Method of producing pectin from seaweed

FIELD: chemistry.

SUBSTANCE: invention relates to food industry. The method involves preparing raw material, hydrolysis of the prepared plant material with acid solution at pH 3-5 and temperature 50-60°C for not more than 4 hours and separation of the hydrolysate. The hydrolysed plant material is then washed with water and pectin is then extracted therefrom in an extractor with a false bottom in extraction agent circulation conditions in two steps. First, pectin is extracted from the material with 0.5% ammonium oxalate solution while heating at temperature 45-50°C and pressure 1.5-2.5 atm for not more than 40 min, and then with 1.5% ammonium oxalate solution while heating at temperature 75-80°C and pressure 3-4 atm for not more than 5 min. Further, the extract undergoes ultrafiltration purification and concentration. Pectin is then precipitated from the extract with ethyl alcohol containing sodium chloride and then dried. In one version, the pectin precipitate is further washed with 80% ethyl alcohol before drying.

EFFECT: invention significantly cuts duration of the process of obtaining pectin and lowers the cost of the obtained product by cutting power consumption and optimising the amount of reagents used, particularly by cutting the amount of ethyl alcohol used to precipitate pectin three-fold.

7 cl, 2 ex

 

The invention relates to biotechnology, namely to receive the pectin from the sea grasses of the family Zosteraceae, with a complex of biologically active properties that enable its use, in particular, as a tonic, AIDS in the treatment of the digestive system, an additional source of dietary fiber, as well as complexing and stuporously ability that allows them to effectively use in medicine, the pharmaceutical and food and other industries.

In the traditional methods of obtaining pectin from plant materials are operations such as preparation of raw materials, hydrolysis of the raw material, washing prohydrolized material by water extraction of pectin from prohydrolized raw materials, the deposition of pectin, rinsing and drying.

Known methods for producing pectin combine impacts on different pectin containing raw materials chemicals, temperature and pH. Despite some disadvantages of these methods (the depolymerization of pectin in the case of rigid regimes of temperature and pH, using for cleaning impurities of large amounts of organic solvents and others), various modifications to the present time are the basis of the technological scheme for industrial paucisymptomatic substances.

In this regard, it seems reasonable to search for new softer technologies, allowing to intensify mussalman in the system of pectin containing feedstock - solvent, and to accelerate the processes of hydrolysis and extraction of pectic substances, which are directed to the claimed invention.

A known method of producing pectin from sea grasses species of eelgrass (Zostera marina L. and Zostera pacifica Wats., Zostera japonica Aschers, et Graebn., next - Zoster) and phyllospadix (Rhyllospadix scouleri Hook.), including the grinding of raw materials, the processing solution of hydrochloric acid at a temperature of 50°C and pH 4-5 with constant stirring, separating the acid, washing with water processed raw materials to neutral reaction and extraction of pectin (Zosterin) of the hydrolyzed raw material 1%ammonium oxalate solution at a temperature of 75-80°C for 6 hours under stirring. Then the extract obtained is cooled to room temperature, cleaned from mechanical impurities and precipitate the pectin from the ethanol extract taken three times the number compared to the number of the obtained extract. The precipitated pectin is separated from the aqueous ethanol by filtration, pulverized and washed with ethanol. Then to achieve high-quality pectin perform repeated washing and filtering of pectin organic solvents (methanol in the mixture is from acetyl chloride, methanol, ethanol and subsequent drying of pectin (A.S. USSR №921500, publ. 23.04.1982, BI No. 15). Obtained in this way pectin can be used as gelling agents in the food industry and Microbiology.

The disadvantages of this method are the necessity of using large quantities of organic solvents on the stage of purification of pectin and a multi-stage process, due to repeated washing the product to remove the non-solvent. Furthermore, multiple leaching of pectin leads to depletion of its composition due to the leaching or destruction of such nutrients, such as fiber, protein, tannins and flavonoids, and reduce the biological value of pectin.

The closest in purpose and technical nature of the claimed method is a method of producing pectin from the sea grasses of the family Zosteraceae (U.S. Pat. Of the Russian Federation No. 2000064, publ. 07.09.1993, BI No. 33-36), selected as a prototype. According to this invention prepared raw material is subjected to hydrolysis by hydrochloric acid with a pH of 2.0 to 4.0 at a temperature of 50-60°C for 2.5 to 4 hours. Upon completion of hydrolysis, the hydrolysate is separated and carried out washing the material with water until neutral wash water. Extraction of pectin exercise of 0.5-1.0%ammonium oxalate solution PR is a temperature of 50-60°C for 2.5 to 4 hours. Then spend the ultrafiltration purification and concentration of the extract pectin in the hollow-fiber membranes with a transmission capacity 15000-30000 daltons, and drying the target product is performed by sputtering at a temperature that ensures the final temperature of the finished product 85-90°C. In the result, the method pectin is suitable for use in the food industry, which has a higher P-vitamin activity and greater capacity for excretion of heavy metal ions in comparison with pectin obtained by A.S. USSR №921500.

