CN102786418B - Chlorogenic acid brilliant II type sign and preparation method and apply in medicine and health products - Google Patents
Chlorogenic acid brilliant II type sign and preparation method and apply in medicine and health products Download PDFInfo
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- CN102786418B CN102786418B CN201110128518.XA CN201110128518A CN102786418B CN 102786418 B CN102786418 B CN 102786418B CN 201110128518 A CN201110128518 A CN 201110128518A CN 102786418 B CN102786418 B CN 102786418B
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Abstract
The invention discloses the brilliant II type of the one state of matter of the chlorogenic acid shown in formula (I); The preparation method of the brilliant II type of chlorogenic acid sample; Product using the brilliant II type of chlorogenic acid material as active fraction preparation, described product comprises medicine and health products, and application in chlorogenic acid brilliant II type disease preventing and treating and health care.
Description
Technical field
The present invention relates to a kind of brilliant II type state of matter of chlorogenic acid, the preparation method of the brilliant II type of chlorogenic acid sample, adopts chlorogenic acid crystalline substanceII type material is as the product of active component, and the purposes of the brilliant II type of chlorogenic acid, belongs to medical technical field.
Background technology
Chlorogenic acid, English Chlorogenicacid by name, molecular structure is suc as formula shown in (I)
In Chinese patent CN1181042C (publication number), record " the carrying of Chlorogenic Acid of Flos Lonicerae of people's inventions such as Han LujiaGet purification process "[1]. Wherein, relate to a kind of method for extraction and purification of Chinese herbal medicine functional components, become by honeysuckle coarse crushingSegment, extracts in the best condition, and through preliminary removal of impurities and repurity, method is simple, Yi Hang, and the loss of chlorogenic acid is few, productRecovery rate and purity are all very high.
In Chinese patent CN1168698C (publication number), record " the macroporous resin adsorption extraction high-load of Liu Bin inventionThe process of chlorogenic acid "[2]. Wherein, having related to one is extracted and macroreticular resin by honeysuckle pulverizing, chlorogenic acid aqueous extractThe separating technology of absorption chlorogenic acid in high content, this law has that technique is simple, cost is low, easy to operate, produce finished product chlorogenic acid contentHigh, there is the outstanding advantages such as distinct economic.
In Chinese patent CN1435406A (publication number), record " a kind of side of preparing chlorogenic acid of people's inventions such as Liu ShimingMethod "[3]. Wherein, relate to a kind of method of preparing chlorogenic acid, belonged to a kind of extracting method of plants ' medicinal component, for green formerAcid is produced and has been searched out a kind of burdock leaf source new drugs, has reduced the production cost of chlorogenic acid, and simple to operate.
In Chinese patent CN1568960A (publication number), record " high purity chlorogenic acid prescription " of the inventions such as Zhang Jie[4]。Wherein, having related to a kind of high-purity chlorogenic acid is that raw material is prepared into the medicine that pharmaceutically can be applicable to clinical various formulations, and existingHave these Chinese patent drugs to compare, can give full play on the one hand the pharmacological effect of chlorogenic acid, the purity of chlorogenic acid and content are high on the other hand,Easily operation of the formulation of quality index and inspection.
In Chinese patent CN1616402A (publication number), record " the side that a kind of chlorogenic acid extraction separates of Tang Huazhao inventionMethod "[5]. Wherein, relate to a kind of chlorogenic acid and extracted the method separating, particularly from Folium Eucommiae, acer truncatum leaf, extract,Separate, the method for purifying chlorogenic acid, comprise the steps such as extraction, resin adsorption, extraction, dry, crystallization. The present invention withPrior art comparison, has the advantages such as technique is simple, production cost is low, good product quality, benefit height, product purity 95% withUpper, the present invention has passed through industrial test.
In Chinese patent CN100494393C (publication number), record " the high-purity chlorogenic acid of the people such as Zhang Jie, Zhang Liang inventionIndustrialized producing technology "[6]. Wherein, having related to the technique that a kind of high purity chlorogenic acid in industrialization scale is produced, is to add in techniqueBiological complex enzyme improve the dissolution rate of chlorogenic acid and reduction solvent protection chlorogenic acid molecular radical to avoid oxidized technology be high-purityThe important breakthrough that chlorogenic acid is produced, has solved contained phenolic hydroxyl group oxidation, the olefin(e) acid ester linkage hydrolyzing of commercial process Content of Chlorogenic AcidMolecule lactone group is moved and generation Heterogeneity in succession.
