CN105596559A - Girald daphne bark tablet for treating arthritis and nursing assistant medicine for metabolic syndrome - Google Patents
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- 210000000582 semen Anatomy 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 201000011549 stomach cancer Diseases 0.000 description 1
- 201000000498 stomach carcinoma Diseases 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000000153 supplemental effect Effects 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002435 venom Substances 0.000 description 1
- 210000001048 venom Anatomy 0.000 description 1
- 231100000611 venom Toxicity 0.000 description 1
- 230000002618 waking effect Effects 0.000 description 1
- 230000003442 weekly effect Effects 0.000 description 1
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Abstract
The invention relates to the technical field of traditional Chinese medicines, and in particular relates to a girald daphne bark tablet for treating arthritis and a nursing assistant medicine for a metabolic syndrome. The medicine is prepared by the following steps: taking girald daphne bark, adding water to decoct for three times, two hours for the first time, an hour for the second time and an hour for the third time; merging a decoction solution, filtering and concentrating filtrate into clear paste of which the relative density is 1.22-1.26; adding ethanol until the alcohol content reaches 75%; standing to participate, taking the supernatant, recovering ethanol and concentrating the supernatant; adding calcium carbonate, starch and dextrin, and mixing the calcium carbonate, the starch and the dextrin evenly to prepare particles; drying and pressing the particles into tablets; and coating each tablet with a film coating or a sugar coating. The medicine is used for preparing medicines or health products for treating the arthritis and the metabolic syndrome.
Description
Technical field
The present invention relates to the field of Chinese medicines, be specifically related to a kind of Giraldi daphne tablet and method for making thereof and new purposes.
Background technology
Girald daphne bark is the yellow winter daphne (Daphnegiraldii of Thymelaeceae (Thymelaeaceae) daphne plantNitsche) root skin and stem skin. Giraldi daphne tablet is dampclearing prescription, has and dispels rheumatism, effect of promoting blood circulation and stopping pain. Cure mainly chill wetImpatency, the numbness due to obstruction of collaterals by blood stasis, disease sees that limbs joint swells and ache, aversion to cold and cold limbs; Rheumatoid arthritis is shown in above-mentioned patient. ConventionalIn treatment of arthritis, rheumatoid arthritis; Also can be used for sciatica, scapulohumeral periarthritis. The drug standards of Giraldi daphne tablet are recordedIn version " Chinese pharmacopoeia " the 1321st page in 2015.
In existing report, show, 2000, Yang Jianhui, Tu little Wen, the people such as Wang Yanxia are at " the 6th national traditional Chinese and western medicine knotClose the academic meeting paper compilation of kidney trouble " upper report, girald daphne bark can be used for the treatment of glomerulonephritis. 2008, Lin Zhixiang, ZhengGood one-tenth, Dai Yichen, Dai Lushou, the people such as Zhou Mingxuan are at " Hainan medical science " upper report, and Giraldi daphne tablet can be used for treating rheumatoid and closesJoint is scorching. 2009, Chen Jianle reported in Master degree candidate's thesis of its Colleges Of Traditional Chinese Medicine Of Fujian, and Giraldi daphne tablet can be treatedSenile gonitis. 2013, Guo Xingfu, Wu Lijuan, Yu Jinyun, the people such as Song Yuping report at " practical traditional Chinese medicine magazine "Road, Giraldi daphne tablet can be treated acute low back pain. Chinese patent CN201310600707.1 discloses one and has treated weakness of the spleen and the stomachChinese medicine of type cancer of the stomach and preparation method thereof, the each raw medicinal material of Chinese medicine comprises: stomach cold grass, Mongollian Thyme Herb, semen brassicae, girald daphne bark, apricot leaf is anti-Wind, osmanthus, great Ye mountain, Alpinia henryik Schum, purging croton root, dyebark evodia fruit or root or leaf, elecampane, in one's early teens, Gomphocarpus Fruticosus L. b. br and Phoenix Tree Seed, Chinese medicine warm of the present inventionIn loose cold, strengthening the spleen and stomach, can significantly improve the symptom of due to weakness of spleen and stomach patients with gastric cancer. In Chinese patent CN201310714450.2Disclose one and treated migrainous Chinese medicine preparation of obstruction of collaterals by blood stasis type and preparation method thereof, the each raw medicinal material of Chinese medicine preparation comprises:Scaly holly root, the deer leaves of pulse plants, Rabdosia rubescens, dentiferous dendropanax root and stem, sweet basil, devilpepper, indian nightshade root, lemongrass, hookedhairypod tickclover leaf, girald daphne bark, laciniate blumea herb, tripGrass, Bai Guimu root and china creeper root, Chinese medicine preparation of the present invention is promoting blood circulation and removing blood stasis, removes obstruction in channels to relieve pain, and obstruction of collaterals by blood stasis type antimigraine is had definitelyCurative effect. A kind of Chinese medicine composition and preparation side thereof with antitumor action disclosed in Chinese patent CN201010195115.2Method and application, this Chinese medicine composition is made up of the raw material of following parts by weight: 10 ~ 100 parts of Ligusticum wallichiis, 10 ~ 200 parts of decumbent corydalis tubers, system1 ~ 50 part of monkshood, 10 ~ 300 parts of girald daphne barks, 10 ~ 100 parts of bark of ash, 1 ~ 50 part of the dried venom of toads; Chinese medicine composition provided by the invention hasWell inhibition tumor cell is grown and can be promoted the effect of apoptosis of tumor cells, and all has stronger to kinds of tumor cellsKilling action. Chinese invention patent CN201310299158.9 disclose a kind of Chinese medicine preparation for supplemental treatment depression andPreparation method, the constitutive material of this Chinese medicine preparation active ingredient is radix cynanchi bungei, bamboo juice, broomrape, Chinese ixeris herb, jasmine, red ginseng, foxThe heart, rhizoma Gastrodiae, iron essence, bark of ash, Michelia figo, the root of gansui, folium photiniae, cajeputtree, Radix Ariliae and girald daphne bark; Medicine of the present invention has thinLiver solution is strongly fragrant, nourishing blood and tranquilization, the calm tired effect of dispelling, the various causes of disease of neurasthenia, spirit cause because of to(for) auxiliary psychotherapyDivision, depression etc. have good effect.