However, the way the prototype is characterized by the following disadvantages: high duration of the process of obtaining the target product (stage hydrolysis and extraction take 5-8 hours, drying the concentrated extract in spray without prior deposition of the extract pectin requires more time) and the associated increased cost of pectin, due to the large consumption of electricity.

The objective of the invention is to develop a method of producing pectin from the sea grasses of the family Zosteraceae, providing a reduction in the duration of the process of obtaining pectin and reducing its cost due to the reduction of energy consumption and optimize the flow of reagents at the stage of deposition of p is China.

The problem is solved by the proposed method of producing pectin from the sea grasses of the family Zosteraceae, including the preparation of original plant material, the hydrolysis of the raw material with an acid solution at a temperature of 50-60°C for a time not exceeding 4 hours, the separation of the hydrolysate, the washing water prohydrolized plant materials and extraction of pectin by ammonium oxalate solution when heated, the subsequent ultrafiltration purification by concentrating the obtained extract and drying by heating, in which, in contrast to the known method, the hydrolysis is performed with an acid solution with a pH of 3.0 to 5.0, and the extraction of pectin from prohydrolized vegetable raw materials is carried out in the extractor with "false" the bottom in the conditions of circulation of the extractant in two stages: first, preferably of 0.5%ammonium oxalate solution when heated in the range of temperature of 45-50°C and a pressure of 1.5 to 2.5 ATM for no more than 40 min, then preferably of 1.5%ammonium oxalate solution when heated in the range of temperature of 75-80°C and a pressure of 3-4 atmospheres for a period of not more than 50 minutes, and after ultrafiltration purification and concentration of the extract is carried out the deposition of pectin ethanol containing sodium chloride.

The proposed method of producing pectin from the sea grasses of the family Zosteraceae carry ledouxnebria.

As a source of plant raw materials containing pectin, in the invention use sea grass Zostera mainly of two types: "Zostera asiatica Maki syn" and "Pasifica auct, Zostera marina growing, particularly along the coast of Primorsky Krai.

The zoster mined in the terms established by the Rules harvesting of marine plants, namely from August 15 until the end of October.

Sea grass Zoster can be extracted in two ways - through underwater mowing grass or the gathering fresh grass after a storm of emissions for a period of not more than 8 hours after release.

The extracted sea grass washed from mechanical impurities in a suitable volume of the capacity for 3 fresh running water at a temperature of 15-25°C.

For year-round production of pectin cleaned from mechanical impurities the Zoster dried on a special platform and Packed in plastic bags from a film according to GOST 10354. Then Packed sea grass placed in the freezer, where it can be stored at a temperature(18-20°C for 10 months without losing useful properties. If necessary, processing of sea grass it defroster in the bath at room temperature.

Svezhedobytogo or thawed sea grass is crushed to a size of 1-2 cm and hydrolyzing a solution of a suitable mineral or organic acid, often the spine of hydrochloric or acetic acid, with a pH of 3.0 to 5.0 at a temperature of 50-60°C for a time not longer than 4 hours.

Empirically it is found that the interval of pH 3,0-5,0 used for hydrolysis acid provides optimal conditions for obtaining high-quality target product with a good yield and at the same time allows to avoid possible effects of degradation of pectin in the field of pH values close to 2.

At the end of the hydrolysis of separating the hydrolyzed feedstock and washed prehydrolyzed sea grass running water until neutral wash water.

Then hold the extraction of pectin from prohydrolized plant material in an extractor with a false bottom in the conditions of circulation of the extractant in two stages: first, preferably of 0.5%ammonium oxalate solution at intervals of temperatures of 45-50°C and a pressure of 1.5 to 2.5 ATM for no more than 40 min, and then preferably to 1.5%ammonium oxalate solution at intervals of temperatures of 75-80°C and a pressure of 3-4 atmospheres for a period of not more than 50 minutes

Extraction of pectin in the first stage under conditions of low concentrations of ammonium oxalate solution (preferably 0.5%), and a temperature of 45-50°C and a pressure of not higher than 2.5 (1.5 to 2.5) ATM has a mild effect on progeressive raw materials, resulting in the structure of the raw material becomes less dense.