In Chinese patent CN101133015A (publication number), record " the chlorogenic acid composition of the prosperous great invention such as the people of grade in FeitianManufacture method "[7]. Wherein, relate to one and obtained containing chlorogenic acid with high concentration with high yield, and caffeine minimizingThe method of chlorogenic acid composition, is characterized in that making the water-soluble composition from fresh coffee beans or roasted coffee beans extraction to be adsorbed onBe filled with in the post of adsorbent, then make the logical liquid of ethanol water of 0.5～20vol%, to carry out wash-out.
In Chinese patent CN101293832A (publication number), recorded people's inventions such as Zhao Yu " chlorogenic acid and derivative thereofSynthetic method "[8]. Wherein, relate to the synthetic method of a kind of chlorogenic acid and derivative thereof, with traditional chloride method preparation methodCompare, this method is simple to operate, and reactions steps is short, and post processing is simple, and productive rate is better.
In Chinese patent CN101302156A (publication number), record " a kind of Eupatorium adenophorum medium green of people's inventions such as Cao's col journeyThe extraction process of ortho acid "[9]. Wherein, related to a kind of extraction process of Eupatorium adenophorum Content of Chlorogenic Acid, the method makes up with gold and silverThe deficiency of resource-constrained when flower is raw material chlorogenic acid extracting, can also be in changing harmful to treasure Eupatorium adenophorum, and high productivity obtainsObtain chlorogenic acid, and method is simple, with low cost, be suitable for suitability for industrialized production.
In Chinese patent CN101314568A (publication number), record " a kind of adsorption separation of high purity of the inventions such as Lu DingqiangThe new method of chlorogenic acid "[10]. Wherein, related to a kind of new method of adsorption separation of high purity chlorogenic acid, comprise adsorption process,Wash assorted process, elution process, can be widely used in food, medicine, in the fields such as cosmetics. The chlorogenic acid that this method makes is pureThe solid that solution convection drying obtains, dry chlorogenic acid powder can directly be applied without reprocessing, is convenient to transport.
In Chinese patent CN101324546A (publication number), recorded people's inventions such as Li Xifeng " HPLC method is measured simultaneouslyThe method of dandelion preparation Content of Chlorogenic Acid, caffeic acid content "[11]. Wherein, relate to a kind of HPLC method and measured dandelion simultaneouslyThe method of preparation Content of Chlorogenic Acid, caffeic acid content, can effectively solve using chlorogenic acid and caffeic acid as index composition, enters simultaneouslyRow assay, to the quality standard of dandelion preparation lay the foundation solve problem.
In Chinese patent CN101367729A (publication number), record " a kind of complexometric extraction of the invention such as Lu Dingqiang, Wang JunThe method of purification chlorogenic acid "[12]. Wherein, relate to a kind of method of utilizing Complexation Extraction Technique purification chlorogenic acid, can be suitable forIn low concentration plant extraction liquid, complexometric extraction chlorogenic acid separating technology can reduce production costs, and reduces organic solvent residual, slowThe pollution of separating environment, meets the requirement of green chemistry process.
In Chinese patent CN101445456A (publication number), recorded " extracting and divide of the inventions such as Chen Yuru from goldenrodFrom the method for chlorogenic acid "[13]. Wherein, relate to a kind of method of goldenrod chlorogenic acid extracting, can improve obtaining of chlorogenic acidRate, shortens the production cycle, obtains chlorogenic acid sterling instead of the mixture with other compositions, from goldenrod chlorogenic acid extracting listBody, can expand the raw material sources of chlorogenic acid; Particularly can turn waste into wealth to the exploitation of Solidago Canadensis, turn harm into good,There are good economic benefit, social benefit and environmental benefit.