Medicine provided by the invention can be used for the treatment of arthritis and metabolic syndrome. Show after deliberation medicine of the present inventionArthritis and metabolic syndrome are had to good result for the treatment of.
Summary of the invention
The object of this invention is to provide a kind of medicine of Giraldi daphne tablet.
Another object of the present invention is to provide the preparation method of this medicine.
The present invention also provides the new pharmaceutical use of this medicine.
The object of the invention is to be realized by following mode:
A medicine for Giraldi daphne tablet is to be made up of following raw material: girald daphne bark.
This medicine is adopted with the following method preparation: get girald daphne bark, and boiling three times, 2 hours for the first time, for the second time, the 3rdInferior 1 hour, collecting decoction, filtered, and it is 1.22 1.26 clear cream that filtrate is concentrated into relative density, added ethanol and made to reach containing alcohol amount75%, leave standstill and make precipitation, get supernatant, reclaim ethanol concentrated, add calcium carbonate, starch, dextrin, mix, granulation, dryDry, in flakes, film coating or sugar-coat, to obtain final product in compacting.
This medicine can be for the preparation for the treatment of of arthritis, metabolic syndrome medicine or health products.
Experiment one: the experimental study of medicine treatment metabolic syndrome of the present invention
One, materials and methods
1. experiment material
1.1 instrument reagent
Blood sugar test paper and rapid blood sugar instrument are purchased from Abbott of the U.S., and four items of blood lipid tests reagent is opened up biological skill in examining purchased from Beijing worldArt Co., Ltd, micro-injection pump is purchased from German Bei Lang company, and insulin uses Novolin R, hand held FEJ-1000B electronicsScale, purchased from Foochow Electronics Co., Ltd. of Furistock.
1.2 animal used as test
50 of clean level SD rats in male 6 week age, feed, experimental site are carried by medical board animal portion of Nanjing University of Traditional Chinese MedicineConfession, 4～5, every cage, freely drinks drinking water, and the 12h daily cycle feeds.
1.3 Experimental agents
Medicine of the present invention: prepare with reference to the embodiment 1 in description detailed description of the invention of the present invention.
The composition of Avandia is Rosiglitazone Maleate Tablets (RM), and 4mg/ sheet, by U.S.'s GlaxoSmithKline PLC (Tianjin) Co., LtdProduce the accurate word H20020475 of traditional Chinese medicines.
2. the foundation of model
Rats in normal control group is fed with common standard feed (carbohydrate 60%, fat 11%, protein 29%); Model groupRat is fed 8 Zhou Houcheng with high lipid food (78.8% basal feed, 1% cholesterol, 10% yolk powder, 10% lard, 0.2% cholate)Mould, weight and visceral fat mass all significantly raise.
3. grouping and administration
Rat is divided into 4 groups at random, Normal group, metabolic syndrome group, Avandia group, medicine group of the present invention, every group each 10Rat; Normal group is fed and is raised common standard feed, all the other rat feeding high lipid foods.
The medicine of throwing something and feeding: after Cheng Mo, model group rat is divided at random to metabolic syndrome group, Avandia group, medicine of the present inventionGroup; Start Avandia group from the 9th week and press 2mgkg-1·d-1, to feed and raise Avandia, medicine group of the present invention is pressed 60mgkg-1·d-1Feed and raise medicine of the present invention, medicine is all with physiological saline solution; Normal group, the metabolic syndrome group same ratio volume of throwing something and feedingPhysiological saline, continues to feed after 4 weeks the test of row clamp.
4. experimental index is measured
Under waking state, get blood, use EDAT anti-freezing, TG, TC, HDL-C, LDL-C measures with biochemical process. FPI (IFNS)Measure with putting the method for exempting from. All rats, in process of the test, are measured weekly weight 1 time. With RBP-l type rat blood pressure meter, adoptMouse tail cuff pressurization blocked method Measure blood pressure, measures 1 time for every two weeks.
5. visceral fat mass takes method
After rat is put to death, cut abdominal cavity open, get the attached wet quality of other fat of starting in right side and replace visceral fat mass.
