GB2060673A - Method of Treating Vegetable Raw Materials Containing Thioglycoside - Google Patents
Method of Treating Vegetable Raw Materials Containing Thioglycoside Download PDFInfo
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- GB2060673A GB2060673A GB8032321A GB8032321A GB2060673A GB 2060673 A GB2060673 A GB 2060673A GB 8032321 A GB8032321 A GB 8032321A GB 8032321 A GB8032321 A GB 8032321A GB 2060673 A GB2060673 A GB 2060673A
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- Prior art keywords
- pressure
- extraction
- thioglycoside
- oil
- raw materials
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- 238000000034 method Methods 0.000 title claims abstract description 39
- 229930182475 S-glycoside Natural products 0.000 title claims abstract description 24
- 150000003569 thioglycosides Chemical class 0.000 title claims abstract description 24
- 239000002994 raw material Substances 0.000 title claims abstract description 14
- 235000013311 vegetables Nutrition 0.000 title claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000000605 extraction Methods 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000009835 boiling Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000007669 thermal treatment Methods 0.000 claims description 4
- 239000010903 husk Substances 0.000 abstract description 13
- 238000011282 treatment Methods 0.000 abstract description 10
- 235000011331 Brassica Nutrition 0.000 abstract description 9
- 241000219198 Brassica Species 0.000 abstract description 9
- 150000002632 lipids Chemical class 0.000 abstract description 9
- 235000003901 Crambe Nutrition 0.000 abstract description 7
- 241000220246 Crambe <angiosperm> Species 0.000 abstract description 7
- 230000000433 anti-nutritional effect Effects 0.000 abstract description 5
- 239000000470 constituent Substances 0.000 abstract description 4
- 230000001143 conditioned effect Effects 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 23
- 230000008569 process Effects 0.000 description 15
- 239000000126 substance Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- 150000001875 compounds Chemical class 0.000 description 10
- 108090000623 proteins and genes Proteins 0.000 description 10
- 102000004169 proteins and genes Human genes 0.000 description 10
- 239000002904 solvent Substances 0.000 description 8
- 150000001298 alcohols Chemical class 0.000 description 6
- 244000068988 Glycine max Species 0.000 description 5
- 235000010469 Glycine max Nutrition 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 239000005864 Sulphur Substances 0.000 description 4
- 230000002779 inactivation Effects 0.000 description 4
- 230000001965 increasing effect Effects 0.000 description 4
- 231100000331 toxic Toxicity 0.000 description 4
- 230000002588 toxic effect Effects 0.000 description 4
- 150000003626 triacylglycerols Chemical class 0.000 description 4
- 108090000790 Enzymes Proteins 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 150000002540 isothiocyanates Chemical class 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 235000016709 nutrition Nutrition 0.000 description 3
- 230000035764 nutrition Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 240000002791 Brassica napus Species 0.000 description 2
- 235000011293 Brassica napus Nutrition 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003125 aqueous solvent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 235000014633 carbohydrates Nutrition 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000003750 conditioning effect Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002255 enzymatic effect Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 235000021588 free fatty acids Nutrition 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000006317 isomerization reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000035479 physiological effects, processes and functions Effects 0.000 description 2
- 239000010499 rapseed oil Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- ZIIUUSVHCHPIQD-UHFFFAOYSA-N 2,4,6-trimethyl-N-[3-(trifluoromethyl)phenyl]benzenesulfonamide Chemical compound CC1=CC(C)=CC(C)=C1S(=O)(=O)NC1=CC=CC(C(F)(F)F)=C1 ZIIUUSVHCHPIQD-UHFFFAOYSA-N 0.000 description 1
- TULQBOZEHGWQCN-UHFFFAOYSA-N 5-ethenylsulfanyl-2H-1,3-oxazol-2-id-4-one Chemical compound C(=C)SC1C(N=[C-]O1)=O TULQBOZEHGWQCN-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- 102000009027 Albumins Human genes 0.000 description 1
- 108010088751 Albumins Proteins 0.000 description 1
- DPUOLQHDNGRHBS-UHFFFAOYSA-N Brassidinsaeure Natural products CCCCCCCCC=CCCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- URXZXNYJPAJJOQ-UHFFFAOYSA-N Erucic acid Natural products CCCCCCC=CCCCCCCCCCCCC(O)=O URXZXNYJPAJJOQ-UHFFFAOYSA-N 0.000 description 1
- 102000006395 Globulins Human genes 0.000 description 1
- 108010044091 Globulins Proteins 0.000 description 1
- 244000299507 Gossypium hirsutum Species 0.000 description 1
- 102000004882 Lipase Human genes 0.000 description 1
