RU2253458C2 - Method for pectin production from citrus refuses - Google Patents

Abstract

FIELD: technology for production of pectin extract from citrus refuses.

SUBSTANCE: citrus refuses are subsequently extracted with dimethylformamide and liquid carbon dioxide followed by solid phase separation. Then hydrolysis-extraction of solid phase 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 are used, respectively.

EFFECT: decreased pectin losses.

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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 its concentration or drying (Donchenko L.V., Technology of pectin and pectin products - M .: DeLi, 2000, p. 96 -105).

The disadvantage of this method is the high loss of pectin with an aqueous extract.

The technical result of the invention is to reduce the loss of pectin without compromising its organoleptic properties.

This result is achieved by the fact that in the method for producing a pectin preparation from citrus extracts, which provides for their hydrolysis-extraction and separation of the liquid phase, according to the invention, before hydrolysis-extraction they are sequentially extracted with dimethylformamide and liquid carbon dioxide, while the hydrolysis-extraction is carried out by sequential the process in a direct flow and in counterflow with an intermediate extraction and use as an extractant at the stage of countercurrent extraction I am water, and at the stage of direct-flow extraction of the extract, separated after counter-current extraction.

In this text, the term "pectin preparation" is used in a well-known sense (Brovko O.G. 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, if necessary, are crushed (Donchenko L.V., Technology of pectin and pectin products. A textbook for university students - M .: DeLi, 2000, pp. 96-105), and then extracted with dimethylformamide and the extract is separated by known methods (Bykova S .F., Theoretical and experimental foundations for creating a fundamentally new resource-saving technology for the production of vegetable oils. Abstract of thesis, Doctor of Technical Sciences, St. Petersburg: VNIIZh, pp.21-26; Demchenko PP, Improving the technology of extraction of oil from seeds Sunflower. Abstract of thesis. .: ARSRIF 1982, s.6-14) containing essential oils and glycosides, which have a bitter taste. Next, the solid phase is extracted with liquid carbon dioxide and the extract is separated by known methods (Kasyanov G.I. et al. Processing of plant materials with liquefied and compressed gases - M .: AgroNIITEIPP, 1993, 40 pp.). Residues of dimethylformamide pass into the extract, which excludes the further transition of dimethylformamide according to the stages of the process and its entry into the target product. Next, the solid phase is directed to 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. so-called - M .: VNIIKOP - RosZITLP, 1996, p.28) with process parameters determined by known methods (Ilina I.L. Scientific basis of the technology of modified pectins - Krasnodar: SKZNIISiV, 2001, .88-156). Direct and countercurrent mass transfer processes are carried out with continuous phase transfer and are considered in the steady state (stationary) mode (Kosmodemyansky Yu.V., Processes and Food Production Equipment. Textbook for students of technical schools - M .: Kolos, 1997, p.145-152) . 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 occurs due to the presence of both native citrus acid extracts and acids introduced into the extract. 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 hydrolysis-extraction process by known methods: by adjusting the ratio of phase flow rates and / or introducing into the extract separated after countercurrent extraction, an additional amount of acids according to the results of measuring the pH of the reaction mixture at the input of the solid phase, which ensures optimal flax 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.

Despite the fact that the initial pectin content in citrus squeezes is from 8.9 to 14.9% by dry matter, and the content of water-soluble fraction in it is about 33% (Donchenko L.V., Technology of pectin and pectin products - M .: DeLi, 2000, p. 53, 97), the loss of pectin as a result of its deep hydrolysis can be estimated for the proposed method and the closest analogue according to the known dependencies (Altunyan MK, Kinetics of the destruction of the polysaccharide in the process of producing pectin. Abstract of dissertation .n. - Krasnodar: KPI, 1988). According to experimental data, pectin losses are reduced on average from 33% to 8% of the initial content and coincides with the analytical calculation according to 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, did not allow to identify differences between them in any of the regulated indicators.

Thus, the proposed method can reduce the loss of pectin without compromising its organoleptic properties.

Claims (1)

A method of producing a pectin preparation from citrus squeezes, providing for their hydrolysis-extraction and separation of the liquid phase, characterized in that before hydrolysis-extraction they are sequentially extracted with dimethylformamide and liquid carbon dioxide, while the hydrolysis-extraction is carried out by sequentially conducting the process in a direct flow and in counterflow with an intermediate extraction and using water as an extractant at the stage of countercurrent extraction, and at the stage of direct-flow extraction ation extract separated after countercurrent extraction.