That in Chinese patent CN101486651A (publication number), has recorded the inventions such as Zhang Dongsheng " extracts green in a kind of folium cortex eucommiaeThe method of ortho acid and application thereof "[14]. Wherein, relate to a kind of method of extracting chlorogenic acid from Eucommia leaves, the invention also disclosesThe application of chlorogenic acid in fish disease prevention and cure thing, method has that technological operation is easy, cost is low, high without hazardous solvent, yield,Be applicable to the advantages such as suitability for industrialized production, and chlorogenic acid has good fungistatic effect to pathogen common in aquaculture, rightThe fungistatic effect of Aeromonas hydrophila is suitable with antibiotics antibacterials, can strengthen immunity of organisms, to bacteriosis toolThere is stronger prevention effect.
In Chinese patent CN101503356A (publication number), recorded the people such as Lu Dingqiang, Zhao Hui invention " one is prepared heightThe new method of purity chlorogenic acid "[15]. Wherein, related to a kind of new method of preparing high-purity chlorogenic acid, applicable to low concentrationChlorogenic acid stoste, quantity of sample handling is large, simple to operate, can reduce production costs, and reduces organic solvent residual, alleviates environmentPollution.
In Chinese patent CN101503357A (publication number), recorded people's inventions such as Su little Fei " Chlorogenic Acid of Flos LoniceraeExtracting process "[16]. Wherein, relate to a kind of extracting process of Chlorogenic Acid of Flos Lonicerae, solved current chlorogenic acid extract and existedThe filtration difficulty causing greatly because of precipitation capacity in impurity elimination purge process, purity and the yield of raising product; And extracting honeysuckleWhen chlorogenic acid, produce the product that a series of added values are higher, better utilize the raw material resources of honeysuckle.
In Chinese patent CN101613278A (publication number), record " one Quick from sweet potato leaves of Li Guangfeng inventionGet the industrial technology of high-purity chlorogenic acid "[17]. Wherein, related to a kind of from sweet potato leaves the production method of chlorogenic acid extracting, mainWanting feature is that raw material does not need dry directly use, hydrochloric acid solution lixiviate, and energy consumption is little, and organic solvent uses few, Environmental Safety,Production cost is low, and yield is high.
In Chinese patent CN101618016A (publication number), having recorded Huabao Edible Essence & Condiment (Shanghai) sends outBright " a kind of preparation method, its product and purposes of W/O/W type emulsion of embedding chlorogenic acid "[18]. Wherein, related to oneThe W/O/W type emulsion preparation method who plants embedding chlorogenic acid, this preparation method carries out embedding to chlorogenic acid, can not only be to chlorogenic acidPlay protection, storage effect, can also realize chlorogenic acid in human body evenly, effectively discharge, meanwhile, sorbefacient slowly-releasing,Controlled release and Targeting Effect, give full play to its effect.
In Chinese patent CN101638366A (publication number), record " a kind of microwave auxiliary reflux of people's inventions such as He RonghaiExtract the method for chlorogenic acid of sunflower seed dregs "[19]. Wherein, related to a kind of extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary refluxMethod, leaching process microwave can continuous action, extraction time is short, efficiency is high, solvent load is few, product Content of Chlorogenic Acid yield1.54 times to 2.39 times of traditional ethonal extraction method.
That in Chinese patent CN101674821A (publication number), has recorded this grade of M.J. Allan people invention " uses Quercetin, poplarThe composition of plum flavones and chlorogenic acid treatment diabetes and metabolic disease "[20]. Wherein, related to one provide be used for the treatment of rightThe diabetes of elephant and metabolic disease and the composition losing weight for realizing object, described composition comprises Quercetin, red bayberry HuangKetone and chlorogenic acid, comprise the combination of the compound of natural generation.
In Chinese patent CN101704748A (publication number), record " a kind of extraction of chlorogenic acid of people's inventions such as Liu DongfengMethod "[21]. Wherein, related to a kind of cost low, output is large, and the cycle is short, is easy to realize industrialized separating-purifying chlorogenic acidMethod. Processing step comprises squeezing, macroporous resin adsorption, film is concentrated, spraying is dry. Adopt the present invention to produce chlorogenic acid,Technique is simple, energy resource consumption is few, very high purity.
