RU2719436C1 - Polymethylsilsesquioxane hydrogel - Google Patents

Abstract

FIELD: chemistry.SUBSTANCE: invention relates to sorbents. Disclosed is polymethylsilsesquioxane hydrogel of general formula (1), where at x = 1, y takes value from 0.1 to 0.4, z takes value from 0.001 to 0.2, n takes value from 20 to 80.(1)EFFECT: technical result is disclosed polymethylsilsesquioxane hydrogel has high sorption capacity to standard test components and to biologically active compounds, can be used for analysis of content of biologically active compounds, as well as an enterosorbent active to compounds such as cholesterol.1 cl, 1 tbl, 5 ex

Description

The present invention relates to the field of sorbents, in particular enterosorbents.

In the framework of the present invention, the use of polymethylsilsesquioxane hydrogel as a sorbent in the analysis of the content of biologically active compounds, as well as as an enterosorbent active to compounds such as cholesterol, is proposed.

In the prior art there is no data on the use of polymethylsilsesquioxane hydrogel as a sorbent in the analysis of the content of biologically active compounds and enterosorbent active to compounds such as cholesterol.

The present invention is based on the task of developing a sorbent that is active against compounds such as cholesterol, and increasing its sorption ability to such compounds.

The technical result achieved by the present invention is to provide a sorbent for sorption of cholesterol and increase its sorption ability.

The technical result is achieved using polymethylsilsesquioxane hydrogel of the General formula

where at x = 1, y takes a value from 0.1 to 0.4, z takes a value from 0.001 to 0.2, n takes a value from 20 to 80.

This polymethylsilsesesquioxane hydrogel has a high sorption capacity for standard test components such as Congo red, as well as biologically active compounds such as cholesterol. Thus, polymethylsilsesesquioxane hydrogel can be used as a sorbent in the analysis of the content of biologically active compounds and enterosorbent active to compounds such as cholesterol.

Five polymethylsilsesquioxoxane hydrogel samples were produced within the scope of the present invention.

An analysis of the composition and structure of each of the polymethylsilsesquioxane hydrogel samples was performed using high resolution solid state NMR spectroscopy. The spectra on 29Si nuclei were recorded on a Bruker Avance III 400 spectrometer (with a 9.4 T magnet) rotating at a magic angle with a frequency of 8 kHz using cross-polarization and decoupling from 1 N. The chemical shift for the MeSiO link is 0.5 (OH ) 2 is - 66 (ppm, for MeSiO (OH) - -56 ppm, for MeSiO 1.5 - -46 ppm. The quantitative composition was determined from the values of the integrated intensities of the signals of the corresponding units (x , y, z) of each sample.

Determination of cholesterol adsorption was carried out according to the following method:

5 mass. A% solution of cholesterol in isopropanol is shaken with a portion of the gel, after which the gel is filtered and washed with a 3-fold volume excess of isopropanol. The amount of sorbed cholesterol was determined by the residual cholesterol content in the mother liquor and isopropanol after washing.

The determination of Congo red adsorption was carried out according to the following procedure:

About 2.0 g (accurately weighed) of the sample was placed in a conical flask with a ground stopper with a capacity of 100 ml and 50.0 ml of Congo red solution (Kk solution) was added. The mixture is stirred for 30 minutes on a magnetic stirrer, then centrifuged and for 20 minutes at a speed of 6000 rpm. 2 ml above the precipitating liquid was placed in a 50 ml volumetric flask, the volume was adjusted with a 0.02 M sodium chloride solution to the mark and stirred. The optical density of the resulting solution was measured on a spectrophotometer at the absorption maximum at a wavelength of 492 nm in a cuvette with a layer thickness of 10 mm, using a 0.02 M sodium chloride solution as a comparison solution. At the same time, the optical density of the Congo red solution (Kk ₁ solution) is measured.

