Sorbent silica

 

(57) Abstract:

The invention relates to adsorbents for affinity chromatography and allows, for example, to carry out the separation of glycated hemoglobin from negociating. Proposed sorbent silica containing grafted group m-aminophenylarsonic acid number of 80 to 110 mmol per 1 g of sorbent.

The invention relates to adsorbents for affinity chromatography and can be used in chemistry, biochemistry, medicine, in particular for the chromatographic separation of glycated proteins from negociating proteins.

Known sorbents on the basis of agarose derivatives aminophenylarsonic acid used for separation of glycated hemoglobin.

Also known sorbent containing a polymer matrix, a modified aminophenylarsonic acid and has the structural formula

_O-CH2--CH2-O-(CH2)4-O-CH2-

As disadvantages of these sorbents should note the change in volume of the sorbent with the composition of the eluent, the compressibility of the sorbent when the pressure increases, microbiological instability. This makes it impossible to use this type of sorbents for RMS is based on silica, containing grafted group aminophenylarsonic acid with the following structural formula

SiOi(CH2)3-NH-

and used for affinity chromatography of sugars.

The disadvantage of this sorbent is the presence of hydrophobic ligaments, which leads to nonspecific adsorption of proteins and the unsuitability of its use for analysis, such as glycated hemoglobin.

The objective of the invention is to provide a sorbent silica for separation of glycated hemoglobin with high grafting density modifier affine hydrophilic groups, which provides effective shielding of the surface source of silica and increases the separation ability and capacity of the sorbent with respect to glycated hemoglobin.

The problem is solved described sorbent silica containing grafted group m-aminophenylarsonic acid and has the structural formula

-O-Si(CH2)3-O-CH2--CH2-NH-

This sorbent can be obtained by treatment of silica-glycidoxypropyltrimethoxysilane, then m-aminophenylarsonic acid and subsequent washing buffer solution and wodoodporne with a specific surface area of 250 m2/g and an average pore diameter of 100-500 .

The capacity of the obtained sorbent is 80-100 µmol m-aminophenylarsonic acid per 1 g of sorbent.

P R I m e R 1. A. Obtaining sorbent.

The original silica CSC-2 (130 , 250 m2/g) particle size 100-160 μm. To 10 g of the source of silica was added 100 ml of a 5% solution of glycidoxypropyltrimethoxysilane in 0.01 M Na-acetate buffer at pH 5.4 and heated on a water bath for 3 hours, the Product is washed with water, acetone, water, and buffer 0.5 M NaHCO3, 0.5 M NaCl, pH 8, 50 ml each.

1 g of the modified silica is treated with a solution containing 0.15 g m-aminophenylarsonic acid in 5 ml of 0.1 M NaHCO+0.5 M NaCl (pH 8.0) at room temperature for 20 hours in a nitrogen atmosphere at a light mechanical shaking. After that, the sorbent is washed with the same buffer solution, and then 0.5 M NaHCO3water and leave for 12 h with 5 ml of 1M solution of monoethanolamine (pH=9,0). Then the sorbent is washed with water, place the column (0,3x3,6 cm) and uranovaia buffer with a pH of 8.5 (0.25 M ammonium acetate, 0.05 M MgCl2). The resulting sorbent based on SiO2formula:

-O-Si(CH2)3-OCH2--CH2-NH-

containing 80 µmol vaccinated groups per 1 g of sorbent.

B. When the column the quantitative determination of glycated hemoglobin in the blood.

Blood samples taken in tubes containing EDTA, separate the plasma and leukocytes, conduct hemolysis water. 100 μl of the obtained hemolysate applied on the column with sorbent balanced buffer solution pH 8.5. The column was washed with 6 ml of equilibrated buffer, unbound fraction is taken in a test tube and diluted with water. Associated with the sorbent hemoglobin elute 3 ml of 0.2 M sorbitol, the eluate is also diluted with water. Measure the optical density of the obtained solutions at 414 nm and calculate the content of glycated hemoglobin according to the formula: HbGlick< / BR>
Held on 25 re-definitions of glycated hemoglobin in a single column and a variation coefficient of 0.96%

Thus, it is possible at least 25-fold using columns with sorbent, while similar known sorbents guarantee a 10-fold reproduction of results.

P R I m m e R 2. The synthesis of the sorbent similar to that described in example 1, but the particle size of the silica gel was 10 μm.

It is determined that the capacity of the sorbent was 110 μmol of active groups per 1 g of sorbent.

Testing of the sorbent, obtained according to example 2. The sorbent is placed in a column of steel h mm

tx2">

Buffer B: 0.25 M Gly-Gly, 0-05M MgCl2, 0.2 M sorbitol, pH 7.5.

The analysis time of 2 min, the rate of 1.25 ml/min:

0-0,95 min 100% AND

0,95-1.55V min 100% B

Rinse the 1.6-5 min 100% A.

It was shown that the sorbent is not less than 500 entries.

P R I m e R 3. the synthesis of the sorbent according to the method described in example 1, but using silochrome C-80 (80 m2/g, 500 , particle size 100-160 μm). The analysis showed that the obtained sorbent composition:

-O-i(CH2)3-OCH-CH2-NH-

containing 100 μmol of active groups per 1 g of sorbent.

Tests of the obtained sorbent is carried out as in example 2, and shows similar results.

Thus, the obtained sorbent, having a high capacity and separation ability allows the analysis mode high-performance liquid chromatography with carrying out not less than 500 tests on a single column.

SORBENT SILICA containing grafted group m-aminophenylarsonic acid, characterized in that it has the structural formula



 

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