- 108090001060 Lipase Proteins 0.000 description 1
- 239000004367 Lipase Substances 0.000 description 1
- 102000015439 Phospholipases Human genes 0.000 description 1
- 108010064785 Phospholipases Proteins 0.000 description 1
- 244000273256 Phragmites communis Species 0.000 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 235000019728 animal nutrition Nutrition 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007073 chemical hydrolysis Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- DPUOLQHDNGRHBS-KTKRTIGZSA-N erucic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-KTKRTIGZSA-N 0.000 description 1
- 235000013861 fat-free Nutrition 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 235000019421 lipase Nutrition 0.000 description 1
- 235000004213 low-fat Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 238000011328 necessary treatment Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- -1 oils Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 235000020238 sunflower seed Nutrition 0.000 description 1
- 108010058651 thioglucosidase Proteins 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L11/00—Pulses, i.e. fruits of leguminous plants, for production of food; Products from legumes; Preparation or treatment thereof
- A23L11/30—Removing undesirable substances, e.g. bitter substances
- A23L11/32—Removing undesirable substances, e.g. bitter substances by extraction with solvents
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Agronomy & Crop Science (AREA)
- Botany (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a method of treating vegetable raw materials containing thioglycoside, particularly brassica and crambe seeds. According to the invention, vegetable thioglycoside-containing raw materials, particularly brassica and crambe seeds and processed products thereof, are pre-crushed, possibly conditioned, flocculated and subjected to repeated extraction with ethanol under pressure, at a boiling temperature corresponding to the excess pressure applied, with a view to obtaining oil and reducing harmful materials. With alternating pressure and relief from pressure after each ethanol treatment, the oil-containing micell is separated at the high pressure, whereupon the extraction residue, still under pressure, is abruptly relieved of pressure. The method removes lipids and thioglycosides as completely as possible from brassica and crambe seeds and processed products thereof, in one operation for obtaining a high quality oil and extracted husk which is substantially free from anti-nutritive constituents.
Description
SPECIFICATION
Method of Treating Vegetable Raw Materials Containing Thioglycoside
The invention relates to a method of treating vegetable raw materials containing thioglycoside with simultaneous fat removal and detoxication, particularly brassica and crambe seeds and products obtained by processing them; the purpose being to enable the oil and extracted husks to be utilised in human and animal nutrition.
Brassica and crambe seeds and products obtained by processing them are known, firstly, to contain antinutritive compounds, chiefly thioglycosides, in large or small quantities according to the type and variety. By enzymatic-hydrolytic splitting in vitro or in vivo, with possible secondary conversion with other materials contained in the seeds, these form goitrogenous or toxic artefacts, such as isothiocyanates (ITC), vinyl thiooxazolidone (VTO), nitriles and thioureas; thereby greatly reducing the usefulness of the husks obtained after the extraction of the oil for animal feeding and making its useful human nutrition value questionable.Rape oils obtained by traditional methods of pressing and extraction, in addition to their content of erucic acid, generally contain relatively large quantities of sulphur-containing products resulting from the splitting of thioglycosides, and certain lipid constituents (phosphatides, free fatty acids). This again limits the use of the oils or necessitates a large amount of refinement to eliminate these materials.
On the other hand, the increasing demand for highgrade protein-rich fodder materials and the increasing interest in opening up potential protein sources for novel foods represents a permanent challenge to use available resources which, like the above mentioned products, are distinctive in having good properties in respect of functional and nutrition physiology and methods of application, i.e.
resources which are very serviceable. However, this again presupposes the removal of the above mentioned accompanying anti-nutritive substances either by steps taken in growing the plants or by technical processes.
The growing international trend to increase the acreage for brassica seeds is also due to the high output and favourable growth conditions in those climatic regions where the cultivation of other oil seeds, such as soya bean, cotton and sunflower seed, is impossible or only possible to a limited degree.
