RU2248373C2 - Pectin preparation production method - Google Patents

Abstract

FIELD: vegetable-origin chemicals production.

SUBSTANCE: method envisages breakage and mixing of sunflower anthodia and citrus squeezings at weight ratio between 1:9 and 9:1, hydrolysis-extraction of the mixture, separation of liquid phase, and recovery of desired product therefrom. According to invention, before mixing, raw material is consecutively extracted with acetone and liquid carbon dioxide at superatmospheric pressure, after which second extract is separated and pressure is dropped to atmospheric value, hydrolysis-extraction is effected consecutively in concurrent and countercurrent process realization modes with intermediate squeezing operation. Extractant used in countercurrent extraction stage is water and, in the subsequent concurrent extraction stage, extractant is acidified.

EFFECT: improved quality of desired product due to eliminated unwanted taste and scent without worsening technological properties and reducing yield of pectin.

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 for the production of a pectin preparation from baskets of sunflower, providing for their grinding, heating to protein denaturation, extraction with acetone or ethyl acetate, hydrolysis-extraction of the solid phase, separation of the liquid phase and isolation of the target product from it (Sobol I.V., Biochemical substantiation of the technology for producing pectin of increased biological value from sunflower inflorescences. Abstract of thesis, Candidate of Technical Sciences - Krasnodar: KubGAU, 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, pp. 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 acetone and liquid carbon dioxide at a pressure above atmospheric with the separation of the corresponding extracts, after separation of the second extract, the pressure the precipitation is sharply reduced to atmospheric, the solid phases of baskets of sunflower and citrus squeezes are mixed in a weight ratio of 1: 9 to 9: 1 with their direction for hydrolysis-extraction, while hydrolysis-extraction is carried out by sequentially conducting the process in a direct flow and in countercurrent flow with intermediate extraction and use of water as an extractant at the stage of countercurrent conduct of the process, and at the stage of direct flow of the process of the extract separated after the countercurrent stage with the addition of acid,

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 acetone 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 science - L .: VNIIZh, 1982, p.6-14), which respectively contain essential bitter oils and glycosides cous, and high molecular weight non-polar substances of different groups having resinous odor. Next, the solid phase is also separately extracted with liquid carbon dioxide at a pressure above atmospheric and the corresponding extracts are separated without changing the pressure by known methods (Kasyanov G.I. et al. Processing of plant materials with liquefied and compressed gases. - M.: AgroNIITEIPP, 1993, 40 from.). The residual acetone passes into the extracts, which excludes the further transition of acetone through 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 carbon dioxide 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 in a direct flow and in counterflow 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 extracts in the food industry. Thesis. - M.: VNIIKOP - RosZITLP, 1996, p. 28) with process parameters determined by known methods (I. Ilyina, Scientific basis of the technology of modified pectins. - 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, squeeze, according to 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., inetika degradation of the polysaccharide during the manufacture of pectin Abstract Ph.D. Thesis - 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. The 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 extraneous odors present in the target product from the target method product according to 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 in the same 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 identical the ratios of the same types of raw materials in mixtures differed by a value 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 weight ratio of 1: 9 to 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 mixed before mixing sequentially extracted with acetone and liquid carbon dioxide 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 sequential tion of the process in cocurrent or in countercurrent with intermediate squeezing and using as the extractant in stage countercurrent water conducting the process, and the step of conducting the continuous-flow process, the extract separated after countercurrent stage, with the addition of acid.