The method of obtaining water-soluble derivatives of fullerenes

 

(57) Abstract:

The invention relates to organic chemistry, namely the chemistry of fullerenes. The method of obtaining water-soluble derivatives of fullerenes involves mixing pre-dissolved in an organic solvent fullerene polymer matrix in chloroform, evaporation of the mixture under vacuum to remove the solvent, dissolving the obtained complex in phosphate-buffered saline (pH 7.4 and 7.6) followed by treatment of the product by ultrasound, as a water-soluble polymer matrix used membrane Catalina that differ from other phospholipids ability to dissolve in both water and organic solvents. The technical result is an improvement of characteristics of aqueous solutions of fullerenes, manifested in the increase in stability of the suspension during storage, improved membranotropic fullerene complexes, their ability to optistruct and biotransformation in the cell. 3 C.p. f-crystals, 2 Il.

The invention relates to organic chemistry, namely the chemistry of fullerenes. The invention can be used in pharmacology and Microbiology, in particular to create a lipophilic, membrane-lakshita membranes from various chemical, physical and biological factors. This can lead to the creation of a new class of drugs.

A method of obtaining physiologically active derivatives of fullerenes having hydrophilic properties, consisting of chemical modification of fullerenes; thus conduct the reaction between phenylhydrazine and fullerenes (C60C70in the presence of triethylamine (JP N 07247273, C 01 B 31/02).

The disadvantage of this method is that the substances used for chemical modification of fullerenes, are products of organic synthesis, therefore, we can expect the occurrence of allergic reactions. On the other hand, is considerably complicated transport into the cell molecules p-methoxybenzylideneamino-1,3-diyl fullerene because of the large spatial patterns.

The closest in technical essence is a method of obtaining a water-soluble complexes of fullerenes with polyvinylpyrrolidone (10000 MM), including mixing pre-dissolved in an organic solvent is toluene fullerenes with a solution of polyvinylpyrrolidone employee polymer matrix, in chloroform, evaporation of the mixture under vacuum until complete removal is to increase the degree of dispersion of the suspension (Yoko Nakajima Yamakoshi et al. Solubilization of Fullerenes into Water with PVP Applicable to Biological Tests. J. Chem. Soc., 1994, p.517).

This method has several disadvantages, among which the toxicity of reagents used, the need for additional purification of the final products. Polyvinylpyrrolidone is a product of organic synthesis, therefore, in the framework of biological research there is a need for more Toxicological and allergological inspection.

The problem to be solved in the present invention, is to obtain complexes of fullerenes based kefallinos able to dissolve in water, which has improved performance of the process of transport of these compounds into the cell.

The technical result is an improvement of characteristics of aqueous solutions of fullerenes, manifested in the increase in stability of the suspension during storage, improved membranotropic fullerene complexes, their ability to biodegradation and biotransformation in the cell.

This object is achieved in that in the method of obtaining water-soluble derivatives of fullerenes, including mixing pre-dissolved in an organic solvent fullerene polymer matrix in chloroform, evaporation of the MCA is the development of a product by ultrasound, as the water-soluble polymer matrix used membrane Catalina that differ from other phospholipids ability to dissolve in both water and organic solvents. Catalina are natural components of the cells of humans and animals. According to the invention, dissolution of the complexes at the final stage is carried out in phosphate-buffered saline (pH of 7.4 and 7.6).

The method of obtaining water-soluble fullerenes is carried out as follows. The whole process is carried out in an insulated box in a nitrogen atmosphere. To create a nitrogen atmosphere in a hermetically sealed box blown gas within 30-50 minutes. A portion of fullerenes dissolved in benzene (density 0,879 g/cm3in the flask with a glass lid. The process was performed at room temperature, mixing (by hand) the contents of the flask until then, until complete dissolution of fullerenes. To the obtained solution of fullerenes poured chloroform, in which pre-dissolved hanging kefallinos. The contents of the flask stirred (manually). This is followed by evaporation of the mixture under vacuum for 1-3 hours.

The choice of benzene as a solvent for fullerene allows this stage the s complex. Lowering the temperature increases the duration of the process at this stage, and the probability is high that is not achieved complete removal of solvents, which will have a negative impact on the quality of the product.

The resulting complex is dissolved in phosphate-buffered saline (pH of 7.4 and 7.6). The dissolution is carried out at room temperature. The buffer is used to further use of the obtained complex of fullerenes in biological research, require strict adherence to the level of acidity of the environment. The selected interval, the pH of the medium is the norm for biological systems.

Final processing of aqueous suspensions of fullerenes spend ultrasound with a frequency of 22 kHz, the intensity of 10-60 watts/cm2within 30-60 seconds. Sonication at the last stage of the process allows to increase the degree of dispersion of the suspension, and thus extend the shelf life, which is very important for pharmaceutical preparations. Thus, the decrease of intensity of ultrasonic treatment leads to the necessity of increasing the time of exposure, therefore, additional costs of time and energy. When increasing the intensity of the sound is stoikosti suspension.