In patent literature therefore, particularly in the last decade, an increasing number of processes have been proposed, aiming to remove thioglycosides and their products by extractive, thermal, enzymatic or chemical methods.
Of these, the processes which have to be taken into account in assessing the state of the art for the present invention are those based on extraction. These include processes directed towards extractive preliminary treatment of the seeds or corresponding post-treatment of the degreased residues of the process using binary aqueous ethanol solvent systems, with a view to removing in tact thioglycosides. Processes based on the extraction of hydrolysed thioglycosides with methanol are also involved. The former processes again require preliminary enzyme inactivation in order to obtain maximum extraction effects, while the latter necessitate deliberate enzymatic or chemical splitting in order to affect solubility.
The above mentioned processes generally have the disadvantage of losing a large amount of the materials, such as carbohydrates and soluble proteins, which give them their value and which involve an additional economic outlay to recover. Considerable extra costs are involved in the necessary treatment of the waste water and rectification of the solvent. Furthermore, these processes, as already mentioned, require two separate stages of treatment for obtaining the oil and detoxicating the husks, and a special procedure involving cost-intensive separation lines is needed for solid-liquid separation of the lixiviated raw materials.
It is also known to use pure alcohols and alcohol-containing non-aqueous or aqueous solvent systems in obtaining oil from raw materials of vegetable and animal origin, largely soya beans and fish.
The use of such solvents can chiefly be seen in connection with the desired improvement in the quality of the final products, oil and husk, and the intensification of development in the fields of extraction by displacement and direct extraction of oil seeds rich in fat.
However, the main drawback of these processes is the fact that the critical step of digesting the cells, i.e. the step with a great influence on the yield and quality of the oil, has not yet been adequately mastered. In direct extraction digestion is brought about mainly by thermal treatment of the seeds, whereas in extraction by displacement it is effected by mechanolytic treatment only. Such operations preferably include steam conditioning, possibly at increased pressure, or intensive comminution possibly in conjunction with flocculation or granulation.
The effectiveness of an extraction process is known to depend not only on the speed at which the solvent is diffused in the seed material to be extracted (this is determined inter alia by the morphological character of the seeds and the extent to which they are reduced in size), but also on the solubility of the compounds to be extracted in the extracting agent. An improvement in the extracting action is consequently sought both through intensifying the diffusion process, e.g. through treating the seeds by ultrasonics or alternating pressure, possibly in combination with heat treatment (conditioning), and through a change in the polarity of the solvent, e.g. by adding alcohols.
In the case of the known use of low-molecular-weight alcohols, preferably ethanol and isopropanol, the basic assumption is that these have a low oil-dissolving capacity as compared with hexane or gasoline, which are most commonly used. The composition of whatever substances contained in the seeds are being considered functions as the molecular limiting value. The water content of the alcohol or of the extraction material also has an influence, and certain principles have to be observed in respect of the effective solid-liquid ratio to be chosen and the temperature control.Thus triglycerides become more soluble with an increase in chain length, an increase in the degree of isomerisation and a reduction in the water content of the alcohol; the solubility of triglycerides therein is moreover inversely proportional to the chain length and degree of saturation of the constituent fatty acids. Thioglycosides and products obtained by splitting them behave quite differently in their solubility, as shown by our own tests. These compounds in fact become less soluble with an increase in chain length, an increase in the degree of isomerisation and a reduction in the water content of the alcohol. The different solubility of triglycerides, e.g. oils, and thioglycosides in alcohols, and the comparatively large content of these compounds in brassica seeds is thus the main reason why alcohols have not hitherto been used for direct extraction of these seeds.Another factor which in the past was regarded as a serious disadvantage of extraction with alcohols was that a large amount of solvent is required to obtain a high extracting action, even with relatively low-fat soya beans, if extraction is not carried out within a temperature range far above the boiling point of the alcohol used i.e. under pressure.
The invention aims to remove lipids and thioglycosides as completely as possible from brassica and crambe seeds and processed products thereof, in one operation; and to obtain a high quality oil, i.e.
an oil with few accompanying substances, and an extracted husk material which is substantially free from anti-nutritive substances and which can be used, as a semi-refined material or mixed feed constituent or as an initial substrate, to obtain isolated and concentrated proteins in the food or fodder industry.
