CN105596353A - Preparation method for direct combination of graphene oxide and triptolide - Google Patents
Preparation method for direct combination of graphene oxide and triptolide Download PDFInfo
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- CN105596353A CN105596353A CN201410601891.6A CN201410601891A CN105596353A CN 105596353 A CN105596353 A CN 105596353A CN 201410601891 A CN201410601891 A CN 201410601891A CN 105596353 A CN105596353 A CN 105596353A
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Abstract
The present invention belongs to the field of applications of graphene oxide, and discloses a preparation method for direct combination of graphene oxide and triptolide. The preparation method comprises: adding graphite powder and sodium nitrate to concentrated sulfuric acid, adding potassium permanganate or potassium dichromate, carrying out an ice bath reaction, heating to continuously carrying out the reaction, adding deionized water, adding hydrogen peroxide, carrying out suction filtration, washing with hydrochloric acid and deionized water, adding a catalyst and beta-cyclodextrin, stirring, carrying out suction filtration, washing with deionized water, placing into a vacuum environment, carrying out freeze-drying, weighing the dried product, adding deionized water, carrying out an ultrasonic treatment, adding sodium hydroxide, continuously carrying out the ultrasonic treatment, adding hydrochloric acid, adding a triptolide liquid prepared with methanol or ethanol, placing into a vacuum environment, and carrying out freeze-drying to obtain the complex of the direct combination of graphene oxide and triptolide.
Description
Technical field
The invention belongs to graphene oxide application, be specifically related to a kind of graphene oxide and thunder godvineFirst element is directly combined into the preparation method of compound.
Background technology
Graphene oxide and medicine are directly in conjunction with being a kind ofly can increase the solubility of medicine in water or fallThe method of low adverse drug reaction. Triptolide is one of main active ingredient of thunder godvine plant, be fromIsolated epoxidation diterpenic lactone in Celastraceae plant thunder godvine, triptolide is dissolved in hardlyWater, is dissolved in the organic solvents such as methyl-sulfoxide, chloroform, ethyl acetate, acetone, methyl alcohol, ethanol. ThunderPublic rattan first element has the effects such as anti-inflammatory, antitumor, immunosupress, is widely used in tumour, rheumatism jointThe treatment of the difficult and complicated illness such as inflammation, lupus erythematosus. Thunder godvine is oxidized by suppressing cyclooxygenase 2 and induction type oneThe expression of nitrogen synzyme, suppresses the generation of NO, thereby reaches inflammation-inhibiting effect. But, triptolideBelong to again the medicine that toxicity is very strong, the incidence of its clinical adverse is far above other medicines. Main generationAt digestive system, urinary system, reproductive system, cardiovascular system, marrow and hematological system, wherein digestionSystem is the most common, as: feel sick, vomiting, stomachache, diarrhoea and hemorrhage of digestive tract etc., even can cause stomachEnteron aisle ulcer, hepatic necrosis, renal damage etc.
Graphene is by the carbon atom that only has an atomic diameter thickness, and the list connecting with sp2 hydridization is formerThe two-dimentional atomic crystal that sublayer forms, it is cellular that carbon atom arrangement is. Graphene is to form other dimension carbon materialsThe elementary cell of material, it can be folded into the fullerene of zero dimension, is curled into the CNT of one dimension and is stacked toThree-dimensional graphite, its theoretic throat is only 0.35nm, is the thinnest two-dimensional material of finding at present, is alsoCurrent optimal two-dimensional nano material. Graphene oxide is the containing oxygen derivative of Graphene, its structure withGraphene is substantially identical, is just connected with in its surface the hydrophily such as great amount of hydroxy group, carbonyl oxygen-containing functional group.The existence of these oxygen-containing functional groups makes graphene oxide more easily carry out structure of modification and functionalization, compares GrapheneBe more suitable for the application of biological medicine aspect. Graphene oxide has monoatomic layer thickness, and two basal plane all canWith absorption medicine, so there is the unrivaled superelevation carrying drug ratio of other nano materials.
The object of the invention is: by triptolide and the direct combination of graphene oxide, form oxidation stoneThe compound of China ink alkene and medicine. Having higher medicine carrying amount and triptolide based on graphene oxide is combined intoCompound, is expected to reduce clinically the bad reaction of triptolide, or improves the dissolving in waterDegree.
Summary of the invention
The object of the invention is to prepare graphene oxide and triptolide and be directly combined into compoundPreparation method. Graphene oxide has very large specific area, can be by non-covalent bond effect absorption Thunder GodThereby rattan first element forms graphene oxide and triptolide compound. This compound is expected to clinically thunderPublic rattan first element is delivered to tumour target organ and plays a role, and the triptolide that reduces its hetero-organization exists, and reducesThe bad reaction of triptolide. Utilize specific area and triptolide that graphene oxide is very large straight simultaneouslyAccess node is combined into compound, by the Stability Analysis of Structures of non-covalent bond effect protection triptolide, improves thunder godvineThe solubility of first element in water.
Detailed description of the invention
Embodiment 1:
The present embodiment is the preparation method that graphene oxide and triptolide are directly combined into compound.10 grams of graphite powders and 3 grams of-8 grams of sodium nitrate are joined in the chilled concentrated sulfuric acid, slowly add permanganic acid20 grams-40 grams, potassium reacts 2 hours-5 hours in ice bath, then in 30 DEG C of-60 DEG C of water-baths, continuesStir 12 hours-24 hours, add deionized water, stir after 30 minutes, add 500 milliliter 30%Hydrogen peroxide, stirs, suction filtration, and with certain density salt acid elution, then wash by deionized water, add and urgeAgent and 1.5% beta-schardinger dextrin-1-100 milliliter, stir, and suction filtration, with deionized water washing, is put freezing dryIn dry machine, freeze drying 24 hours-48 hours under vacuum condition, obtains dry thing, takes 0.2 gram of dry thingJoin in 50 ml deionized water ultrasonic 2 hours, add after 50 milliliters of the sodium hydroxide solutions of 2mol/LContinue sonic oscillation 3 hours, add afterwards hydrochloric acid, then add the triptolide liquid of ethanol preparation, fullyVibrate 1 hour-2 hours, put in freeze drier vacuum freeze drying 24 hours-48 hours, obtain oxidationThe compound of Graphene and the direct combination of triptolide.