6. measure insulin sensitivity
Evaluate the sensitiveness of insulin by euglycemia hyperinsulinism clamp (GC) method. Each group rat (is pressed with 10% chloraldurateEvery 300g rat weight 1ml) through intraperitoneal anesthesia, insert people's conduit (PE-50) the 2nd day to right carotid and left jugular vein, clearlyWake up under state and measure after fasting blood-glucose (FBS), respectively with initial concentration and the 4mUkg of 25mU/kg-1·min-1Maintain concentration,Continue 150min drip-feed insulin; The every 7min of blood glucose value measures 1 time, instils with 12.5% Glucose Liquid during continuous intravenous infusion simultaneously;For maintaining fasting blood glucose level, suitably adjust; Its infusion velocity. After blood glucose value is stable, with GC method (grape in last 35minThe mean value of sugar infusion velocity, M value) evaluation insulin sensitivity.
7. data analysis
All data with± s represents; Between each group basic statistics amount and homogeneity test of variance and two groups, more all add up with SPSSLearn software analysis.
Two, result
Each group weight and interior fat relatively in Table 1-1, show 1-2.
Table 1-1 respectively organize rat weight variation (±s，g）
Note: with Normal group comparison, * P < 0.05.
The comparison of weight and interior fat when table 1-2 respectively organizes rat 12 weeks (n=10,±s）
Note: with Normal group comparison, * P < 0.05.
Metabolic syndrome group compared with normal control group weight and interior fat increase obviously (P < 0.05); Table 2 can be found outAvandia and medicine group of the present invention are compared with metabolic syndrome group, and weight and interior fat all have downward trend, indifference between two groupsDifferent.
2. the comparison of each group FBS, FINS, M value
In Table 1-3. Metabolic syndrome group compared with normal control group M value obviously reduces (P < 0.01), FINS obviously raise (P < 0.01);Medicine group of the present invention is compared with the obvious rising of metabolic syndrome group M value (P < 0.05), and FINS obviously reduces (P < 0.05).
Table 1-3 respectively organize FBS, FINS and M value comparison (±s）
Note: with Normal group comparison, * P < 0.05, * * P < 0.01; With the comparison of metabolic syndrome group, △ P < 0.05.
3. the comparison of each group blood lipid level
In Table 1-4. Metabolic syndrome group compared with normal control group TC, TG, LDL-C obviously increase, HDL-C indifference; Medicine of the present inventionThing group obviously reduces compared with metabolic syndrome group TC, TG, LDL-C, improves not obvious to HDL-C.
Table 1-4 respectively organize comparison between TC, TG, LDL-C, HDL-C (±s，mmol/L）
Note: with Normal group comparison, * P < 0.05, * * P < 0.01; With the comparison of metabolic syndrome group, △ P < 0.05.
Three, conclusion
Experimental data demonstration, modeling is after 8 weeks, and model group compared with normal control group Insulin Sensitivity Index (M value) obviously reduces, bodyQuality and interior fat obviously increase, and blood lipid level obviously raises, and serum insulin also has rising trend simultaneously; Prompting is with centerProperty fat and insulin resistance centered by, merge that blood pressure increases, the Metabolic Syndrome one-tenth of blood fat disorder, hyperinsulinemiaMerit is set up. Clinical research and epidemiological survey find that obesity, super severe one are often with insulin resistance and abnormalities of sugar/lipid metabolism, fatBe organized in the pathogenesis of insulin resistance and play an important role.
The insulin sensitivity that experimental result demonstration medicine of the present invention can obviously improve metabolic syndrome group has in reductionThe trend of dirty fat and serum insulin levels, has improved serum TC, TG, LDL-C level significantly. Medicine of the present invention can haveEffect treatment complex treatment metabolic syndrome.
Experiment two: medicine high performance liquid chromatography quality determining method research of the present invention
1 instrument and reagent
1.1 instrument
High performance liquid chromatograph (Agilent110 high performance liquid chromatograph and work station, G1311Aquat pump, the inspection of G1314 ultravioletSurvey device).
1.2 reagent
Yellow daphnin A reference substance (Chinese pharmaceutical biological product is examined and determine research institute); Chinese medicine composition of the present invention: say with reference to the present inventionPrepared by the embodiment 1 in bright book detailed description of the invention; Chinese medicine (Kang Ji chain pharmacy provides); Methyl alcohol (chromatogram alcohol, Shanghai biochemistryWork auxiliary reagent factory); Other reagent are pure for analyzing.
2 methods and result
2.1 prescription
Girald daphne bark 1100g
2.2 preparation
Get girald daphne bark, boiling three times, 2 hours for the first time, for the second time, 1 hour for the third time, collecting decoction, filtered, and filtrate is denseBe reduced to relative density and be 1.22 1.26 clear cream, add ethanol and make to reach 75% containing alcohol amount, leave standstill and make precipitation, get supernatant, reclaim secondAlcohol is also concentrated, adds calcium carbonate, starch, dextrin, mix, and granulation, dry, be pressed into 1000, film coating or sugar-coat,Obtain.
