RU2250222C2 - Method for production of pectin material - Google Patents

Abstract

FIELD: technology for production of pectin extract from vegetable raw materials.

SUBSTANCE: claimed method includes grinding and mixing of sunflower heads and citrus refuses in mass ratio from 1:9 to 9:1; hydrolysis-extraction of mixture; liquid phase separation and target product isolating. Before mixing starting materials are subsequently extracted with dimethylformamide and liquid acetylene under elevated pressure. When second extract is separated, pressure is discharged up to atmospheric one, and hydrolysis-extraction is subsequently carried out in forward flow and backflow with intermediate pressing. As extractants in backflow process water and in forward flow process extract separated after backflow stage with acid additive are used, respectively.

EFFECT: target product of improved quality due to removal of undesired taste and odor without losses of technological characteristics and decreasing pectin yield.

Description

The invention relates to a technology for the isolation of pectin from plant materials.

A known method of producing a pectin preparation from citrus squeezes, providing for their extraction with water, hydrolysis-extraction of the solid phase, separation of the liquid phase and isolation of the target product from it (Donchenko L.V., Technology of pectin and pectin products - M .: DeLi, 2000, p. 96-105).

A known method of producing a pectin preparation from baskets of sunflower, providing for their grinding, heating to protein denaturation, extraction with ethyl acetate or acetone, hydrolysis-extraction of the solid phase, separation of the liquid phase and isolation of the target product from it (I. Sobol, Biochemical substantiation of the technology for producing pectin increased biological value from sunflower inflorescences. Abstract of thesis, Candidate of Technical Sciences - Krasnodar: KubSAU, 1997, pp. 8-21).

A common disadvantage of these methods is the low specific yield of pectin.

A known method of producing a pectin preparation, comprising crushing and mixing baskets of sunflower and citrus squeezes, hydrolysis-extraction of the mixture, separation of the liquid phase and isolation of the target product from it (Lakeu M.Y., Development of the technology of combined pectins from plant materials of Ethiopia. Abstract of diss. To Ph.D. - Krasnodar: KubSAU, 2001, p. 8-20).

This method allows to increase the specific yield of pectin, but the target product has a specific smell and a bitter taste, which limits the possibility of its use.

The technical result of the invention is to improve the quality of the target product by eliminating undesirable taste and odor without compromising its technological properties and without reducing the specific yield of pectin.

This result is achieved in that in a method for the production of a pectin preparation, comprising crushing and mixing baskets of sunflower and citrus squeezes, hydrolyzing-extracting the mixture, separating the liquid phase and isolating the desired product from it, according to the invention, before mixing the baskets of sunflower and citrus squeezes separately and sequentially extracted with dimethylformamide and liquid acetylene at a pressure above atmospheric with separation of the corresponding extracts, after separation of the second extract, yes the luminescence is sharply reduced to atmospheric, the solid phases of baskets of sunflower and citrus squeezes are mixed in a ratio by weight from 1: 9 to 9: 1 with their direction for hydrolysis-extraction, while hydrolysis-extraction is carried out by sequentially carrying out the process in a direct flow and in countercurrent with intermediate extraction and use of water as an extractant at the stage of countercurrent conduct of the process, and with the addition of acid at the stage of direct flow of the process of the extract separated after the countercurrent stage.

In this text, the term "pectin preparation" is used in a well-known sense (Brovko OG, Study of some merchandising and physicochemical properties of marmalade masses and marmalade based on applesauce and pectin preparations. Abstract of thesis. Ph.D. - M .: MINH, 1975, 30 p.).

The method is implemented as follows.

Citrus squeezes and baskets of sunflower are separately chopped, separately extracted with dimethylformamide and the extracts are separated according to well-known methods (Bykova SF, Theoretical and experimental principles for creating a fundamentally new resource-saving technology for the production of vegetable oils. Abstract of thesis, Doctor of Technical Sciences - St. Petersburg: VNIIZh, p.21-26; Demchenko PP, Improving the technology of extraction of oil from sunflower seeds. Abstract of the dissertation, candidate of technical sciences -L .: VNIIZh, 1982, p.6-14), which respectively contain essential oils and glycosides possessing bitter taste, and high molecular non-polar substances of various groups with a tarry odor. Next, the solid phase is also separately extracted with liquid acetylene at a pressure above atmospheric and the corresponding extracts are separated without changing the pressure according to known methods (Kasyanov G.I. et al., Processing of plant materials with liquefied and compressed gases - M .: AgroNIITEIPP, 1993, 40 pp. ) The residues of dimethylformamide are transferred to extracts, which excludes the further transition of dimethylformamide according to the stages of the technological process and its entry into the target product. Further, the pressure over the solid phase of both types of raw materials is sharply reduced to atmospheric. This leads to a sharp boiling of acetylene and explosive grinding of plant materials, accompanied by the destruction of cell membranes. Next, the solid phase of baskets of sunflower and citrus squeezes is mixed in a weight ratio from 1: 9 to 9: 1, in which there was an increase in the specific yield of pectin (Lakeu M.Y., Development of the technology of combined pectins from plant materials of Ethiopia. Abstract of thesis. the so-called Krasnodar: KubSAU, 2001, pp. 8-20), and sent for hydrolysis-extraction.

