g: A, take lauryl sodium sulfate, polyoxyethylene sorbitan monoleate and 30 POVIDONE K 30 BP/USP by the following method 30be mixed with containing 30 POVIDONE K 30 BP/USP 30being 5% aqueous solution, is the A product; B, take the Scullcap total-flavonoid aglycone of 120 mesh sieves, added microcrystalline cellulose, pregelatinized starch and sodium carboxymethyl starch, mixed in mixer-granulator, obtained the B product; C, A product and B product being mixed, add the water of 1 times of amount of B product to stir, granulate, obtain particle, is the C product; D, get the C product at the temperature of 80 ℃ dry 2 hours, dried particle, with after whole of 40 mesh sieves, adds polyvinylpolypyrrolidone and talcum powder to sieve and mixes, and trimmer is heavily 0.35g, and compressing tablet, obtain.
Described detection method is:
Differentiate: get 2, tablet of the present invention, be ground into fine powder, get 0.1g, the 50ml that adds diethyl ether, ultrasonic processing 15 minutes, get ether solution 1ml, evaporate to dryness, residue adds methyl alcohol 1ml and dissolves, as need testing solution; Separately get root of large-flowered skullcap control medicinal material 0.5g, be made in the same way of control medicinal material solution; According to the Chinese Pharmacopoeia thin-layered chromatography, test, draw each 2 μ l of need testing solution and control medicinal material solution, put on same silica gel g thin-layer plate respectively, take chloroform: methyl alcohol: formic acid=be at 95: 5: 1 developping agent, pre-equilibration 30 minutes, launch, take out, dry, put under visible ray and inspect, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the principal spot of aobvious same color.
Embodiment 3:
Prepared by tablet of the present invention: take Scullcap total-flavonoid aglycone 150g, microcrystalline cellulose 80g, pregelatinized starch 60g, sodium carboxymethyl starch 15g, polyvinylpolypyrrolidone 1g, lauryl sodium sulfate 0.1g, polyoxyethylene sorbitan monoleate 0.5g, talcum powder 3g and 30 POVIDONE K 30 BP/USP like this 30prepared by 1g: A, take lauryl sodium sulfate, polyoxyethylene sorbitan monoleate and 30 POVIDONE K 30 BP/USP by the following method 30be mixed with containing 30 POVIDONE K 30 BP/USP 30being 5% aqueous solution, is the A product; B, take the Scullcap total-flavonoid aglycone of 80 mesh sieves, added microcrystalline cellulose, pregelatinized starch and sodium carboxymethyl starch, mixed in mixer-granulator, obtained the B product; C, A product and B product being mixed, add the water of 0.03 times of amount of B product to stir, granulate, obtain particle, is the C product; D, get the C product at the temperature of 60 ℃ dry 4 hours, dried particle, with after whole of 20 mesh sieves, adds polyvinylpolypyrrolidone and talcum powder to sieve and mixes, and trimmer is heavily 0.35g, and compressing tablet, obtain.
Described detection method is:
Differentiate: get 2, tablet of the present invention, be ground into fine powder, get 0.1g, the 60ml that adds diethyl ether, ultrasonic processing 20 minutes, get ether solution 3ml, evaporate to dryness, residue adds methyl alcohol 3ml and dissolves, as need testing solution; Separately get root of large-flowered skullcap control medicinal material 1g, be made in the same way of control medicinal material solution; According to the Chinese Pharmacopoeia thin-layered chromatography, test, draw each 3 μ l of need testing solution and control medicinal material solution, put on same silica gel g thin-layer plate respectively, take chloroform: methyl alcohol: formic acid=be at 100: 7: 2 developping agent, pre-equilibration 35 minutes, launch, take out, dry, put under visible ray and inspect, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the principal spot of aobvious same color.
Embodiment 4:
The preparation method of tablet of the present invention is with embodiment 1
Described detection method is:
Differentiate: get 2, tablet of the present invention, be ground into fine powder, get 0.1g, the 40ml that adds diethyl ether, ultrasonic processing 10 minutes, get ether solution 0.5ml, evaporate to dryness, residue adds methyl alcohol 0.5ml and dissolves, as need testing solution; Separately get root of large-flowered skullcap control medicinal material 0.2g, be made in the same way of control medicinal material solution; According to the Chinese Pharmacopoeia thin-layered chromatography, test, draw each 2 μ l of need testing solution and control medicinal material solution, put on same silica gel g thin-layer plate respectively, take chloroform: methyl alcohol: formic acid=be at 90: 2: 0.5 developping agent, pre-equilibration 20 minutes, launch, take out, dry, put under visible ray and inspect, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the principal spot of aobvious same color.
