HU189617B - Process for removing simultaneously adipic materials and polyphenols from barked sunflower seeds - Google Patents

Abstract

The invention relates to a solubilizer for the solid-liquid extraction of lipids and poly-phenols from the most recent, in bladder or dandruff-transmitted, sunflowerseed. THE OBJECTIVE OF THE INVENTION IS TO PROVIDE A NEW SOLVENT WHICH CAN EXTRACT MORE THAN AN UNEXPECTED COMPONENT AT THE SAME TIME FROM SUNFLOWER SEED. According to the invention, the new solvent comprises a mixture of hydrocarbons, preferably n-hexane, aethanol and water, the content of which is varied from 40 to 70% by volume of the total mixture by volume of 40 to 70% by volume and the other components by 60 to 30% by volume. % VARIATES WITH AN ALTERNATIVE VARIABLE AGENT OF AETHANOL TO WATER OF 95: 5 TO 50; 50.

Description

The present invention relates to a process for the simultaneous removal of fatty substances and palifenols from sunflower seeds.

Several extraction methods are known for removing fatty matter from sunflower seeds. For example, in the procedure described in Agriculture and Industry, Vol. 3, pp. 11-12, pp. 8-11 (1949), sunflower seeds were prepared with 96% ethanol, Chem. Prod. -10, 12, and extracted with hexane. In both cases, only fatty substances are extracted, the polyphenol content of the seeds remaining in the seeds, so that the seeds so treated are of limited use due to the presence of undesirable polyphenols.

Polyphenols are, according to the literature, removed from sunflower seeds by first treating the seeds with hexane to remove greasy material and then extracting them with alkaline solutions to recover the polyphenols. However, alkaline treatment causes irreversible denaturation of proteins.

The invention is based on the discovery that extraction of sunflower seeds with a two-phase mixture containing n-hexane and aqueous ethanol simultaneously eliminates both fatty substances and polyphenols. Thus, double extraction is avoided and a product completely free of undesirable substances is obtained.

According to the invention, the husked sunflower seeds are extracted with a mixture of n-hexane / aqueous ethanol (40:60) to 70:30; in aqueous ethanol. ethanol and water between 95, 5 and 5O, 5O, sunflower seeds and. the extraction solvent mixture had a weight ratio cg / volume of 1: 1 to 1: 10 and the extraction was carried out at a temperature of 20 to 50 ° C for 0.5 to 6 hours.

The process of the invention, which is a solid-liquid type extraction process, can be carried out by any of the methods recommended in the literature. The use of the method described in U.S. Patent No. 4,387.110 has been found to be particularly advantageous. The solid-liquid extraction process described therein comprises: introducing a fresh solvent or mixture of solvents into a group of series-connected extraction vessels; each extraction vessel contains a solid material, the vessels being provided with an inlet and outlet nozzle, a stirring device and a filter insert to prevent excess solids from escaping through the solvent outlet; the filter cartridge protrudes into the vessel near the agitator such that the movement of the solvent or solvent agitator reduces the risk of clogging of the filter by transferring the extracted material (s) from one extraction vessel to another and then extracting the extractable substance (s) from the solid in one of the vessels, switching the fresh solvent feed to the next vessel, removing the solid residue from the first, and filling the vessel with fresh solids, followed by the last member of the group of connected vessels.

The process can extract some components with a single solvent or a mixture of two or more solvents through n series connected extraction vessels, using mixing during the extraction process.

The solvent (s) is / are fed (and removed) at a well-selected flow rate from the vessels, usually at a specific flow rate of 2 nr / h nr ^{2 to} 15 nr ³ / hm ² , with continuous flow through the series connected vessels. .

Practically, after each vessel is filled with a suitably comminuted solid, the solvent is introduced into each vessel and stirring is initiated.

Then, fresh solvent is fed into the first vessel, which dilutes what is already contained therein and extraction becomes very efficient.

The solvent leaving the first vessel is introduced into the next vessel and the operation described above is repeated and then repeated over and over again in successive n number of extraction vessels.

As soon as the solids in the first vessel do not contain any extractable components, they are drained and fresh solvent is added to the vessel, which is then bound as the last member of the row. The feed of fresh solvent is changed from the first vessel to the second vessel and so on.