The problem underlying the invention is therefore, as far as possible, to indicate specific conditions necessary for digesting the seed cells and extracting the substances in question, so as to eliminate a separate procedure for fat removal and detoxication. Statement of essence of invention.
According to the present invention there is provided a method of treating vegetable raw materials containing thioglycoside for simultaneous fat removal and de-toxication, comprising extracting the raw
material, after preliminary pre-crushing or thermal treatment, with ethanol boiling under superatmospheric pressure, separating the resulting oil-containing micell while still under the superatmospheric pressure, and then rapidly relieving the pressure on the extraction residue.
In this connection it has been found that the effectiveness of simultaneous extraction of lipids and thioglycosides is determined, to a decisive extent, by abrupt depressurising of the seed material freed from the ethanol phase. The drop in pressure per unit of time represents and important limiting value and must take place within a time limit of 1 to 1 0 seconds, preferably 1 to 3 seconds.As a result of the concomitant expansion of the seed material, still moistened with alcohol, there is not only a bursting of the cell membranes and thus a high degree of ceil digestion; the use of ethanol in conjunction with a rise in temperature at the same time results in chemical denaturing and thus aggregation of stored proteins, leading to desirable changes in the structural mechanics of the seed material (channel formation, porosity), thereby greatly enhancing the step of diffusing the solvent in the seed material (together with the solubility this step determines the speed).
The treatment according to the invention furthermore inactivates endogeneous and exogeneous seed enzymes; this is particularly important in the case of myrosinase, which is responsible for decomposing thioglycoside. in traditional methods of obtaining oil, on the one hand, there is more or less incomplete inactivation of myrosase, dependent on the technological system chosen and particularly the temperature and humidity used in the process, so that thiogiycosides are decomposed to varying degrees in the course of obtaining the oil. On the other hand these decomposed products are converted into toxic artefacts by irreversible interaction with proteins, preferably with drastic temperature treatment, and these artefacts are either impossible to extract or can be extracted only after chemical hydrolysis.
Due to the changed solubility of the compounds produced from thioglycosides, this leads either to a relatively high content of sulphur compounds in the oil or to a relatively large proportion of harmful substances, irreversibly bonded to proteins, in the extracted husks. In the first case this will result in comparatively high refinement costs, since the compounds in question act as a catalyst poison in the hydrogenation of rape oil; in the latter case the usefulness of the extracted husks is greatly reduced or special procedures have to be considered to eliminate it.
The invention thus provides the pre-requisites for arresting the undesirable redistribution of sulphur-containing compounds from the seed material into the raw oil and the formation of antinutritive or toxic artefacts; it is desirable to have a certain set water content in the entire seed-alcohol system.
It has further been found that, with a view to simultaneous extraction of lipids and intact thioglycosides, the water content does not substantially exceed a limit of 15% and must not drop substantially below a limit of 1%, since otherwise lipids or thioglycosides will only be extracted to an inadequate extent. It is possible to provide for control of the water content of the entire system by adjusting the water content of the alcohol or seed material. Consequently the use of 85% to absolute ethanol is effective, when the water content of the seed behaves correspondingly within the given limits.
However, a preferred embodiment of the invention uses 96% ethanol and a seed material predried to water contents of < 3%; under these conditions the water content of their alcohol remains virtually constant, so that rectification is no longer necessary. In addition an effective alternative embodiment of the process has been found to consist of setting an excess pressure during extraction of 40 kPa (0.4 bar) to 250 kPa (2.5 bars), preferably 150 kPa (1.5 bars), with a residence time of 10 to 60 mins., preferably 1 5 to 30 mins., per extraction cycle.
The saturated micells obtained can easily be separated into 2 or 3 phases by immediate or successive cooling to approximately 20 and/or 1 OOC; the bottom phase will contain most of the oil.
The middle phase consists preponderantly of substances contained in the seeds, dissolved or dispersed in water, and the top phase consists largely of ethanol. This last or an unsaturated micell should desirably be re-cycied to the processing circuit of the first extraction stages, while fresh ethanol should be fed into the last extraction stages.
The method may be carried out with equipment consisting of known or modified units extractors with separating and pressure-releasing means) from the oil industry. This equipment may be included in a production line and will permit continuous production.