The assay of 2.3 yellow daphnin A
2.3.1HPLC chromatographic condition
Adopt HypersilDs(4.0mm × 125mm, m) chromatographic column of 5 μ; Mobile phase: the acetonitrile-water that ratio is 30:70; Detect rippleLong: 200nm; Column temperature: 20 DEG C; Flow velocity: 1.0mLmin-1; Sample size: 10 μ L; Under this chromatographic condition, reference substance and sample lookSpectrum peak is good, noiseless to measuring without girald daphne bark's negative control.
2.3.2 the preparation of reference substance solution
It is appropriate that precision takes 80 DEG C of yellow daphnin A reference substances that are dried to constant weight, adds methyl alcohol and make the solution of every 1mL containing 0.2mg.
2.3.3 the preparation of need testing solution and negative controls
Precision takes medicine 10g of the present invention, adds methyl alcohol 40mL, adds hot reflux 4h, extract reflux solvent and be concentrated into dry, residueThe 10mL that adds water dissolves, extracts 5 times with water saturated n-butanol jolting, and each 20mL, merging n-butanol extracting liquid, washes with ammonia solutionWash 3 times, each 15mL, n-butanol extracting liquid reclaims solvent to dry, and residue adds methyl alcohol and dissolves and be transferred in 10mL volumetric flask, addsMethyl alcohol, to scale, shakes up, and filters, and gets filtrate and get final product; Separately do not contain girald daphne bark's negative control product in the preparation of prescription ratio, same to legal systemBecome negative controls.
2.3.4 the drafting of calibration curve
It is appropriate that precision takes 80 DEG C of yellow daphnin A reference substances that are dried to constant weight, makes 10.4,20.8,41.6 with methyl alcohol,83.2，166.4μgmL-1The solution of series concentration, precision measures the each 10 μ L of above-mentioned 5 kinds of concentration solution respectively, injects high efficiency liquid phaseChromatograph is measured.
Carry out linear regression with peak area ratio and concentration, obtain regression equation and be: A=21.2763C-0.1391, r=0.9999. Show that yellow daphnin A is at 10.4～166.4 μ gmL-1In concentration range, be good linear relationship.
2.3.5 stability test
The accurate need testing solution 10 μ L that draw, respectively at 0,1,2,4,8h sample introduction, and calculate yellow daphnin A content. In result 8hRSD is 0.45%(n=5). Show that sample solution is stable in 8h.
2.3.6 replica test
Press 5 parts, need testing solution preparation method parallel processing sample, measure yellow daphnin A content in accordance with the law and calculate. Result recordsYellow daphnin A average content is 0.12mgmL-1, RSD is 1.3%.
2.3.7 Precision Experiment
The yellow daphnin A reference substance solution of accurate absorption, repeats sample introduction 5 times, measures peak area in accordance with the law. Result RSD is 0.23%(n=5). Show that precision is better.
2.3.8 rate of recovery experiment
Precision takes 6 parts, the sample of the same lot number of known yellow daphnin A content, by high, medium and low concentration respectively precision add suitableThe yellow daphnin A reference substance solution of amount by operating under sample determination item, is measured calculate recovery rate in accordance with the law. Result average recovery rateBe that 100.3%, RSD is 0.45%(n=5).
2.3.9 sample size is measured
Measure reference substance solution respectively and need testing solution is appropriate, filter with miillpore filter, each sample introduction 10 μ L, by above-mentioned chromatostripPart is measured 3 batch samples, parallel determination 5 times. Content by external standard method with the yellow daphnin A of calculated by peak area need testing solution. This productShould be and indicate 95%～105% of content containing yellow daphnin A, containing yellow daphnin A, must not be less than 0.12mg in every 1g this product. 3 batchesSample size is respectively 100.8%(RSD=1.2%), 101.7%(RSD=1.3%), 99.2%(RSD=1.1%).
Experiment three: the containing of medicine air phase chromatography Simultaneous Determination AP20am16 of the present invention, podocarpus lipidolAmount
1 instrument and reagent
Agilent7890N gas chromatograph: fid detector, A.01.12.1 chromatographic work station; SGH-300 high-purity hydrogen is sent outRaw device (Beijing Orient elite science and technology garden Science and Technology Ltd.); Chromatographic column fused-silica capillary column (30m × 0.25mm, 0.25 μM); Plum Teller-Tuo benefit 100,000/electronic analytical balance; AP20am16 reference substance (content 99.9%,National Institute for Food and Drugs Control); Podocarpus lipidol reference substance (content 99.9%, National Institute for Food and Drugs Control); ThisInvention medicine (preparing with reference to the embodiment 1 in description detailed description of the invention of the present invention), reagent: cyclohexanone, absolute ethyl alcohol is equalFor chromatographically pure.
2 chromatographic conditions
Chromatographic column: ZB-WAX fused-silica capillary column (30m × 0.25mm, 0.25 μ is m); Carrier gas: N2，1.0mL·mL-1; HydrogenGas, 40mLmL-1; Air, 400mLmin-1; Split ratio: 10:1; Injector temperature: 250 DEG C, 300 DEG C of detector temperatures;Temperature programming: initial 80 DEG C, 5 DEG C per minute rise to 120 DEG C, and 10 DEG C per minute rise to 180 DEG C, keeps 3.5min; Internal standard method.