There is essential difference in the present invention and above-mentioned patent or document, above-mentioned patent is all from Therapy effect, from different plantsMiddle extraction and purification preparation method, point of penetration of the present invention be to start with from chlorogenic acid solid chemical material existence research, pass throughScreening polymorph technical research, the novel crystal forms kind of searching in the raw material aspect of active constituents of medicine, discovery chlorogenic acid solid matterClass and status flag, and crystal formation research is combined with clinical and healthcare applications, have optimal efficacy for finding, find, developingChlorogenic acid state provides basic scientific research data; Meanwhile, be also from chlorogenic acid solid crystal formation raw material basis application countryOr international intellectual property invention patent protection provides scientific basis.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of new crystal formation of the chlorogenic acid shown in formula (I), i.e. brilliant II type
Another technical problem that the present invention will solve is to provide the preparation method of the brilliant II type of chlorogenic acid material.
Another technical problem that the present invention will solve is to provide the product of the brilliant II type of chlorogenic acid composition as active component.
Another technical problem that the present invention will solve is to provide the application of the brilliant II type of chlorogenic acid.
Particularly, be the technical problem solving, adopt following technical scheme:
1. the brilliant II type of chlorogenic acid sample morphological feature:
The brilliant II type of 1.1 chlorogenic acids material, (CuK in the time using powder x-ray diffraction analysisαRadiation), show as Height%=100 peak positions in 2-Theta=26.0 ± 0.2 ° orLocating and have 40 its positions of diffraction maximum exists respectively2-Theta (°) ± 0.2 ° value orValue has following expression:
And diffraction maximum relative intensity value allows Height% ± 10% excursion (Fig. 1).
The brilliant II type of 1.2 chlorogenic acids solid matters, its infrared absorption spectroscopy (Fig. 2) 3621,3355,3059,2953,2635,1869、1725、1706、1686、1639、1612、1601、1528、1516、1442、1381、1322、1304、1289、1251、1221、1189、1158、1133、1113、1085、1038、1001、977、969、936、909、889、864、852、817、767、739、713、676、602、563、513、457、423cm-1±2cm-1Absworption peak be chlorogenic acidThe diffuse reflectance infrared spectroscopy peak position that brilliant II type solid matter presents.
The brilliant II type of 1.3 chlorogenic acids solid matter, contains a Peak endothermic peak in its DSC collection of illustrative plates (Fig. 3), and transformation value exists212 DEG C ± 3 DEG C positions.
The brilliant II type of 1.4 chlorogenic acids solid matter, its melting point values is 205 DEG C ± 2 DEG C.
2. the preparation method characteristic of the brilliant II type of chlorogenic acid sample:
2.1 the invention provides the preparation method of the brilliant II type of a kind of chlorogenic acid sample, it is characterized in that using acetone, methyl alcohol, 95% secondThe single solvent of alcohol, isopropyl alcohol, normal propyl alcohol, oxolane, DMF, DMSO, pyridine is under 15 DEG C～80 DEG C temperature conditionsChlorogenic acid sample is dissolved completely and through 10 DEG C～80 DEG C of environment temperatures, ambient humidity 10%～75%, normal pressure or vacuum pressure barPart prepares the brilliant II type of chlorogenic acid sample.
2.2 the invention provides the preparation method of the brilliant II type of another kind of chlorogenic acid sample, it is characterized in that using acetone, methyl alcohol, 95%Ethanol, isopropyl alcohol, normal propyl alcohol, oxolane, DMF, DMSO, pyridine arbitrarily two or more solvent are joined by differenceThe system that is compared to is dissolved chlorogenic acid sample completely and through 4 DEG C～80 DEG C of environment temperatures, ambient humidity at 15 DEG C～80 DEG C temperature10%～75%, the recrystallization preparation technology under normal pressure or vacuum experiment condition obtains the brilliant II type of chlorogenic acid solid matter.
3. the brilliant II type of chlorogenic acid is as using dosage and the purposes feature of active material:
3.1 of the present inventionly also provide a kind of product, using the brilliant II type of chlorogenic acid composition as active component and contain other auxiliary materials. ThisBright described product, comprises medicine, health products.
The crystal formation purity of the described brilliant II type of product Content of Chlorogenic Acid is 1%～100%.
