Method for preparing calcium pectate

FIELD: medicine.

SUBSTANCE: dry powder of pectic acid or its water-soluble salt is mixed with aqueous solution of calcium salt at concentration at least 0.6 mol/l. The prepared calcium pectate is separated from aqueous phase.

EFFECT: process simplification and reduction of power inputs.

2 cl, 7 ex

 

The invention relates to methods for pectate calcium and can be used in various branches of industry and medicine, in particular the pharmaceutical industry for the manufacture of chelators.

Pectin calcium is a water-insoluble calcium salt of pectic acid. Pechova acid is a plant polysaccharide.

Pechova acid in nature is quite rare in the composition of cell walls in some plants. In industry it is usually produced by deesterification pectic acid (pectin). The basis of pectic and pectinic acid is poly-D-galacturonic acid. In pectic acid part of the residues of D-galacturonic acid is in the form of methyl esters. If the proportion of such residues is less than 50%, such pectic acid is nizkoemissionnoi. Fully deesterification, i.e. not containing methyl esters or containing a small amount of pectic acid is called pectic acid and its salts - pectates or polygalacturonate.

Pechova acid and its salts - pectates, currently considered as a promising natural sorbents, which can be widely used as therapeutic and prophylactic agents in poisoning by salts of heavy metal and radionuclide, when food and bacterial toxicosis, hepatitis and for the normalization of lipid metabolism.

Industry produces mainly soluble pectates (sodium, potassium and ammonium salts pekovich acids), which are presented on the world market in a wide range. Compared with them, the production pectate calcium minor, and it is produced mainly for technical purposes. For obvious reasons, this product quality does not meet sanitary and hygienic requirements for food and medical products. At the same time, pectin calcium as enterosorbent has a number of significant advantages over soluble pectates.

A characteristic feature of the instant pectates is their ability to form viscous solutions, so they are widely used in various industries as an effective thickeners. Solubility and zagustiteleyj properties are a serious disadvantage in those situations, when to achieve the desired therapeutic result it is necessary to introduce a large enough dose to 10-15 g/ day, and in some cases up to 45 g/day. In this regard, pectin calcium differs from other pectates the fact that he is practically insoluble in water and can be used for the reception of patients in any required quantities of the x as in dry form, and in the form of a concentrated suspension.

As pectin calcium has virtually no effect on the rheological properties of most foods, it can be included in the required amount as a dietary Supplement.

Another significant drawback of all commercially produced pectates is their characteristic flavour. Pectin calcium has no taste and does not break, so the taste of the product to which it is added.

A common shortcoming of all sorbents chelators, forming stable complexes with metal ions, is their ability to bind and excrete calcium, breaking, thus, its metabolism, which may eventually lead to serious consequences. Pectin calcium unlike other sorbents do not disturb the balance of calcium salts in the body.

Widely known method of getting pectate calcium is the method that formed the basis of quantitative determination of pectic substances in the extracts (Kertesz Z.J. The Pectic Substances. - N.Y.-L., 1951. - P.225-226).

According to this method, to 300 ml of the diluted (0,01%) solution of pectin was added 100 ml of 0.1 N NaOH solution and subjected to deesterification for several hours at room temperature.

Then to the resulting solution pectate sodium added with stirring 50 ml of 0.1 N acetic acid and 50 ml of 1 the solution of calcium chloride. The mixture is left for 1 hour to Deposit formation of pectate calcium, then boil for a few minutes and filtered through a paper filter. Sediment pectate calcium is washed with several portions of water and dried at 100C.

The disadvantage of this method is the use of aqueous solutions pectates, which are known to have a high viscosity, and therefore, efficient processing is possible only at low concentrations of polysaccharides - no more than 1-2%.

This necessitates the processing of large volumes of solutions and the use of technological equipment of the appropriate size.

Another disadvantage is that during the precipitation from aqueous solutions pectin calcium is precipitated in the form of bulk, watered gel (solids content is 0.4 to 2.0%), further squeezing and rinsing which is rather time-consuming process and requires special equipment.