3 test methods and result
The preparation of 3.1 inner mark solutions
Get cyclohexanone appropriate, add anhydrous alcohol solution dilution and make the solution of every 1g containing 12.5mg, shake up, molten as interior markLiquid.
The preparation of 3.2 need testing solutions
Precision measures this product 1.0g, puts in 10mL volumetric flask, add absolute ethyl alcohol and be diluted to scale, then precision measures 1.0mL, putsIn 10mL volumetric flask, precision adds inner mark solution 1.0mL, adds absolute ethyl alcohol and is diluted to scale, shakes up.
The preparation of 3.3 reference substance stock solutions
Precision takes AP20am16 reference substance, podocarpus lipidol reference substance is appropriate, adds anhydrous alcohol solution rareRelease and make containing AP20am16 0.301mgmL-1And podocarpus lipidol 0.901mgmL-1Reference substance depositSolution, for subsequent use;
The preparation of 3.4 negative control solutions
Get by the blank solution that does not add AP20am16 and podocarpus lipidol in prescription, by " 3.2 " lower preparation sideMethod, makes negative control solution.
The investigation of 3.5 linear relationships
Respectively precision pipette 0.2,0.5,1.0,1.5,3.5mL reference substance storing solution in 10mL volumetric flask, add inner mark solution1.0mL, adds absolute ethyl alcohol and is diluted to scale, shakes up, and product solution in contrast, gets respectively 1 μ L sample introduction, records chromatogram, with 4-Methyl-7-hydroxy-coumarin, podocarpus lipidol and interior target peak area ratio are ordinate (Y), and concentration (C) is abscissa (X),Drawing standard curve, obtains regression equation and is respectively: Y(4-Methyl-7-hydroxy-coumarin respectively)=1.1148X-0.0016, R2=0.9999, AP20am16 concentration is at 0.146～2.555mgmL-1In scope, linear relationship is good; Y(arhatRosin spirit)=1.1347X+0.0035, R2=0.9998, podocarpus lipidol concentration is at 0.198～3.465mgmL-1In scope, lineSexual intercourse is good.
3.6 precision test
Getting AP20am16 concentration is 0.230mgmL-1With podocarpus lipidol concentration be 0.290mgmL-1'sReference substance solution, repeats sample introduction 6 times, records peak area, calculates respectively 2 kinds of compositions and interior target peak area ratio (mark in A/A),The RSD of AP20am16, podocarpus lipidol be respectively 0.24% and 1.2%(n=6).
3.7 replica test
Get same batch sample, by the method replication under sample determination item 6 times, result AP20am16, arhatThe RSD of rosin spirit is respectively 0.36%, 1.8%(n=6).
3.8 stability test
Get same batch sample solution, at room temperature place respectively 0,2,4,6,8, measure after 12h, result is pressed 4-methyl-7-hydroxylThe RSD of cumarin, podocarpus lipidol is respectively 0.38%, 1.7%, and interpret sample solution is measured in 12h, and result is stable.
3.9 average recovery tests
Get 9 parts of the sample solutions of known content, and add suitable basic, normal, high reference substance solution, measure 4-by sample determination methodMethyl-7-hydroxy-coumarin, podocarpus lipidol content, calculate recovery rate, the results are shown in Table 3-1 respectively.
Table 3-1 determination of recovery rates result (n=9, %)
Result shows, the rate of recovery of this method is better, the rate of recovery of AP20am16 respectively 99.4%～100.2%, the rate of recovery of podocarpus lipidol is between 98.1%～100.7%, and relative standard deviation is respectively 0.28% and 0.86%,This assay method can meet the assay of AP20am16 and podocarpus lipidol in medicine of the present invention.
3.10 quantitative limit and detectability
Adopt " signal to noise ratio method " to determine quantitative limit and the detectability of this research, line taking standard liquid is appropriate, and employing adds anhydrousEthanol progressively dilution method dilutes, when sample introduction concentration is 6.27,9.90 μ gmL-1Time, get 1 μ L sample introduction, continuous sample introduction 3 times,Obtain AP20am16, interior mark, podocarpus lipidol signal to noise ratio mean value and approach respectively 10.0, can be with this concentrationFor quantitative limit; Continue dilution sample introduction, when sample introduction concentration is 1.044,1.65 μ gmL-1, continuous sample introduction 3 times, obtains 4-methyl-7-Hydroxycoumarin, interior mark, podocarpus lipidol signal to noise ratio mean value approach 3.0, can be taking this concentration as detectability.
3.11 serviceability test
Investigate and stability of solution investigation through different chromatographic columns, and column temperature, injector temperature and detector temperature are investigated, and showThis method good tolerance, is applicable to the assay of two components in medicine of the present invention.
3.11.1 the impact of chromatographic column
Select the chromatographic column of 3 different commercial specifications, measure the content of same batch sample, the RSD% that calculates content value is respectively1.3,1.7,1.6. Result shows, different PEG chromatographic column mensuration content for sample, AP20am16, podocarpusLipidol all can effectively separate with interior mark, illustration method good tolerance.