Then pressure the e shed, bring the concentration of ammonium oxalate solution to 1.5%, increase the temperature to 75-80°C, pressure up to 3-4 ATM and continue the extraction.

Extraction of pectin in the second stage takes place in more severe conditions, namely the ammonium oxalate solution with a higher concentration at a higher temperature and pressure. Under these conditions, the extraction of pectin is more fully and intensely, which dramatically reduces the extraction time and simultaneously increases the yield of the target product.

The presence extractor "false bottom with holes allows you to organize at both stages of the extraction of the effective circulation of ammonium oxalate solution with pump, further reducing the total time of the extraction process.

In the particular case of carrying out the invention use an extractor with a false bottom, which made holes with a diameter of 3-5 mm and a pitch of 6 mm

Experimental studies on the development and substantiation of optimal extraction parameters showed that the time of extraction of pectin in the first stage is not more than 40 min, and the second stage is not more than 50 min, in General, no more than 90 minutes, in contrast to the prototype method, in which the extraction time is 2.5-4 hours.

Then spend the ultrafiltration purification of the extract pectin from low molecular weight organic and Neorganicheskie the impurities and the concentration of the extract on the installation OLA-6 through the hollow fiber filter with a transmission capacity of 15,000 daltons, the pressure is maintained at the level not more than 2 ATM, the temperature of the extract to prevent studnyvrtane support at the level not lower than 40°C, and impurities washed with distilled water.

In the ultrafiltration processing the extract is cleaned from impurities, and the concentration of pectin in the extract is brought to 3%.

The precipitation of the pectin from the concentrated extract spend 96%ethyl alcohol with the addition of salt, sodium chloride in an amount of not more than 10 g per litre of alcohol.

In the prior art it is known that the addition of small amounts of chloride of sodium, chloride, or calcium carbonate intensifies the process of coagulation of pectin due to the increased density of the solution extract pectin.

In experiments to test the optimal consumption of ethanol for precipitation of pectin from the concentrated extract was unexpectedly found that along with the intensification of the process of coagulation of pectin appears an additional advantage of the proposed method lies in the possibility to reduce the number used for the deposition of pectin ethyl alcohol about three times, which is very important for the implementation of pectin production.

The explanation of this effect in the sources of scientific, technical and patent information could not be found. On the contrary, from f the th applicant information sources should the deposition of pectin substances from the extract of lead, adding to the extract with an equal volume of 96%ethanol (U.S. Pat. Of the Russian Federation No. 2095996, publ. 20.11.1997, or adding to the finished extract three times the amount of 96%ethanol (A.S. USSR №921500, publ. 23.04.1982 year).

Next, the precipitated crude pectin washed with 80%ethanol and press hydraulic press. Pressed pectin pulverized using an industrial mixer and spray dried in a tunnel dryer with hot air.

In the particular case of the invention, the drying of pectin is carried out at a temperature not exceeding 70°C to avoid decomposition present in the pectin D-apiose, one of the most important component of the galacturonic acid, providing a product of high pharmacological activity.

The dried product is ground in a ball mill.

Exhaust alcohol solution is subjected to distillation unit distillation complex and return to the production process.

Pectin obtained by the proposed method, in addition to the pharmacological activity has complexing ability in relation to heavy metal ions and stuporously capacity, making it suitable for use in various industries.

Thus, the technical result of the proposed method is the fast reduction in the duration of the process of obtaining pectin due to the substantial reduction of the time of extraction of pectin and, accordingly, reduction in the cost of the resulting product by reducing energy consumption and optimizing the amount of reagent used at the stage of precipitation of the pectin from the extract.

An additional advantage of the invention is the ability to produce pectin year-round from frozen raw material.

The possibility of carrying out the invention the following examples.

Example 1.

Getting pectins from sea grass family Zosteraceae.

90 kg thawed and crushed to a size of 1-2 cm of sea grass placed in gidroizolyator and hydrolyzing with hydrochloric acid to pH 5 at 50°C for 3 hours. The working solution of hydrochloric acid has a concentration of 5%. Then the hydrolysate is drained, and the sea grass washed with water till neutral reaction of wash water. Extraction of pectin from progeressive sea grass is carried out in the extractor with a false bottom with holes with a diameter of 3-5 mm and 6 mm pitch, which provides for circulation of the solvent in the extractor with the help of the pump. First extraction was carried out with 0.5%ammonium oxalate solution at a temperature of 45-50°C and a pressure of 1.5 to 2.5 psi for 40 minutes, after which relieve pressure, adjusting the concentration of ammonium oxalate to 1.5%, heat the ammonium oxalate solution to a temperature of 75-80°C, ivysaur pressure up to 4 bar and continue the extraction for 50 minutes Separated from the recycled raw extract in the amount of 110 l is subjected to ultrafiltration treatment, maintaining the temperature of the extract is not lower than 40°C and a pressure of not more than 2 ATM for installation of hollow fiber cartridges 15000 daltons (UPV-6). For washing impurities using distilled water. The concentration of pectin in the ultrafiltration is brought to 3%. Coagulation pectin spend 96%ethanol containing sodium chloride in an amount of 10 g of salt per litre of alcohol, the addition of ethanol to the extract in the amount of 37 l with obtaining raw sludge pectin. Selected crude precipitate pectin washed with 80%ethyl alcohol in an amount of 5 l and press hydraulic press. Pressed pectin crushed in an industrial mixer and dried in a tunnel dryer with hot air at a temperature not exceeding 70°C.