It should also be noted that the pharmaceutical industry is often easier to get pectin calcium not from vegetable raw materials and pectates.

This is because in modern medicine there is a need for a wide range of calcium pectates, differing, for example, sorption properties, degree of swelling and adhesion. The range issue is by industry pectic acid and its water-soluble salts amounts to several hundreds of brands and types, varying in composition and physico-chemical properties, allowing you to get on the basis of different types of calcium pectates with different properties and in the appropriate range.

Closest to the claimed method is a method of obtaining galacturonase (galactarate) of calcium by the interaction of galacturonase sodium with calcium chloride in water (USSR Author's certificate No. 1432064, CL SW 37/04). This method differs in that, in order to intensify the process of interaction, galacturonic sodium subjected to interaction in the form of an emulsion of the aqueous solution in a hydrophobic liquid, stable 12,5% vol. Surfactants (surface active agents), and calcium chloride in the form of a microemulsion containing 4,8-5,6% vol. 40%aqueous solution of calcium chloride, about 23-24.% Surfactants and 71-72% vol. hydrophobic liquid. As the hydrophobic liquid is used alkanes composition With13-C16or mineral oil, and as a surfactant is ethoxylated fatty acid esters and sorbitol.

The method is as follows. Prepare 8 ml of 25%aqueous solution of the surfactant is a polyoxyethylene ether of synthetic fatty acids and sorbitol twin-81 and it is saturated with 0.2 ml of water. Then with stirring, add 8 ml of a 9%aqueous solution of galactarate sodium. To the resulting emulsion is added with stirring micromol the July calcium chloride, prepared with a mixture of 15.1 ml of 25%aqueous solution of tween in hexadecane and 0.9 ml of 40%aqueous solution of calcium chloride. Stirring is carried out for 10 minutes Then the system can withstand without stirring for two hours at room temperature. The entire volume of the suspension is transferred into a test tube, and the suspension was separated by centrifugation at 3000 rpm for 15 minutes and Then the suspension is washed from the oil phase with acetone or alcohol, washed with water and again with acetone or alcohol. The product is dried in a desiccator under vacuum.

The disadvantages of this method are:

a) use of water (but concentrated) solution pectate (polygalacturonate), which leads to the formation of a wet gel pectate calcium (calculated solids content of the gel is less than 9%) and is associated with additional costs dehydration and drying;

b) the use of organic solvents (oils, alkanes, acetone) and surfactant necessary to create conditions for the intensification of ion exchange between viscous polysaccharide solutions and a concentrated solution of calcium chloride;

C) a multi-stage and the technological complexity of the process.

The goal of the invention is to simplify the process of obtaining pectate calcium.

The task of resets the same time, according to the method of processing pectinesterase product is conducted in an aqueous solution of calcium salts, in accordance with the claimed invention as pectinesterase product take pochtovuyu acid or its water soluble salt, and the original pectinesterase product take dry and treated with aqueous calcium salt solution with a concentration of not less than 0.6 mol/L.

As calcium salts take calcium salts that can form a solution with a concentration of not less than 0.6 mol/l, in particular calcium chloride, calcium nitrate, calcium acetate.

The original pectinesterase products in dry form to obtain the target product prevents their dissolution, or significant swelling in the reaction due to the rapid formation of insoluble calcium salts, i.e. pectate calcium.

As pectinesterase product is recommended pochtovuyu acid or its water-soluble salts, since these compounds may conduct exchange reaction with concentrated solutions of calcium salts.

The main condition for the practical implementation of the proposed method is to create a reaction medium specific concentrations of calcium salts is high enough that the rate of ion exchange, the result of which is formed on the insoluble calcium salt of the polysaccharide, far exceeded the rate of hydration of the polysaccharide molecules, a process leading to swelling and dissolution of the granules of the powder of polysaccharide.