3.11.2 the impact of column temperature
Column temperature is mainly on the impact separating the appearance time that affects main peak, and temperature is higher, and main peak appearance time is shorter, firstStage, while being 80 DEG C, AP20am16 main peak AP20am16 and impurity peak energy ensured that baseline dividesDuring from 120 DEG C of, second stage, podocarpus lipidol main peak and impurity peak energy ensure baseline separation, and the RSD of content is little at each temperatureIn 2.0%.
3.11.3 the impact of injector temperature
Injector temperature is during higher than column temperature, and AP20am16 and impurity peaks can ensure baseline separation, arhat rosinAlcohol separates good with impurity, and the RSD of content is less than 2.0% at each temperature.
3.11.4 the impact of detector temperature
Detector temperature is during higher than injector temperature, and AP20am16 and impurity peaks can ensure baseline separation, sieveChinese rosin spirit separates good with impurity, and the RSD of content is less than 2.0% at each temperature.
3.12 sample size measurement result
Through methodology checking, this content assaying method is easy and simple to handle, the degree of accuracy is high, favorable reproducibility, can more effectively control productProduct quality. Therefore apply the method to 10 batch samples, adopt internal standard method to carry out assay according to preceding method, the results are shown in Table 3-2。
Table 3-2 sample size measurement result
4 discuss
4.1 system suitability test
Under this test gas chromatography system, draw respectively sample determination with mixing reference substance solution, need testing solution and feminine genderThe each 1 μ L of contrast solution, records chromatogram. 2 kinds of components all can separate preferably with internal standard compound, negative noiseless. This system is suitableAnswering property the results are shown in Table 3-3.
Table 3-3 system suitability test
The selection of 4.2 internal standard compounds
Once tried out cyclohexanone, naphthalene, biphenyl, gaultherolin etc., because sample volatile ingredient is many, result is with the reservation of cyclohexanoneTime and separating effect are most suitable.
The selection of 4.3 column temperatures
The boiling point of AP20am16, cyclohexanone and podocarpus lipidol differs larger, when column temperature is low, and arhat rosinThe retention time of alcohol is long, and when column temperature is high, AP20am16 can not effectively separate with impurity, through adopting two sections of journeysWhen meeting two kinds of compositions, order heating mode analyzes.
The content limit of 4.4 this product
By 10 batch products measurement results, the content limit of tentative this product is: the every 1g of this product is not containing AP20am160.200mg must be less than, 0.200mg must not be less than containing podocarpus lipidol.
This method separates simultaneously and detects 2 kinds of compositions, and method is quick, sensitive, and separating degree is good, specificity is good, energyEffectively control drug quality.
Detailed description of the invention:
Embodiment 1: medicine of the present invention
Prescription: girald daphne bark 1100g
Method for making: get girald daphne bark, boiling three times, 2 hours for the first time, for the second time, 1 hour for the third time, collecting decoction, filtered,It is 1.22 1.26 clear cream that filtrate is concentrated into relative density, adds ethanol and makes to reach 75% containing alcohol amount, leaves standstill and makes precipitation, gets supernatant,Reclaim ethanol concentrated, add calcium carbonate, starch, dextrin, mix, granulation, dry, be pressed into 1000, film coatingOr sugar-coat, to obtain final product.
Cure mainly: be used for the treatment of arthritis, metabolic syndrome.
Usage and consumption: oral. One time 13,23 times on the one.
Detection method:
1, adopt high-efficient liquid spectrometry to carry out assay to yellow daphnin A:
(1) chromatographic condition: adopt HypersilDs chromatographic column; Mobile phase: the acetonitrile-water that ratio is 30:70; Detect wavelength:200nm; Column temperature: 20 DEG C; Flow velocity: 1.0mLmin-1; Sample size: 10 μ L;
(2) reference substance solution preparation: it is appropriate that precision takes 80 DEG C of yellow daphnin A reference substances that are dried to constant weight, adds methyl alcohol and dissolvesMake the reference substance solution of every 1mL containing 0.2mg;
(3) preparation of need testing solution: precision takes medicine 10g of the present invention, adds methyl alcohol 40mL, adds hot reflux 4h, and extract returnsStream solvent is also concentrated into dryly, and the residue 10mL that adds water dissolves, extract 5 times with water saturated n-butanol jolting, and each 20mL, merging is justButanols extract, with ammonia solution washing 3 times, each 15mL, n-butanol extracting liquid reclaims solvent to dry, and residue adds methyl alcohol and dissolves alsoBe transferred in 10mL volumetric flask, add methyl alcohol to scale, shake up, filter, get filtrate, obtain need testing solution;
(4) measure: precision measures above-mentioned need testing solution, the each 10 μ L of reference substance solution respectively, inject high performance liquid chromatograph, enterRow detects;
(5) measurement result: containing yellow daphnin A, must not be less than 0.12mg in every 1g this product.