The formulation of described product is selected from tablet, capsule, pill, injection, slowly-releasing or controlled release agent, pulvis.
3.2 the invention provides the various product of the brilliant II type of chlorogenic acid material as active component exploitation, comprise medicine, health products,It is characterized in that its every daily ingestion dosage is in 1mg～30g scope using the brilliant II type of chlorogenic acid material as active component.
3.3 the invention provides the various product of the brilliant II type of chlorogenic acid material as active component exploitation, comprise medicine, health products,It is characterized in that using and contained the brilliant II type of chlorogenic acid material and ensured its Absorption Characteristics in vivo, effectively as active componentBioavilability, effective blood drug concentration, stablize the lasting time and reach the prevention of making the most of the advantage, treatment, health-care effect and shouldWith.
4. the Absorption Characteristics of the brilliant II type of chlorogenic acid sample after oral:
The invention provides the product of the brilliant II type of chlorogenic acid material as active component exploitation, comprise medicine and health products, oral administrationAfter biology absorption, it is characterized in that the brilliant II type of chlorogenic acid material as active component by intestines and stomach after 0.5 hourIn blood, can reach Cmax value and play a role. After accompanying drawing 4 provides the brilliant II type of chlorogenic acid sample oral administration and absorbs ratPlasma concentration curve in body.
5. the application of the brilliant II type of chlorogenic acid in pharmacy.
The brilliant II type of the chlorogenic acid that the invention provides is antibacterial, antiviral in preparation, increase white blood cell, hepatic cholagogic, antitumor,Hypotensive, reducing blood lipid, anti-oxidant, remove free radical, stimulating central nervous system system, increase gastrointestinal peristalsis or promote gastric secretionMedicine in application.
The present invention also provides the application of the brilliant II type of chlorogenic acid in the medicine of preparing preventing and curing of fish disease.
Brief description of the drawings
The x-ray diffractogram of powder spectrum of the brilliant II type of Fig. 1 chlorogenic acid sample
The infrared absorpting light spectra of the brilliant II type of Fig. 2 chlorogenic acid sample
The DSC collection of illustrative plates of the brilliant II type of Fig. 3 chlorogenic acid sample
Plasma concentration curve after the brilliant II type of Fig. 4 chlorogenic acid sample oral administration absorbs in rat body
Detailed description of the invention
For better explanation technical scheme of the present invention, spy provides following examples, but the present invention is not limited to this.
Embodiment 1
The preparation method of the brilliant II type of chlorogenic acid sample:
The preparation method of the brilliant II type of chlorogenic acid sample, it is characterized in that using 10ml methyl alcohol as solvent under normal temperature condition by chlorogenic acid1g sample dissolves completely, removes solvent at the constant pressure and dries of 40 DEG C, prepares chlorogenic acid crystal form samples.
The x-ray diffractogram of powder of gained chlorogenic acid crystal form samples is composed as shown in Figure 1
The infrared absorpting light spectra of gained chlorogenic acid crystal form samples as shown in Figure 2
The DSC collection of illustrative plates of gained chlorogenic acid crystal form samples as shown in Figure 3
Above spectrum data result shows, the crystal formation of the present embodiment gained crystal is the brilliant II type of chlorogenic acid.
Embodiment 2
The preparation method of the brilliant II type of chlorogenic acid sample:
The preparation method of brilliant II type chlorogenic acid sample, is characterized in that first adding 45ml cyclohexane mixed solvent at 30 DEG C with 15ml acetoneAfter chlorogenic acid 1g sample being dissolved completely under water bath condition, go down to desolventize at the vacuum condition of 40 DEG C of temperature, prepare greenOrtho acid crystal form samples.
The x-ray diffractogram of powder of gained chlorogenic acid crystal form samples is composed as shown in Figure 1
The infrared absorpting light spectra of gained chlorogenic acid crystal form samples as shown in Figure 2
The DSC collection of illustrative plates of gained chlorogenic acid crystal form samples as shown in Figure 3
Above spectrum data result shows, the crystal formation of the present embodiment gained crystal is the brilliant II type of chlorogenic acid.