The minimum valid value for the concentration of calcium salts is 0.6 mol/L. When using the concentration of calcium salts below this value is too large swelling and thus increasing the volume of the granules of the powder of polysaccharide, which leads to a considerable decrease of their mechanical strength, adhesion and transformation into a homogeneous mass, difficult to further processing - washing, filtering and drying.

On the contrary, the upper limit of the concentration of calcium salts is limited only by the solubility of this salt and is, in particular, calcium chloride 4-5 mol/l under normal conditions (room temperature and atmospheric pressure). The use of more concentrated solutions obtained, for example, at elevated temperatures, it is technically possible, but impractical, as it does not lead to any appreciable improvement of the technological process and quality of product, but causes the excessive calcium salts and the need for subsequent removal of the excess water from the finished product.

In the scientific and patent documentation, the applicant discovered the essential features of the claimed invention, enabling the et to conclude that, that the claimed invention meets the criteria of patentability "novelty" and "inventive step".

The method is as follows.

Dry powder pectic acid or its water-soluble salt is mixed with an aqueous calcium salt solution, a concentration of not less than 0.6 mol/L. the Mixture was mixed thoroughly, incubated for at least 10 minutes, then the obtained pectin calcium is separated from the aqueous phase (if formed) by decantation, centrifugation or filtration. In cases where you require additional cleaning from water-soluble impurities, including the remains of salts or acids, obtained pectin calcium washed with water, then separated from the liquid phase, for example by filtration or centrifugation. The obtained wet pectin calcium is dried in the usual shelf convection dryer or dryers other designs. The output of finished pectate calcium depends on the quality of the raw materials is not less than 90% of uronic acids.

Example 1. 100 g of dry powder pectate sodium containing 68.4% of pectic acid, poured under stirring into a vessel containing 400 ml of a 2.0m solution of calcium chloride. The mixture is stirred for 10 minutes. The resulting suspension pectate calcium filtered through a nylon filter under low vacuum (0,01-0,03 MPa). Sediment pectate calcium on Phil the tre washed with 1000 ml of water to remove salts and dried in a drying Cabinet at atmospheric pressure and a temperature of 70-90C.

The yield of dry pectate calcium is 96,2, the resulting product contains 67,7% pectic acid and 8.3% calcium.

Example 2. 100 g of dry powder pectic acid containing 77.8% of net pectic acid, poured under stirring into a vessel containing 400 ml of a 2.0 M solution of calcium acetate. The mixture is stirred for 10 minutes. The resulting suspension pectate calcium treated as described in example 1.

The yield of dry pectate calcium is 105.5, the resulting product contains 72.3% of pectic acid and 8.0% calcium.

Example 3. 10 g of dry powder pectate ammonium containing 70,2% pectic acid, poured under stirring into a vessel containing 1000 ml of a 0.6 M solution of nitrate of calcium. The mixture is stirred for 10 minutes. The resulting suspension pectate calcium centrifuged for 15 minutes at 1000 g, the liquid phase is drained by decantation, the residue is suspended in 200 ml of water and re-centrifuged. The liquid phase is poured, the precipitate is re-suspended in 200 ml of water and centrifuged. The precipitate of pectate calcium is dried in a drying Cabinet at a temperature of 70-90C.

The yield of dry pectate calcium is 9,7, the resulting product contains 67,0% pectic acid and 9.5% calcium.

Example 4. To 100 g of dry powder pectate sodium containing 68.4% of pectic acid, added with constant stirring to 50 ml of a 5.0 M solution of chlorine is Yes calcium. The mixture is stirred for 10 minutes. The obtained wet powder pectate calcium is transferred on a filter, washed with 1000 ml of water and dried in a drying Cabinet at a temperature of 70-90C.

The yield of dry pectate calcium amounts to 98.6, the resulting product contains 68.2% of pectic acid and 8.0% calcium.