Hydrolysis-extraction is carried out initially in a direct-flow and then counter-flow, on any sequentially installed direct-flow and counter-current extractors or on a sectional extractor of a special design (O. Kvasenkov, Improving the technology for obtaining and using plant raw material extracts in the food industry. Thesis. the so-called - M .: VNIIKOP - RosZITLP, 1996, p.28) with process parameters determined by known methods (I. Ilyina, Scientific principles of modified pectin technology - Krasnodar: SKZNIISiV, 2001, p. 88-156). To reach the steady state, the entire extraction system is filled with one of the phases: liquid, that is, water, or solid, that is, squeezed, according to a subjective choice. After this, the supply of the second phase begins, and as soon as it reaches the exit, they start feeding and moving the first phase, and the process enters into a steady state. In the steady state, at the countercurrent extraction stage, water is used as the extractant. Water does not have a hydrolyzing ability with respect to pectin substances and extracts from the raw material only those substances that are in it in advance in a water-soluble form. In addition to pectin, at the countercurrent extraction stage, mono- and oligosaccharides and organic acids pass into the extract.

The separated extract is fed to a straight-through extraction step. The solid phase at the outlet practically does not contain soluble substances, which allows us to conclude that the loss of pectin is reduced in comparison with the closest analogue, in which hydrolysis-extraction by insisting in the solid phase after extraction always contains extract residues and loss of pectin is inevitable.

At the stage of direct-flow management of the hydrolysis-extraction process, intensive hydrolysis of protopectin takes place not only due to the introduced acids, but also due to the native acids of citrus extracts and additionally introduced acids with the extract, which are returned from the countercurrent process stage. Since the content of acids in citrus fruits and squeezes, respectively, varies depending on the type, variety and growing conditions, the required acid concentration is achieved at the stage of direct-flow management of the hydrolysis-extraction process by known methods: by adjusting the ratio of phase flow rates and introducing into the extract separated after countercurrent extraction, additional amount of acids according to the results of measuring the pH of the reaction mixture at the inlet of the solid phase, which ensures optimal hydrolysis conditions. After completion of the direct-flow stage of the process, the liquid phase is separated by gravity and the extraction of the solid phase. The concentration of pectin in the liquid phase is higher than in the closest analogue, which in some cases eliminates the need for its concentration, for example, when using the target product in the food industry in the beverage industry. The solid phase, containing the remains of extractive substances, enters the countercurrent stage of the process. At this stage, pectin substances that are converted to a soluble state are exposed to acids, the concentration of which decreases during the process, which reduces the possibility of deep hydrolysis of pectin and, accordingly, reduces its loss compared to the closest analogue.

While the initial pectin content in citrus squeezes is from 8.9 to 14.9% by dry matter, the content of water-soluble fraction in it is about 33%, and in sunflower baskets, respectively, from 12 to 24% by dry matter when contained in water-soluble fraction from 30 to 40% (Donchenko L.V., Technology of pectin and pectin products - M .: DeLi, 2000, p. 53, 55, 97), the loss of pectin as a result of its deep hydrolysis can be estimated for the proposed method and the closest analogue to known dependencies (Altunyan M.K., K polysaccharide degradation inetics during the production of pectin. Abstract of thesis, Candidate of Technical Sciences - Krasnodar: KPI, 1988) According to experimental data, the losses of pectin in the proposed method and in the closest analogue are the same, which coincides with the analytical calculation by the above method.

The product obtained according to the described technology complies with GOST 29059.

Determination of the organoleptic properties of the products obtained by the proposed method and the closest analogue, carried out according to GOST 8756.1, revealed the absence of the bitter taste and odors present in the target product from the target product by the closest analogue.

As indicated above, the pectin preparations obtained by the proposed technology for any tested combinations of sunflower varieties, types and varieties of citrus fruits, in any weight proportions from the above interval, did not have a bitter aftertaste and tarry odor. The specific yield of pectin substances in all cases was not lower than that of the closest analogue with identical mass ratios of the same types of raw materials in mixtures. Gelling and sorption ability determined by the standard method (L. Donchenko, Technology of pectin and pectin products - M .: DeLi, 2000, p. 41-48), preparations obtained by the proposed method and by the closest analogue with the same ratios of the same types raw materials in mixtures differed by an amount close to the error in their determination.

Thus, the proposed method can improve the quality of the target product by eliminating undesirable taste and smell without compromising its technological properties and without reducing the specific yield of pectin.

Claims (1)

A method for the production of a pectin preparation, comprising crushing and mixing baskets of sunflower and citrus squeezes in a ratio by weight of 1: 9-9: 1 hydrolysis-extraction of the mixture, separation of the liquid phase and isolation of the target product from it, characterized in that the raw materials are sequentially extracted with dimethylformamide before mixing and liquid acetylene at a pressure above atmospheric, and after separation of the second extract, the pressure is reduced to atmospheric, while hydrolysis-extraction is carried out by the following carrying out the process in a direct flow and in a counterflow with an intermediate extraction and using water as an extractant at the stage of the countercurrent process, and with the addition of acid, at the stage of the direct flow process, of the extract separated after the countercurrent stage.