2, adopt gas chromatography to carry out assay to AP20am16, podocarpus lipidol:
(1) chromatographic condition: chromatographic column: ZB-WAX fused-silica capillary column; Carrier gas: N2，1.0mL·mL-1; Hydrogen, 40mLmL-1; Air, 400mLmin-1; Split ratio: 10:1; Injector temperature: 250 DEG C, 300 DEG C of detector temperatures; Temperature programming:Initial 80 DEG C, 5 DEG C per minute rise to 120 DEG C, and 10 DEG C per minute rise to 180 DEG C, keep 3.5min; Internal standard method;
(2) preparation of inner mark solution: get cyclohexanone appropriate, add anhydrous alcohol solution dilution and make molten containing 12.5mg of every 1mLLiquid, shakes up, as inner mark solution;
(3) preparation of need testing solution: precision measures this product 1.0g, puts in 10mL volumetric flask, and add absolute ethyl alcohol and be diluted to scale,Precision measures 1.0mL again, puts in 10mL volumetric flask, and precision adds inner mark solution 1.0mL, adds absolute ethyl alcohol and is diluted to scale, shakesEven;
(4) preparation of reference substance solution: precision takes AP20am16 reference substance, podocarpus lipidol reference substance is suitableAmount, adds anhydrous alcohol solution and dilution is made containing AP20am16 0.301mgmL-1And podocarpus lipidol0.901mg·mL-1Reference substance stock solution, for subsequent use;
(5) measure: precision measures above-mentioned need testing solution, the each 10 μ L of reference substance solution respectively, and inject gas chromatograph, examinesSurvey;
(6) measurement result: the every 1g of this product must not be less than 0.200mg containing AP20am16, must not containing podocarpus lipidolBe less than 0.200mg.
In addition although should be appreciated that this description is described according to embodiment, be not that each embodiment only wraps,Contain an independently technical scheme, this narrating mode of description is only that for clarity sake those skilled in the art shouldDescription is done as a whole, the technical scheme in each embodiment also can be through appropriately combined, forms those skilled in the artUnderstandable other embodiments.
Claims (8)
1. a Giraldi daphne tablet medicine, is characterized in that, this medicine is to be made up of following raw material: girald daphne bark.
2. medicine as claimed in claim 1, is characterized in that, this medicine is adopted preparation with the following method: get girald daphne bark, add decoctingBoil three times, 2 hours for the first time, for the second time, 1 hour for the third time, collecting decoction, filtered, and filtrate is concentrated into relative density and is1.22 1.26 clear cream, adds ethanol and makes to reach 75% containing alcohol amount, leaves standstill and makes precipitation, gets supernatant, reclaims ethanol concentrated, addsCalcium carbonate, starch, dextrin, mix, and granulation is dry, and in flakes, film coating or sugar-coat, to obtain final product in compacting.
3. the medicine as described in any one in claim 1～2 is for the preparation of in treatment metabolic syndrome medicine or health productsApplication.
4. the medicine as described in any one in claim 1～2 is for the preparation of answering in medicament for treating arthritis or health productsWith.
5. the medicine as described in any one in claim 1～2, is characterized in that, adopts high performance liquid chromatography auspicious to HuangFragrant glycosides A carries out assay:
(1) chromatographic condition: adopt HypersilDs chromatographic column; Mobile phase: the acetonitrile-water that ratio is 20～40:60～80; DetectWavelength: 190～210nm; Column temperature: 15～25 DEG C; Flow velocity: 0.5～1.5mLmin-1; Sample size: 5～20 μ L;
(2) reference substance solution preparation: precision takes that to be dried to the yellow daphnin A reference substance of constant weight appropriate, adds methyl alcohol and dissolves and makeReference substance solution;
(3) preparation of need testing solution: precision takes medicine of the present invention, adds methyl alcohol, adds hot reflux, extract reflux solvent is also denseBe reduced to dryly, residue is dissolved in water, and extracts with water saturated n-butanol jolting, merges n-butanol extracting liquid, with ammonia solution washing, justButanols extract reclaims solvent to dry, and residue adds methyl alcohol and dissolves, and shakes up, and filters, and gets filtrate, obtains need testing solution;
(4) measure: precision measures above-mentioned need testing solution, each 5～20 μ L of reference substance solution respectively, inject high performance liquid chromatographyInstrument, detects.
6. medicine as claimed in claim 5, is characterized in that, adopts high-efficient liquid spectrometry to carry out assay to yellow daphnin A:
(1) chromatographic condition: adopt HypersilDs chromatographic column; Mobile phase: the acetonitrile-water that ratio is 30:70; Detect wavelength:200nm; Column temperature: 20 DEG C; Flow velocity: 1.0mLmin-1; Sample size: 10 μ L;
(2) reference substance solution preparation: it is appropriate that precision takes 80 DEG C of yellow daphnin A reference substances that are dried to constant weight, adds methyl alcohol and dissolvesMake the reference substance solution of every 1mL containing 0.2mg;
(3) preparation of need testing solution: precision takes medicine 10mL of the present invention, adds methyl alcohol 40mL, adds hot reflux 4h, and extract returnsStream solvent is also concentrated into dryly, and the residue 10mL that adds water dissolves, extract 5 times with water saturated n-butanol jolting, and each 20mL, merging is justButanols extract, with ammonia solution washing 3 times, each 15mL, n-butanol extracting liquid reclaims solvent to dry, and residue adds methyl alcohol and dissolves alsoBe transferred in 10mL volumetric flask, add methyl alcohol to scale, shake up, filter, get filtrate, obtain need testing solution;
(4) measure: precision measures above-mentioned need testing solution, the each 10 μ L of reference substance solution respectively, inject high performance liquid chromatograph, enterRow detects.