Example 5. To 100 g of dry powder pectate sodium containing 68.4% of pectic acid, added with constant stirring to 40 ml of a 5.0 M solution of calcium chloride. The mixture is stirred for 10 minutes. The obtained wet powder pectate calcium, without rinsing, dried in a drying Cabinet at a temperature of 70-90C.

The yield of dry pectate calcium is 122,0, the resulting product contains 56,0% pectic acid, 6,6% calcium, 19.5% of sodium chloride (formed during the exchange reaction between PECCATUM sodium and calcium chloride).

Example 6. To 100 g of dry powder pectic acid containing 77,8% polygalacturonic acid, added with constant stirring to 110 ml of a 2.0 M solution of calcium acetate. The mixture is stirred for 10 minutes. The obtained wet powder pectate calcium, without rinsing, dried in a drying Cabinet at a temperature of 70-90C.

The yield of dry pectate calcium is 109,3, the resulting product contains 62,5% polygalacturonic acid and 8.1% calcium.

Example 7. To 100 g of dry powder pectate sodium containing 68.4% of pectic acid, add constant is remesiana 20 ml of a 5.0 M solution of calcium chloride. The mixture is stirred for 10 minutes. The obtained wet powder pectate calcium, without rinsing, dried in a drying Cabinet at a temperature of 70-90C.

The yield of dry pectate calcium is 111,0, the resulting product contains 61.5% of pectic acid, 3.6% calcium, 10.5% of sodium chloride. This product contains calcium in an amount substantially smaller equivalent (approximately 50%), and when contact with water is strongly swelling, turning into a viscous gel-like mass.

The advantage of the proposed method, in comparison with the known, is that it, firstly, allows the translation of any soluble salt or acid forms of pectate in the form of its calcium salt without the use of any organic solvents using only water solutions.

Secondly, the translation pectates in the form of the calcium salt occurs without changing the state of aggregation of the polysaccharide powder particles of polysaccharide not only do not have time to dissolve, but even significantly swell, and, in General, retain their shape and sufficient rigidity. This is fundamentally important, as it allows easy enough and just spend further technological processing of the calcium salt. On the contrary, the loss of particles of polysaccharide mechanical strength contributes to their deformation, fracture, adhesion, and so the rotation in a homogeneous jelly-like mass, what complicates and makes it impossible technological operations for separation of the liquid phase, washing and drying (in conventional dryers for solids) of the obtained product.

The proposed method can also receive a partial calcium salt pekovich acids, i.e. such calcium pectates, in which the calcium content less equivalent. These compounds may be of some practical interest, for example, in medicine, due to the fact that they can absorb a lot of moisture, much to swell and form a solid gel-like layer on any surface. The receipt of such compounds in the usual way - precipitation from aqueous solutions is impractical or difficult to implement, because the resulting precipitate incomplete pectate calcium is a jelly-like amorphous structure has a weak consistency and may be partially soluble. Obtaining incomplete calcium pectates the proposed method can be implemented, for example, by mixing soluble pectates with a concentrated solution of calcium salts by the method described in example 7. This forms a moist, dense enough powder incomplete pectate calcium that can be easily dried.

In economic terms, a significant advantage of the proposed method is what I am also a high content of dry substance in their pectate calcium 22-36% and more, while svezheosazhdennoi pectin calcium obtained by traditional technology, contains only 0.4 to 2.0% of dry substance. Therefore, to obtain pectate calcium proposed method requires technological equipment is significantly smaller, which allows to compactly arrange the production, even on a small pharmaceutical company. In addition, such high solids content provides greater energy savings in the drying of the product - the most energy-consuming stage of the process.

1. The method of obtaining pectate calcium by processing pectinesterase products in an aqueous solution of calcium salts, characterized in that as pectinesterase products take pochtovuyu acid or its water soluble salt, and the original pectinesterase products take the form of a dry powder and treated with an aqueous calcium salt solution in a concentration of not less than 0.6 mol/L.

2. The method according to claim 1, characterized in that as the calcium salts take calcium salts that can form a solution with a concentration of not less than 0.6 mol/L.



 

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