The invention covers the post-treatment of the extraction residue with normal non-aqueous or aqueous solvents to obtain special lipids and proteins, such as cephalins or globuiins. The ethanol phase may further be distilled to recover dissolved compounds such as carbohydrates.
The used of ethanol as the extracting agent is not restricted to seeds. It can also be applied to compressed reeds, provided that the seed material is subjected to a preliminary treatment of complete inactivation of myrosase, e.g. by steeping it in boiling water, in order to avoid any decomposition of thioglycosides.
The method of the invention has a number of advantages over traditional processes. Thus it is possible for the first time to remove fat from and reduce the harmful substances in brassica and crambe seeds or processed products thereof, in a single stage of the process and with industrially realisable parameters obtaining (pressure, temperature, humidity), e.g. in special two stage revolving extractor under pressure, with the release of pressure taking place while the raw material is passing from the first to the second stage.
In this way it becomes possible to reduce processing and capital costs. The raw oil obtained by inactivation of lipid-decomposing enzymes (lipoxydase, lipase and phospholipase) and selective fractionation of polar and non-polar lipids (phosphatides, free fatty acids, triglycerides) corresponds to the semi-refined quality, and a considerable reduction in refining costs and improved hydrogenating behaviour can be expected of it. The extracted husk obtained as a by-product contains only small quantities of thioglycosides and decomposition products thereof and no toxic artefacts; its unrestricted use as a fodder component for monogastrides would provide a complete substitute, for example, for husk extracted from soya, which would have considerable effects on the importation of soya.Another factor is that there is only slight wastage of the material contained in the seeds which determines their value, as a result of the restricted water content of the ethanol. Furthermore, the proteins are denatured in such a way that certain functional properties, such as the solubility and precipitation behaviour of low molecular albumins, are equated with those of the globulin fraction, so that isolated or concentrated proteins can be obtained from the extracted husk in high yields and with good features from the point of view of nutrition physiology.
The invention will now be explained in greater detail with reference to the following examples.
Examples
Example 1
250 g rape seeds (ITC-content 0.45% in the fat-free dry material (i.f.d.), VTO-content 1.58% (i.f.d.), water content 7.3%) is dried to a water content of 1.5%, reduced to particle sizes between 2 and 4 mm, mixed with 375 g of 96% by vol. ethanol in a pressure autoclave and heated to 1 50C. An excess pressure of approximately 250 kPa (2.5 bars) is established and maintained for 1 5 mins.; the micell is thereupon separated at an approximately constant excess pressure, and the extraction residue saturated with alcohol is relieved of pressure by abruptly opening the autoclave. This process is followed by three further extraction cycles using a similar procedure, after which the solvent is removed from the residue.
The combined micell is cooled to a temperature of 100C, and three phases are formed. The bottom phase, in addition to 64% ethanol, contains mainly neutral lipids; the middle phase contains substances contained in the seeds, dissolved or dispersed in water; and the top, ethanol phase has an oil content of 3.4%. The top phase is re-cycled to each of the first two extraction stages, while fresh ethanol is fed into the third stage.The middle phase could possibly be treated separately (vaporisation), and the bottom phase distilled offThe end products have the following quality parameters:
Extracted husk: ITC-content 0.00%
VTO-content 0.06%
Extracted oil: acid number 0.64
pheophytin 15.0 ppm
phosphatides 10.4 ppm
unsaponifiable material 0.57%
sulphur-containing compounds 36.9 ppm
Example 2
250 g of compressed rape seeds obtained from thermally inactivated (conditioned) seeds (ITC content 0.38% (i.f.d.), VTO content 1.31% (i.f.d.), water content 3.0%) is mixed with 375 g absolute ethanol in a pressure autoclave and heated to 11 OOC. This sets up an excess pressure of approximately 200 kPa (2 bars), which is maintained for 20 mins.; the treatment is then continued as in Example 1.
The end products have the following quality parameters:
Extracted husk: ITC-content 0.02%
VTO-content 0.07%
Extracted oil: acid number 0.44
pheophytin 0.3 ppm
phosphatides 2.8 ppm
unsaponifiable material 0.49%
sulphur-containing compounds 51.9 ppm
Claims (8)
1. A method of treating vegetable raw materials containing thioglycoside for simultaneous fat removal and de-toxication, comprising extracting the raw material, after preliminary pre-crushing or thermal treatment, with ethanol boiling under superatmospheric pressure, separating the resulting oilcontaining micell while still under the superatmospheric pressure, and then rapidly relieving the pressure on the extraction residue.