The compound ethanol of getting graphene oxide and the direct combination of triptolide dissolves, and then uses highSpeed centrifuge centrifugal 10 minutes with 12000rpm, using 219nm as detecting wavelength, by spectrophotometryThe absorbance of supernatant, calculates medicine carrying amount.
Embodiment 2:
The present embodiment is the preparation method that graphene oxide and triptolide are directly combined into compound.10 grams of graphite powders and 3 grams of-8 grams of sodium nitrate are joined in the chilled concentrated sulfuric acid, slowly add dichromic acid20 grams-40 grams, potassium reacts 2 hours-5 hours in ice bath, then in 30 DEG C of-60 DEG C of water-baths, continuesStir 12 hours-24 hours, add deionized water, stir after 30 minutes, add 500 milliliter 30%Hydrogen peroxide, stirs, suction filtration, and with certain density salt acid elution, then wash by deionized water, add and urgeAgent and 1.5% beta-schardinger dextrin-1-100 milliliter, stir, and suction filtration, with deionized water washing, is put freezing dryIn dry machine, freeze drying 24 hours-48 hours under vacuum condition, obtains dry thing, takes 0.2 gram of dry thingJoin in 50 ml deionized water ultrasonic 2 hours, add after 50 milliliters of the sodium hydroxide solutions of 2mol/LContinue sonic oscillation 3 hours, add afterwards hydrochloric acid, then add the triptolide liquid of methyl alcohol preparation, fullyVibrate 1 hour-2 hours, put in freeze drier vacuum freeze drying 24 hours-48 hours, obtain oxidationThe compound of Graphene and the direct combination of triptolide.
The compound methyl alcohol of getting graphene oxide and the direct combination of triptolide dissolves, and then uses highSpeed centrifuge centrifugal 10 minutes with 12000rpm, using 219nm as detecting wavelength, by spectrophotometryThe absorbance of supernatant, calculates medicine carrying amount.
Claims (1)
1. graphene oxide and triptolide are directly combined into the preparation method of compound: by 10 grams of graphite powders and 3Gram-8 grams of sodium nitrate join in the chilled concentrated sulfuric acid, slowly add potassium permanganate or potassium bichromate 20Grams-40 grams, in ice bath, react 2 hours-5 hours, then in 30 DEG C of-60 DEG C of water-baths, continue to stir12 hours-24 hours, add deionized water, stir after 30 minutes, add the dioxygen of 500 milliliter 30%Water, stirs, suction filtration, and with certain density salt acid elution, then wash by deionized water, add catalystWith 1.5% beta-schardinger dextrin-1-100 milliliter, stir, suction filtration, with deionized water washing, puts freeze drierUnder middle vacuum condition, freeze drying 24 hours-48 hours, obtains dry thing, takes 0.2 gram of dry thing and addsBy in 50 ml deionized water ultrasonic 2 hours, add 50 milliliters of the sodium hydroxide solutions of 2mol/L to continue afterwardsSonic oscillation 3 hours, adds hydrochloric acid afterwards, then adds the triptolide liquid of ethanol or methyl alcohol preparation,Fully vibration 1 hour-2 hours, puts in freeze drier vacuum freeze drying 24 hours-48 hours,The compound of graphene oxide and the direct combination of triptolide.
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| CN201410601891.6A CN105596353A (en) | 2014-10-27 | 2014-10-27 | Preparation method for direct combination of graphene oxide and triptolide |
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| CN201410601891.6A CN105596353A (en) | 2014-10-27 | 2014-10-27 | Preparation method for direct combination of graphene oxide and triptolide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108746580A (en) * | 2018-04-04 | 2018-11-06 | 北京石墨烯技术研究院有限公司 | A kind of dispersing method of graphene oxide in metal powder |
Citations (2)
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| CN101565384A (en) * | 2008-12-23 | 2009-10-28 | 南开大学 | Cyclodextrin modified monolayer graphite, supramolecular complex thereof, preparation method and application |
| CN103623419A (en) * | 2013-11-28 | 2014-03-12 | 首都医科大学 | Chlorotoxin-targeted oxidized graphene nanometer material used for transporting antitumor drug |
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2014
- 2014-10-27 CN CN201410601891.6A patent/CN105596353A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565384A (en) * | 2008-12-23 | 2009-10-28 | 南开大学 | Cyclodextrin modified monolayer graphite, supramolecular complex thereof, preparation method and application |
| CN103623419A (en) * | 2013-11-28 | 2014-03-12 | 首都医科大学 | Chlorotoxin-targeted oxidized graphene nanometer material used for transporting antitumor drug |
Non-Patent Citations (3)
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| 张雁雯等: "功能化石墨烯负载氯霉素稳定性的研究", 《中国抗生素杂志》 * |
| 方加龙等: "功能化氧化石墨烯负载氟尿嘧啶制备及体外释放研究", 《中国现代应用药学》 * |
| 苏静: "石墨烯的氧化还原法制备与表征", 《河北化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108746580A (en) * | 2018-04-04 | 2018-11-06 | 北京石墨烯技术研究院有限公司 | A kind of dispersing method of graphene oxide in metal powder |
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