7. the medicine as described in any one in claim 1～2, is characterized in that, adopts gas chromatography to 4-methyl-7-Hydroxycoumarin, podocarpus lipidol carry out assay:
(1) chromatographic condition: chromatographic column: ZB-WAX fused-silica capillary column; Carrier gas: N2，0.5～1.5mL·mL-1; Hydrogen, 30～50mL·mL-1; Air, 300～500mLmin-1; Split ratio: 5～15:1; Injector temperature: 240～260 DEG C, detectActuator temperature: 290～310 DEG C; Temperature programming: initial 80 DEG C, 5 DEG C per minute rise to 120 DEG C, and 10 DEG C per minute rise to 180 DEG C, protectsHold 3.5min; Internal standard method;
(2) preparation of inner mark solution: get cyclohexanone appropriate, add anhydrous alcohol solution and dilute and make solution, shake up, as interior markSolution;
(3) preparation of need testing solution: precision measures this product, puts in volumetric flask, and add absolute ethyl alcohol and be diluted to scale, more accurate amountGet, put in volumetric flask, precision adds inner mark solution, adds absolute ethyl alcohol and is diluted to scale, shakes up;
(4) preparation of reference substance solution: precision takes AP20am16 reference substance, podocarpus lipidol reference substance is suitableAmount, adds anhydrous alcohol solution and the reference substance stock solution containing AP20am16 and podocarpus lipidol is made in dilution,For subsequent use;
(5) measure: precision measures above-mentioned need testing solution, each 5～20 μ L of reference substance solution respectively, and inject gas chromatograph, entersRow detects.
8. medicine as claimed in claim 7, is characterized in that, adopts gas chromatography to AP20am16, sieveChinese rosin spirit carries out assay:
(1) chromatographic condition: chromatographic column: ZB-WAX fused-silica capillary column; Carrier gas: N2，1.0mL·mL-1; Hydrogen, 40mLmL-1; Air, 400mLmin-1; Split ratio: 10:1; Injector temperature: 250 DEG C, 300 DEG C of detector temperatures; Temperature programming:Initial 80 DEG C, 5 DEG C per minute rise to 120 DEG C, and 10 DEG C per minute rise to 180 DEG C, keep 3.5min; Internal standard method;
(2) preparation of inner mark solution: get cyclohexanone appropriate, add anhydrous alcohol solution dilution and make molten containing 12.5mg of every 1mLLiquid, shakes up, as inner mark solution;
(3) preparation of need testing solution: precision measures this product 1.0mL, puts in 10mL volumetric flask, adds absolute ethyl alcohol and is diluted to quarterDegree, then precision measures 1.0mL, puts in 10mL volumetric flask, precision adds inner mark solution 1.0mL, and add absolute ethyl alcohol and be diluted to scale,Shake up;
(4) preparation of reference substance solution: precision takes AP20am16 reference substance, podocarpus lipidol reference substance is suitableAmount, adds anhydrous alcohol solution and dilution is made containing AP20am16 0.301mgmL-1And podocarpus lipidol0.901mg·mL-1Reference substance stock solution, for subsequent use;
(5) measure: precision measures above-mentioned need testing solution, the each 10 μ L of reference substance solution respectively, and inject gas chromatograph, examinesSurvey.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105535271A (en) * | 2016-02-10 | 2016-05-04 | 陈武 | Girald daphne bark tablets for treating scapulohumeral periarthritis and nursing auxiliary medicine thereof for treating epilepsy |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094627A (en) * | 1993-05-03 | 1994-11-09 | 周惠仁 | Giraldi daphne tablet and preparation method thereof |
| CN1362199A (en) * | 2001-01-02 | 2002-08-07 | 杨孟君 | Nano girald daphne medicine and its preparation |
| CN105535271A (en) * | 2016-02-10 | 2016-05-04 | 陈武 | Girald daphne bark tablets for treating scapulohumeral periarthritis and nursing auxiliary medicine thereof for treating epilepsy |
-
2016
- 2016-02-10 CN CN201610083482.0A patent/CN105596559A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094627A (en) * | 1993-05-03 | 1994-11-09 | 周惠仁 | Giraldi daphne tablet and preparation method thereof |
| CN1362199A (en) * | 2001-01-02 | 2002-08-07 | 杨孟君 | Nano girald daphne medicine and its preparation |
| CN105535271A (en) * | 2016-02-10 | 2016-05-04 | 陈武 | Girald daphne bark tablets for treating scapulohumeral periarthritis and nursing auxiliary medicine thereof for treating epilepsy |
Non-Patent Citations (1)
| Title |
|---|
| 国家药典委员会编: "《中华人民共和国药典：2010年版.一部》", 31 January 2010, 中国医药科技出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105535271A (en) * | 2016-02-10 | 2016-05-04 | 陈武 | Girald daphne bark tablets for treating scapulohumeral periarthritis and nursing auxiliary medicine thereof for treating epilepsy |
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