Need the problem of explanation: because the single organic solvent for the preparation of the brilliant II type of chlorogenic acid sample is total multiple, can be forPreparing two kinds of the brilliant II type of chlorogenic acid sample or above solvent combination has tens of kinds, every kind of organic solvent boiling point value difference, to greenOrtho acid sample dissolution different in kind, causes at the environment that uses its experiment while preparing the brilliant II type of chlorogenic acid sample under different solvents conditionThe variate-values such as temperature, humidity, time, pressure all there is some difference property and constant interval scope.
Embodiment 3
The brilliant II type sample of chlorogenic acid Absorption Characteristics and blood concentration feature in rat body:
Animal used as test: SD rat, male, body weight: 300g. Be purchased from animal used as test institute of the Chinese Academy of Medical Sciences.
Experimental technique: the brilliant II type of chlorogenic acid sample. Be mixed with 10mg/ml suspension with 4 DEG C of Wahaha Pure Waters. Rat routineRaising condition is raised, and freely drinks water, and after fasting 12h, gives medicine by 100mg/kg gavage. After administration 0.083,0.25,0.5,1,1.5,2,3,4,6 (h) time point is got the about 0.4ml of blood from eyeball posterior vein, the centrifugal 10min of 5000rpm. Get100 μ l blood plasma, add methyl alcohol 200 μ l, vortex oscillation 2min, and the centrifugal 10min of 13400rpm, gets supernatant layer 40 μ l and carries out HPLCDetect. Detecting instrument and condition: detection system is Aligent1200 highly effective liquid phase chromatographic system, chromatographic column is AgilentZorbaxEclipseXDB-C18(250 × 4.6mm, m), mobile phase is acetonitrile: 0.05%H to 5 μ3PO4Buffer solution=17: 83, sample sizeBe 40 μ l, flow velocity is 1ml/min, and detection wavelength is 328nm, and column temperature is 25 DEG C. Testing result sees the following form and Fig. 4.
The brilliant II type of chlorogenic acid sample blood concentration data
Experimental result shows: the brilliant II type chemistry of chlorogenic acid solid matter can be absorbed by rat, it is characterized in that the brilliant II type of chlorogenic acid solidAfter the administration of medicine oral administration, can be absorbed, after 0.5 hour, can reach maximum plasma concentration, can be in the time of 1.5h again through liver sausage circulationThe inferior maximum plasma concentration that occurs. The brilliant II type of chlorogenic acid material has ensured its Absorption Characteristics in vivo, has had as active componentEffect bioavilability, effective blood drug concentration, stablize the lasting time and reach the prevention of making the most of the advantage, treatment, health-care effect andApplication.
Embodiment 4
The brilliant II type of chlorogenic acid material is as the medicine dosage of active component:
The medicinal tablet or other preparations that use the brilliant II type of chlorogenic acid sample to manufacture as active constituents of medicine, is characterized in that containingHave the active component of the brilliant II type of chlorogenic acid as medicine, every day, dosage was 300mg, can be prepared into respectively every day 3 times/each1 100mg conventional tablet, every day 2 times/each 1 150mg conventional tablet or every day 1 time/each 1 300mg sheetAgent type.
Need the problem of explanation: the brilliant II type of the chlorogenic acid pharmaceutical composition the present invention relates to exists on the dosage of active ingredientThere is perhaps multifactor impact, for example: cause the difference of dosage every day for preventing different with the purposes for the treatment of; Ill characterDifferent from the ill order of severity and cause the different of dosage every day; The difference of Gender, age, body surface area, administrationApproach, administration number of times, therapeutic purposes are different and cause the difference of dosage every day; In addition the absorption existing between crystal form samples,Not equal with blood concentration, also cause the present invention be 0.01 in suitable dose scope every day that uses the brilliant II type of chlorogenic acid composition～200mg/kg body weight, is preferably 1～100mg/kg body weight. Should be according to actual prevention and treatment different situations demand system when useDetermine the brilliant II type of chlorogenic acid active ingredient accumulated dose scheme, and can be divided into repeatedly or single administration mode completes.