Embodiment 5:
The preparation method of tablet of the present invention is with embodiment 1
Described detection method is:
Assay: according to the Chinese Pharmacopoeia high effective liquid chromatography for measuring;
System suitability: be filling agent 3.9 * 150mm with octadecylsilane chemically bonded silica; Methyl alcohol: 8% acetic acid=be at 16: 25 mobile phase; Detect wavelength 277.0nm, 35 ℃ of column temperatures, number of theoretical plate calculates and should be not less than 1500 by the wogonin peak;
The preparation of reference substance solution: precision takes the wogonin reference substance of 50-60 ℃ of drying under reduced pressure to constant weight, adds ethanol and makes the solution of every 1ml containing wogonin 32 μ g, shakes up, and obtains;
The preparation of need testing solution: get 5, tablet of the present invention, be ground into fine powder, get 0.1g, accurately weighed, put in the 25ml measuring bottle, add ethanol 20ml, ultrasonic processing 15 minutes, let cool, and adds ethanol to scale, shake up, filter, the accurate subsequent filtrate 1ml that draws, put in the 10ml measuring bottle, add ethanol to scale, shake up, obtain;
Determination method: precision is drawn reference substance solution and each 5 μ l of need testing solution respectively, injects high performance liquid chromatograph, measures the wogonin peak area, and calculating, obtain.
Embodiment 6:
The preparation method of tablet of the present invention is with embodiment 2
Described detection method is:
Assay: according to the Chinese Pharmacopoeia high effective liquid chromatography for measuring;
System suitability: be filling agent 3.9 * 150mm with octadecylsilane chemically bonded silica; Methyl alcohol: 10% acetic acid=be at 20: 30 mobile phase; Detect wavelength 300nm, 40 ℃ of column temperatures, number of theoretical plate calculates and should be not less than 1500 by the wogonin peak;
The preparation of reference substance solution: precision takes the wogonin reference substance of 50-60 ℃ of drying under reduced pressure to constant weight, adds ethanol and makes the solution of every 1ml containing wogonin 35 μ g, shakes up, and obtains;
The preparation of need testing solution: get 5, tablet of the present invention, be ground into fine powder, get 0.3g, accurately weighed, put in the 25ml measuring bottle, add ethanol 25ml, ultrasonic processing 20 minutes, let cool, and adds ethanol to scale, shake up, filter, the accurate subsequent filtrate 2ml that draws, put in the 10ml measuring bottle, add ethanol to scale, shake up, obtain;
Determination method: precision is drawn reference substance solution and each 7 μ l of need testing solution respectively, injects high performance liquid chromatograph, measures the wogonin peak area, and calculating, obtain.
Embodiment 7:
The preparation method of tablet of the present invention is with embodiment 3
Described detection method is:
Assay: according to the Chinese Pharmacopoeia high effective liquid chromatography for measuring;
System suitability: be filling agent 3.9 * 150mm with octadecylsilane chemically bonded silica; Methyl alcohol: 5% acetic acid=be at 10: 20 mobile phase; Detect wavelength 255nm, 30 ℃ of column temperatures, number of theoretical plate calculates and should be not less than 1500 by the wogonin peak;
The preparation of reference substance solution: precision takes the wogonin reference substance of 50-60 ℃ of drying under reduced pressure to constant weight, adds ethanol and makes the solution of every 1ml containing wogonin 30 μ g, shakes up, and obtains;
The preparation of need testing solution: get 5, tablet of the present invention, be ground into fine powder, get 0.1g, accurately weighed, put in the 25ml measuring bottle, add ethanol 15ml, ultrasonic processing 10 minutes, let cool, and adds ethanol to scale, shake up, filter, the accurate subsequent filtrate 0.5ml that draws, put in the 10ml measuring bottle, add ethanol to scale, shake up, obtain;
Determination method: precision is drawn reference substance solution and each 3 μ l of need testing solution respectively, injects high performance liquid chromatograph, measures the wogonin peak area, and calculating, obtain.