The adsorption activity (X) of the drug in micromoles per gram is calculated by the formula:

where A ₀ is the optical density of the Congo red solution (Kk ₁ solution);

A is the optical density of the Congo red solution after contact with the drug;

and ₀ - a hinge of Congo red, in g;

a - a sample of the drug, in g;

M is the molecular weight of Congo red (696.7)

1. Preparation of a 0.02 M sodium chloride solution.

1.170 g of sodium chloride is placed in a volumetric flask with a capacity of 1000 ml, dissolved in 50 ml of water, the volume of the solution is adjusted to the mark with water and stirred. The pH of the water taken to prepare the solution should be from 6.0 to 6.5. The pH of the water is adjusted with 0.1 M sodium hydroxide solution or 0.1 M hydrochloric acid solution.

2. Preparation of a solution of Congo red.

Solution Kk.

0.381 g (accurately weighed) of Congo red (TU 6-09-07-634-76) is placed in a 1000 ml volumetric flask, dissolved in 500 ml of a 0.02 M sodium chloride solution, the solution volume in the flask is adjusted to the mark with the same solvent and mix.

Solution Kk ₁ .

2 ml of Kk solution is placed in a 50 ml volumetric flask, the volume in the flask is adjusted with a 0.02 M sodium chloride solution to the mark, and stirred.

Below are the data obtained for each of the samples.

Example 1

Polymethylsilsesquioxane hydrogel of the formula

{[((CH ₃ ) SiO _1.5 ] ₁ [(CH ₃ ) SiO (OH)] _0.1 [(CH ₃ ) SiO _0.5 (OH) ₂ ] _0.001 ⋅ 72H ₂ O} _∞ , the dry residue of which is 5.4 wt. %, Congo red adsorption - 3.0 μmol / g, cholesterol adsorption - 3.2 μmol / g.

Example 2

Polymethylsilsesquioxane hydrogel of the formula

{[((CH ₃ ) SiO _1.5 ] ₁ [(CH ₃ ) SiO (OH)] _0.4 [(CH ₃ ) SiO _0.5 (OH) ₂ ] _0.02 ⋅ 70H ₂ O} _∞ , the dry residue of which is 7.1 mass. %, adsorption on Congo red - 6.4 μmol / g, adsorption on cholesterol - 5.9 μmol / g.

Example 3

Polymethylsilsesquioxane hydrogel of the formula

{[((CH ₃ ) SiO _1.5 ] ₁ [(CH ₃ ) SiO (OH)] _0.16 [(CH ₃ ) SiO _0.5 (OH) ₂ ] _0.006 ⋅ 20H ₂ O} _∞ , the dry residue of which is 18.0 mass. %, Congo red adsorption - 17.5 μmol / g, cholesterol adsorption - 16.8 μmol / g.

Example 4

Polymethylsilsesquioxane hydrogel of the formula

{[((CH ₃ ) SiO _1.5 ] ₁ [(CH ₃ ) SiO (OH)] _0.2 [(CH ₃ ) SiO _0.5 (OH) ₂ ] _0.02 ⋅ 80H ₂ O} _∞ , the dry residue of which is 5.4 wt. %, Congo red adsorption - 3.7 μmol / g, cholesterol adsorption - 4.0 μmol / g.

Example 5

Polymethylsilsesquioxane hydrogel of the formula

{[((CH ₃ ) SiO _1.5 ] ₁ [(CH ₃ ) SiO (OH)] _0.1 [(CH ₃ ) SiO _0.5 (OH) ₂ ] _0.2 ⋅ 75H ₂ O} _∞ , the dry residue of which is 6.1 mass. %, Congo red adsorption - 3.4 μmol / g, cholesterol adsorption - 3.8 μmol / g.

The results of the analysis of the composition and structure and adsorption capacity of each of the samples are shown in table 1.

As can be seen from the data presented, the obtained polymethylsilsesquioxane hydrogel is suitable for use as a sorbent in the analysis of the content of biologically active compounds and enterosorbent active to compounds such as cholesterol.

Claims (3)

Polymethylsilsesquioxane hydrogel of the general formula

where at x = 1, y takes a value from 0.1 to 0.4, z takes a value from 0.001 to 0.2, n takes a value from 20 to 80.