2. A method as claimed in claim 1, in which the time taken to completely relieve the pressure on the extraction residue is from 1 to 10 seconds.
3. A method as claimed in claim 2, in which the said time is from 1 to 3 seconds.
4. A method as claimed in any one of claims 1 to 3, in which the water content of the entire system of raw material and alcohol does not exceed a limit of 15% or fall below a limit of 1%.
5. A method as claimed in any one of claims 1 to 4, in which the extraction is carried out with 96% ethanol, the water content of the dried seed material being < 3.0% water.
6. A method as claimed in any one of claims 1 to 5, in which the extraction is carried out at pressure of 40 to 250 kPa over atmospheric and with a residence time of 10 to 60 minutes per extraction cycle.
7. A method as claimed in claim 6, in which the extraction is carried out at pressure of 1 50 kPa over atmospheric and within a time of 1 5 to 30 minutes per extraction cycle.
8. A method of treating vegetable raw materials containing thioglycoside for simultaneous fat removal and detoxication after preliminary pre-crushing or thermal treatment, substantially as hereinbefore described with reference to the examples.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DD79216128A DD145925A1 (en) | 1979-10-10 | 1979-10-10 | METHOD FOR THE TREATMENT OF PLANT LIQUID OF THIOGLYCOSIDE-CONTAINING RAW MATERIALS |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB2060673A true GB2060673A (en) | 1981-05-07 |
| GB2060673B GB2060673B (en) | 1984-01-11 |
Family
ID=5520528
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB8032321A Expired GB2060673B (en) | 1979-10-10 | 1980-10-07 | Method of treating vegetable raw materials containing thioglycoside |
Country Status (6)
| Country | Link |
|---|---|
| BE (1) | BE885635A (en) |
| DD (1) | DD145925A1 (en) |
| DE (1) | DE3036316A1 (en) |
| GB (1) | GB2060673B (en) |
| IT (1) | IT1143038B (en) |
| PL (1) | PL126829B1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017041776A1 (en) | 2015-09-11 | 2017-03-16 | B+B Engineering Gmbh | Method of combined cell digestion and extraction of oil-containing seeds |
-
1979
- 1979-10-10 DD DD79216128A patent/DD145925A1/en not_active IP Right Cessation
-
1980
- 1980-09-26 DE DE19803036316 patent/DE3036316A1/en not_active Withdrawn
- 1980-10-07 GB GB8032321A patent/GB2060673B/en not_active Expired
- 1980-10-08 IT IT49850/80A patent/IT1143038B/en active
- 1980-10-10 PL PL1980227205A patent/PL126829B1/en unknown
- 1980-10-10 BE BE0/202408A patent/BE885635A/en not_active IP Right Cessation
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017041776A1 (en) | 2015-09-11 | 2017-03-16 | B+B Engineering Gmbh | Method of combined cell digestion and extraction of oil-containing seeds |
| US20190085261A1 (en) * | 2015-09-11 | 2019-03-21 | B+B Engineering Gmbh | Method for a combined cell digestion and extraction of oil-containing seeds |
| US10577558B2 (en) | 2015-09-11 | 2020-03-03 | B+B Engineering Gmbh | Method for a combined cell digestion and extraction of oil-containing seeds |
| RU2729822C2 (en) * | 2015-09-11 | 2020-08-12 | Б+Б Инжиниринг Гмбх | Method for combined destruction of cells and extraction of oil-containing seeds |
Also Published As
| Publication number | Publication date |
|---|---|
| BE885635A (en) | 1981-02-02 |
| PL126829B1 (en) | 1983-09-30 |
| IT8049850A0 (en) | 1980-10-08 |
| IT1143038B (en) | 1986-10-22 |
| DD145925A1 (en) | 1981-01-14 |
| PL227205A1 (en) | 1981-07-10 |
| GB2060673B (en) | 1984-01-11 |
| DE3036316A1 (en) | 1981-04-23 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PCNP | Patent ceased through non-payment of renewal fee |