Claims (3)

1. treat the detection method of the medicine of dysmenorrhoea, it is characterized in that: the medicine of described treatment dysmenorrhoea calculates according to composition by weight, by Scullcap total-flavonoid aglycone 150-170 part, microcrystalline cellulose 80-90 part, pregelatinized starch 60-70 part, sodium carboxymethyl starch 15-25 part, polyvinylpolypyrrolidone 1-10 part, lauryl sodium sulfate 0.1-5 part, polyoxyethylene sorbitan monoleate 0.5-5 part, talcum powder 3-5 part and 30 POVIDONE K 30 BP/USP 30prepared by 1-10 part: A, take lauryl sodium sulfate, polyoxyethylene sorbitan monoleate and 30 POVIDONE K 30 BP/USP by the following method 30be mixed with containing 30 POVIDONE K 30 BP/USP 30being 5% aqueous solution, is the A product; B, take the Scullcap total-flavonoid aglycone of 80-120 mesh sieve, added microcrystalline cellulose, pregelatinized starch and sodium carboxymethyl starch, mixed in mixer-granulator, obtained the B product; C, A product and B product are mixed, the water that adds B product 0.03-1 doubly to measure stirs, and granulates, and obtains particle, is the C product; D, get C product dry 2-4 hour at the temperature of 60-80 ℃, dried particle, with after the whole grain of 20-40 mesh sieve, adds polyvinylpolypyrrolidone and talcum powder to sieve and mixes, and trimmer is heavily 0.35g, and compressing tablet, obtain tablet of the present invention; Described detection method comprises the steps:
Differentiate: get 2, tablet of the present invention, be ground into fine powder, get 0.1g, the 40-60ml that adds diethyl ether, ultrasonic processing 10-20 minute, get ether solution 0.5-3ml, evaporate to dryness, residue adds methyl alcohol 0.5-3ml and dissolves, as need testing solution; Separately get root of large-flowered skullcap control medicinal material 0.2-1g, be made in the same way of control medicinal material solution; According to the Chinese Pharmacopoeia thin-layered chromatography, test, draw need testing solution and each 1-3 μ l of control medicinal material solution, put on same silica gel g thin-layer plate respectively, take chloroform: methyl alcohol: formic acid=90-100: 2-7: 0.5-2 is developping agent, pre-equilibration 20-35 minute, launch, take out, dry, put under visible ray and inspect, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the principal spot of aobvious same color.
2. treat according to claim 1 the detection method of the medicine of dysmenorrhoea, it is characterized in that, described detection method also comprises:
Assay: according to the Chinese Pharmacopoeia high effective liquid chromatography for measuring;
System suitability: be filling agent 3.9 * 150mm with octadecylsilane chemically bonded silica; Methyl alcohol: 5-10% acetic acid=10-20: 20-30 is mobile phase; Detect wavelength 255-300nm, column temperature 30-40 ℃, number of theoretical plate calculates and should be not less than 1500 by the wogonin peak;
The preparation of reference substance solution: precision takes the wogonin reference substance of 50-60 ℃ of drying under reduced pressure to constant weight, adds ethanol and makes the solution of every 1ml containing wogonin 30-35 μ g, shakes up, and obtains;
The preparation of need testing solution: get 5, tablet of the present invention, be ground into fine powder, get 0.1-0.3g, accurately weighed, put in the 25ml measuring bottle, add ethanol 15-25ml, ultrasonic processing 10-20 minute, let cool, and adds ethanol to scale, shake up, filter, the accurate subsequent filtrate 0.5-2ml that draws, put in the 10ml measuring bottle, add ethanol to scale, shake up, obtain;
Determination method: precision is drawn reference substance solution and each 3-7 μ l of need testing solution respectively, injects high performance liquid chromatograph, measures the wogonin peak area, calculates, and obtains.
3. according to the detection method of the medicine of the described treatment dysmenorrhoea of claim 1 or 2, it is characterized in that, described detection method is:
Proterties: be yellow sheet; Bitter;
Differentiate: get 2, tablet of the present invention, be ground into fine powder, get 0.1g, the 50ml that adds diethyl ether, ultrasonic processing 15 minutes, get ether solution 1ml, evaporate to dryness, residue adds methyl alcohol 1ml and dissolves, as need testing solution; Separately get root of large-flowered skullcap control medicinal material 0.5g, be made in the same way of control medicinal material solution; According to the Chinese Pharmacopoeia thin-layered chromatography, test, draw each 2 μ l of need testing solution and control medicinal material solution, put on same silica gel g thin-layer plate respectively, take chloroform: methyl alcohol: formic acid=be at 95: 5: 1 developping agent, pre-equilibration 30 minutes, launch, take out, dry, put under visible ray and inspect, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the principal spot of aobvious same color;
Check: should meet every regulation relevant under Chinese Pharmacopoeia tablet item;
Assay: according to the Chinese Pharmacopoeia high effective liquid chromatography for measuring;
System suitability: be filling agent 3.9 * 150mm with octadecylsilane chemically bonded silica; Methyl alcohol: 8% acetic acid=be at 16: 25 mobile phase; Detect wavelength 277.0nm, 35 ℃ of column temperatures, number of theoretical plate calculates and should be not less than 1500 by the wogonin peak;
The preparation of reference substance solution: precision takes the wogonin reference substance of 50-60 ℃ of drying under reduced pressure to constant weight, adds ethanol and makes the solution of every 1ml containing wogonin 32 μ g, shakes up, and obtains;
The preparation of need testing solution: get 5, tablet of the present invention, be ground into fine powder, get 0.1g, accurately weighed, put in the 25ml measuring bottle, add ethanol 20ml, ultrasonic processing 15 minutes, let cool, and adds ethanol to scale, shake up, filter, the accurate subsequent filtrate 1ml that draws, put in the 10ml measuring bottle, add ethanol to scale, shake up, obtain;
Determination method: precision is drawn reference substance solution and each 5 μ l of need testing solution respectively, injects high performance liquid chromatograph, measures the wogonin peak area, and calculating, obtain.
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