The concentration of kefallinos in the reaction mixture was determined experimentally. Decreasing this value is the salting out of fullerenes from a solution - precipitation of a black precipitate particles of fullerenes. The increase of the concentration of kefallinos (50 mg/ml) is impractical and uneconomical.

The final product is a stable suspension of brown, non-stratifying during prolonged storage (more than 14 days) at room temperature. The suspension was stored in a glass under the rubber tubes under nitrogen. Chromatographic analysis showed that in water, the complex is stable.

Obtaining water-soluble derivatives of fullerenes by mixing solutions of fullerenes (in benzene) and kefallinos (in chloroform), evaporation of the mixture under vacuum and dissolve the obtained complex in phosphate-buffered saline (pH 7.0 and 7.6) followed by sonication with a frequency of 22 kHz, the intensity of 10-60 watts/cm2within 30-60 seconds is new compared to the prototype.

The process of obtaining water-soluble derivatives of fullerenes under the above conditions allows to obtain a final product with improved characteristics of the solution, expressing the in, their ability to biodegradation and biotransformation in the cell.

To explain the method of obtaining water-soluble derivatives of fullerenes following drawings, where Fig. 1 shows an installation used for 1-4 stages of the process; Fig. 2 - installation for ultrasonic treatment.

Installation (Fig. 1) is a stand-alone box consisting of a body 1 with two holes 4. At the outer protruding edge of the holes 4 wear sleeves to ensure operation within the box. Through the nozzle 2 into the housing 1 is nitrogen from a cylinder 5. Through the fitting 3 is output displaced with nitrogen air. The cylinder 5 is provided with a gear 6 to regulate the flow of nitrogen into the housing 1.

For carrying out the process of obtaining a water-soluble derivatives of fullerenes inside of the housing 1 is placed in the flask with batches of reagents and solvents. Tightly cover the holes 4 and blow Boxing nitrogen within 30-50 minutes. After this, platitudinal process.

In the first stage, a portion of fullerenes (0.8 mg) was dissolved in 1 ml of benzene (density 0,879 g/cm3in the flask with a glass lid. The process was performed at room temperature, mixing (by hand) the contents of the flask to tellarano poured 2 ml of chloroform, in which pre-dissolved hanging kefallinos (100 mg). The contents of the flask stirred (manually). The mixture was incubated for 10-20 minutes at room temperature.

In the third stage, carry out the evaporation of the mixture under vacuum at a temperature of 40-50oC. the Duration of this stage 1-3 hours.

In the fourth stage the resulting complex is dissolved in 2 ml of phosphate-saline buffer (pH 7.0 and 7.6). The dissolution is carried out at room temperature.

At the fifth stage are treated by aqueous suspensions of fullerenes by ultrasound with a frequency of 22 kHz, the intensity of 10-60 watts/cm2within 30-60 seconds.

Installation for ultrasonic treatment (Fig. 2) consists of an ultrasonic generator 1 (USDN A) connected to the cable 2 with the ultrasonic emitter 3. Ultrasound emitter 3 sets conical nozzle 4, which is immersed in a flask with 5 suspension of fullerenes.

The processing is carried out as follows: adjusted ultrasonic generator 1 by time and intensity of ultrasonic treatment, the flask with the prepared suspension is placed a conical nozzle ultrasonic transducer 4 and include the generator 1.

Offer speof tissue repair, damaged by injury, surgery, etc.;

pharmacological application is the creation of new drugs with improved characteristics transport into the cell;

alternative use instead of liposomal technologies for drug delivery in tissue;

to create antimicrobial and antiviral drugs;

to create ways to protect cell membranes from the effects of chemical, biological and physical factors.

The proposed method can be widely applied, both in the laboratory and on an industrial scale in pharmacology for the preparation of lipophilic, membrane-biologically active compounds with improved characteristics of the process of transport of these compounds into the cell and protect membranes from various chemical, physical and biological factors.

1. The method of obtaining water-soluble derivatives of fullerenes, including mixing pre-dissolved in an organic solvent fullerene polymer matrix in chloroform, evaporation of the mixture under vacuum to remove the solvent, dissolving the obtained complex in water followed by treatment of the product of native origin - Catalina, as a solvent of fullerenes in the first stage of the process using benzene.

2. The method according to p. 1, characterized in that for the dissolution of a complex of fullerene water use of phosphate-saline buffer (pH of 7.4 and 7.6).

3. The method according to p. 1, characterized in that at the final stage of the process the solution is treated with ultrasound at a frequency of 22 kHz, the intensity of 10 - 60 W/cm2within 30 - 60 sec.

4. The method according to p. 1, characterized in that the entire process is carried out in nitrogen atmosphere.

 

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