Embodiment 5
The brilliant II type of chlorogenic acid material is as the health products dosage of active component:
Use the functional health product of the brilliant II type of chlorogenic acid material as active fraction preparation exploitation, it is characterized in that containing in health productsThe brilliant II type of chlorogenic acid is as health active component substances, and its consumption is from 1mg30g.
Bibliography
1. Chinese patent, publication number CN1181042C.
2. Chinese patent, publication number CN1168698C.
3. Chinese patent, publication number CN1435406A.
4. Chinese patent, publication number CN1568960A.
5. Chinese patent, publication number CN1616402A.
6. Chinese patent, publication number CN100494393C.
7. Chinese patent, publication number CN101133015A.
8. Chinese patent, publication number CN101293832A.
9. Chinese patent, publication number CN101302156A.
10. Chinese patent, publication number CN101314568A.
11. Chinese patents, publication number CN101324546A.
12. Chinese patents, publication number CN101367729A.
13. Chinese patents, publication number CN101445456A.
14. Chinese patents, publication number CN101486651A.
15. Chinese patents, publication number CN101503356A.
16. Chinese patents, publication number CN101503357A.
17. Chinese patents, publication number CN101613278A.
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Claims (8)
1. the brilliant II type of the chlorogenic acid shown in formula (I),
It is characterized in that, when using powder x-ray diffraction analysis and adopting CuKαWhen radiation, show as Height%=100 peakPosition in 2-Theta=26.0 ± 0.2 ° orLocate and have 40 its positions of diffraction maximum respectively at 2-Theta(°) ± 0.2 ° value orValue has following expression:
And diffraction maximum relative intensity value allows Height% ± 10% excursion.
2. the each method of system of the brilliant II type of chlorogenic acid sample as described in claim 1, is characterized in that, use acetone,The single solvent of methyl alcohol, 95% ethanol, isopropyl alcohol, normal propyl alcohol, oxolane, DMF, DMSO, pyridine is at 15 DEG C～80 DEG CUnder temperature conditions, chlorogenic acid sample is dissolved completely and through 10 DEG C～80 DEG C of environment temperatures, ambient humidity 10%～75%, normal pressure orVacuum pressure condition prepares the brilliant II type of chlorogenic acid sample.
3. a preparation method for the brilliant II type of chlorogenic acid sample described in claim 1, is characterized in that, uses acetone, firstAlcohol, 95% ethanol, isopropyl alcohol, normal propyl alcohol, oxolane, DMF, DMSO, any two or more solvents of pyridine are by differentProportioning is dissolved chlorogenic acid sample completely at 15 DEG C～80 DEG C temperature as system and is wet through 4 DEG C～80 DEG C of environment temperatures, environmentRecrystallization preparation technology under degree 10%～75%, normal pressure or vacuum experiment condition obtains the brilliant II type of chlorogenic acid solid matter.
4. a product, is characterized in that, using the brilliant II type of chlorogenic acid claimed in claim 1 composition as active component, and containsThere are other auxiliary materials.
5. according to the product of claim 4, it is characterized in that, described product is selected from medicine, health products.
6. according to the product of any one in claim 4-5, the formulation of described product be selected from tablet, capsule, pill, slowly-releasing orControlled release agent, pulvis.
The brilliant II type of the chlorogenic acid of claim 1 antibacterial, antiviral in preparation, increase white blood cell, hepatic cholagogic, antitumor,Hypotensive, reducing blood lipid, anti-oxidant, remove free radical, stimulating central nervous system system, increase gastrointestinal peristalsis or promote gastric secretionMedicine in application.
8. the application of the brilliant II type of the chlorogenic acid of claim 1 in the medicine of preparing preventing and curing of fish disease.
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| CN103951562B (en) * | 2014-05-09 | 2016-04-20 | 四川九章生物化工科技发展有限公司 | A kind of chlorogenic acid crystal formation and preparation method thereof |
| CN104003884A (en) * | 2014-05-30 | 2014-08-27 | 北京健坤和医药科技有限公司 | IV-type crystal of chlorogenic acid as well as preparation method and application of IV-type crystal in pharmaceutical composition or health product |
| SG11202000997YA (en) * | 2017-08-31 | 2020-03-30 | Daiichi Sankyo Co Ltd | Improved method for producing antibody-drug conjugate |
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