Once the finest particles of the solid (about 10% of the solid) have been transferred from each vessel to the solvent stream, a filter must be placed in the vessels to remove solids entrapped in the liquid phase from the liquid phase and complete extraction.

The practical applicability and efficiency of the procedure is closely related to the number of variables.

It has already been shown that the basic parameter is the specific flow rate of the solvent fed to each extraction vessel, typically between 2 and 15 m ³ / hr m ² .

Other parameters such as vessel diameter: height ratio, filter element geometry, filter element aperture size, material, thickness, slurry kinematic viscosity, and mixing intensity to be maintained in the vessel.

The said patent states that anyone skilled in the art will be able to choose the appropriate values for the listed parameters to optimize the extraction process and efficiency, including the material treated, its size, the solvent and all other factors.

However, the said patent does not make any reference to the possibility of using different phases of a mixture of temers, but it seems that the said process is suitable for the use of a single solvent or a mixture of miscible and similar solvents. However, it has been found that the use of the two-phase, three-component mixture of this invention in this extraction process not only results in a high quality product, but is also easy to carry out.

Analytical methods for the chemical characterization of sunflower seeds and products derived therefrom

The moisture, ash and crude fiber content is determined by A.O. A.C. standard method (Association of Official Analytical Chemists, 12th Edition, 1975).

The protein content was determined by the macro-Kjeldald method with a nitrogen content of 5.70 coefficient-22

Expressed as 189,617 densities. The value of total prime material content is specified in A.A.C.C. It was determined by the petroleum ether method described in No. 30-26. Polyphenol compounds were measured by the colorimetric method of Bittoni et al., Riv. Ital. Sost.Crasse, 54, 421, 1977. Total sugars were determined by the method of M Dubois et al. (Analytical Chemistry, 28, 350-356, 1968), with the exception that no separation of the individual sugars was performed, only the total sugar content was considered to be present in the product.

In the P.D.I. (protein distribution index), which is used to measure the amount of nitrogen that can be distributed in water under natural pH conditions, showed good agreement with A.O.C.S.

10-65, Revised 1969).

All the details of the operation will become apparent from the following examples, which are intended to illustrate the invention without limiting it.

Example 1

No. 1 The sunflower seeds of the composition shown in Table I are completely milled in a Hydromecanique et Frottement mill and milled to 0.25 mm in a Diefenback L2 / 30/30 mill. The products thus obtained are treated with a mixture of n-hexane 601% ethanol 35% water 51%

The operating conditions for solid-liquid extraction are as follows:

filling ratio of extraction vessels (weight (kg) to volume ratio (liter)) 1: 4 extraction time 6 hours extraction temperature 45 ° C extraction ratio (volume volume) 1: 7.5

No. 1 spreadsheet

Chemical composition of a sample of sunflower seeds moisture 6% by weight, other components on a dry matter basis 60,0% by weight of proteins 22.01% ash 2.91% crude fiber 3.51% sugars 4.41% phenols 2.41% other nitrogen-free esters 4.8%

The final product obtained has the following composition: moisture 6.51% of the other components on a dry basis; prime substances 0.5% by weight phenols 0.81% proteins (Nx5.7) 65.11% sugars 1.91%

P.D.I. (Protein distribution index) 8.9%

Example 2

Sunflower seeds of the same composition and treatment as in Example 1 were treated with t% n-hexane, t% ethanol, and 10% water

20 containing the mixture under the following solid-liquid extraction conditions: (volume by volume) extraction time extraction temperature 1: 4 6 hours 45 ° C 25 extraction ratio (mass: volume) 1: 7.5

The composition of the extracted product is as follows:

moisture other components calculated on the dry matter: 7.3% prime materials 2.1% phenols 0.17% 30 proteins (Nx5.7) 59.6% sugars 0.6% PD.I. 53%

Patent Claim Point

Claims (1)

Patent Claim Point A process for the simultaneous removal of fatty substances and polyphenols from milled sunflower seeds, characterized in that the sunflower seeds are extracted with n-hexane / aqueous ethanol (40 60) to (70 30); in aqueous ethanol, ethanol and The volume of water is 40 to 955 to 5050, the weight ratio of sunflower seeds to the extraction mixture is 1: 1 to 1:10, and the extraction is carried out at 20 to 50 ° C for 0.5 to 6 hours.