The duration of the process of extraction of pectin is 90 minutes

Consumption of ethanol on the coagulation of pectin and flushing is 42 litres.

Received 1.9 kg of dry pectin.

The yield of dry pectin from raw materials is 2.1%.

Example 2.

The method of producing pectin from sea grass carried out as in example 1, with the modification of the following conditions.

Hydrolysis prepared sea grass conduct solution of acetic acid with a pH of 3 at 60°C for 4 h the century The working solution of acetic acid has a concentration of 8%.

Conditions for processes of extraction of pectin precipitation from the extract, rinsing, and drying correspond to example 1.

The duration of the process of extraction of pectin is 90 minutes

Consumption of ethanol on the coagulation of pectin and flushing is 42 litres.

Received 1.8 kg of dry pectin.

The yield of dry pectin from raw materials is 2.0%.

These examples suggest the advantages of the inventive method for reducing time of extraction in comparison with the known method 1.7-2.7 times, while achieving comparable yield of the target product.

1. The method of producing pectin from the sea grasses of the family Zosteraceae, including the preparation of original plant material, the hydrolysis of the raw material with an acid solution at a temperature of 50-60°C in a period of time not more than 4 h, the separation of the hydrolysate, the washing water prohydrolized plant materials and extraction of pectin by ammonium oxalate solution when heated, the subsequent ultrafiltration purification by concentrating the obtained extract, and drying by heating, characterized in that the hydrolysis is performed with an acid solution with a pH of 3.0 to 5.0, and the extraction of pectin from prohydrolized vegetable raw materials is carried out in the extractor with a false bottom in the conditions of circulation of the former is Magenta in two stages: first, preferably of 0.5%ammonium oxalate solution when heated in the range of temperature of 45-50°C and a pressure of 1.5 to 2.5 ATM for no more than 40 min, then, preferably of 1.5%ammonium oxalate solution when heated in the range of temperature of 75-80°C and a pressure of 3-4 atmospheres for a period of not more than 50 minutes, and after ultrafiltration purification and concentration of the extract is carried out the deposition of pectin ethanol containing sodium chloride.

2. The method according to claim 1, characterized in that the hydrolysis of the raw material is performed with a solution of hydrochloric or acetic acid.

3. The method according to claim 1, characterized in that the extraction of pectin is carried out in the extractor with a false bottom with holes with a diameter of 3-5 mm and a pitch of 6 mm

4. The method according to claim 1, characterized in that the ultrafiltration purification and concentration of the extract is carried out at a temperature of not extract below 40°C and a pressure of not more than 2 ATM.

5. The method according to claim 1, characterized in that the deposition of pectin extract from exercise of 96%ethanol containing sodium chloride in an amount of not more than 10 g per liter of ethanol.

6. The method according to claim 1, characterized in that the precipitated pectin was washed with 80%ethanol, after which the excess ethyl alcohol squeezed and pressed pectin crush.

7. The method according to claim 1, characterized in that the drying of powdered pectin carried out by spraying in a tunnel dryer with hot air at a temperature not exceeding 70°C.



 

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EFFECT: improved isolating method.

FIELD: vegetable raw technology.

SUBSTANCE: invention relates to a method for isolating pectin from vegetable raw. Method for preparing pectin involves milling and mixing sunflower heads and citrus husks, hydrolysis-extraction of mixture, separation of a liquid phase and isolation of the end product from its. Before mixing sunflower heads and citrus husks are extracted with ethyl acetate and liquid carbon dioxide separately and successively under the above atmosphere pressure. The second extract is separated without pressure change followed by dropping pressure over a solid phase up to atmosphere value and feeding a solid phase to hydrolysis-extraction. Invention provides enhancing quality of the end product due to elimination of undesirable taste and odor and without deterioration of its technological properties and without reducing the specific yield of pectin.

EFFECT: improved preparing method.

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