Method for the separation of rapeseed germ and rapeseed germ oil

The purpose of the present invention is to efficiently separate and utilize the rapeseed germ. The present invention relates to a method for the production of a fraction containing a rapeseed germ as a main component, comprising crushing a rapeseed and separating said fraction. One of the specific products derived from rapeseed germ is the oil and fat prepared by extraction or expression of the rapeseed germ.

TECHNICAL FIELD
 The invention relates to a method for the production of rapeseed germ, to
 oil and fat, and protein composition prepared from the rapeseed germ thus
 produced.
 BACKGROUND ART
 A huge amount of rapeseeds that are used as oil seeds is mainly imported
 from abroad.
 A rapeseed contains approximately 40-45 wt % of oil, which is the highest
 ratio among those of oil seeds including soybean, sesame and the like. For
 that reason, mechanical expression of the rapeseed can be easily carried
 out, and the rapeseed is a very useful material for vegetable food oil and
 fat.
 A rapeseed oil is usually produced by first flaking the rapeseed, then
 subjecting the flaked rapeseed to a heat treatment, and finally expressing
 it by means of an expressing machine named an "expeller" so as to obtain
 about 1/2-3/4 of the total oil contained in the rapeseed. The oil
 remaining in an expression cake, i.e., the cake obtained in the expression
 process, is then extracted with n-hexane.
 The oil that is obtained by the expression process (referred to as
 "expression oil" hereinafter) and the oil that is obtained by the
 extraction process (referred to as "extraction oil" hereinafter) are
 combined and purified to give the rapeseed oil.
 On the other hand, after being separated from the solvent, an extraction
 cake that is obtained in the extraction process is utilized mainly as
 fertilizer or feed. However, as these by-products other than oil is sold
 at a very low price, it has been desired to more effectively utilize the
 above by-products.
 For example, it has been tried to increase a protein content by removing a
 hull from the rapeseed, or to increase a value of the extraction cake as
 feed by removing bitterness components such as tannin from it with water
 or an organic solvent.
 Like the other oil seeds, the rapeseed consists of a cotyledon, a hull and
 a germ. The germs of the oil seeds other than the rapeseed, such as those
 of soybean, wheat, rice, corn and the like have already been actually
 utilized.
 On the other hand, since the germ of a relatively small oil seed such as
 the rapeseed (ca. 1.9 mm in diameter) is very small (ca. 1.5 mm in length
 and ca. 0.5 mm in diameter), when compared with that of corn (ca.8 mm in
 length, ca.3 mm in width, and ca.2 mm in thickness), an attention has been
 hardly made to the rapeseed germ and no try has been made to separate and
 utilize a fraction of the rapeseed that has a high germ content.
 The investigation of the present inventors has revealed that the ratio of
 the germ content in the rapeseed is approximately 12 wt %, which is much
 higher than that of soybean (ca.2-3 wt %).
 It is therefore expected that an efficient separation and recovery of the
 rapeseed germ in an industrial scale could expand its utility.
 For the purpose of efficiently separating and utilizing the rapeseed germ,
 the present inventors have studied and found that not only the hull but
 also the germ can be peeled off from the cotyledon during the crushing
 process of the gains of the rapeseed under compact stress so as to
 efficiently separate a fraction containing its germ as a main component.
 It is also revealed that the thus separated fraction has such a higher
 germ content as about 95 wt % at maximum than that of the soybean (75 wt %
 at maximum).
 DISCLOSURE OF THE INVENTION
 The present invention relates to a method for the production of a fraction
 containing a rapeseed germ as a main component, comprising crushing a
 rapeseed and separating said fraction.
 The present invention further relates to oil and fat, defatted cake, and
 protein composition that are prepared from a material containing the
 rapeseed germ as a main component. Said fraction prepared according to the
 present invention may be used as the above material.
 BEST MODE FOR CARRYING OUT THE INVENTION
 The present invention will be further described in more detail.
 Before being subjected to the present method, grains of the rapeseed may be
 treated by means of washing with water, sieving-out, magnetism, suspension
 selection, and the like in order to optionally remove foreign substances
 such as grains of sand, metals, and small stones. Any variety of the
 rapeseed species may be used in the present invention.
 The rapeseed may be crushed by any method known in the art without any
 limitation with respect to its principle or mechanism, making use of, for
 example, compressive stress, impact stress, shearing stress, and friction.
 For instance, an impact stress-type crusher may be used in the present
 invention in which a centrifugal force is applied to materials to be
 crushed by a disc rotting at a high speed, so that said materials will
 collide with baffles or pins provided in the crusher or on the wall of it.
 Alternatively, a pin mill-type crusher may be used in the present
 invention.
 The impact stress-type crusher includes an entrainment-type, a hammer
 mill-type, a roller mill-type, etc., and any type of which may be used in
 the present invention.
 The "crushing" means in this specification to break larger gains into
 smaller ones, including crude crushing, medium crushing, fine crushing and
 the like, depending on the size of the thus crushed grains. The degree of
 crushing may be optionally controlled by those skilled in the art. It is
 desirable in terms of yield that the germ is effectively peeled off from
 the cotyledon while substantially keeping its original size in the
 crushing process.
 Prior to the crushing, the rapeseeds may be subjected to a heat or drying
 treatment.
 The separation process may be carried out by any means known in the art
 without any limitation with respect to its principle or mechanism. For
 example, the separation may be done by making use of difference in the
 specific gravity such as sorting with air or under flow, or by using a
 sieve. The conditions in the separation process may be optionally
 determined by those skilled in the art depending on the means adopted in
 this process.
 The separation process may be efficiently performed by removing the hulls
 and fine fractionicles with a vibrating fluidized bed, a light-fraction
 sucking apparatus and the like prior the separation process of the crushed
 rapeseeds.
 The fraction separated according to the present invention, which may be
 also named a "germ fraction", contains as a main component the rapeseed
 germ of at least 38 wt %, preferably 75 wt % or more, more preferably 95
 wt % or more.
 The germ fraction may be obtained by separating the crushed rapeseed into a
 fraction of 16 mesh or less (1 mm or less), 20 mesh (850 .mu.m or less),
 or 24-32 mesh (710 .mu.m-500.mu.m) with a sieve, for example.
 The oil and fat, defatted cake, and protein composition according to the
 present invention are prepared from a material containing the rapeseed
 germ as a main component. The material contains at least 38 wt %,
 preferably 75 wt %, more preferably 95 wt % or more for the germ. Although
 the germ fraction prepared according to the present invention may be used
 as the above material, other materials obtained by any other methods than
 the above separation process may be used as well.
 The oil and fat according to the present invention has a lower chlorophyll
 content (ca.10 ppm or less) and a lower content of an eluted phosphorous
 component (ca. 450 ppm or less) than those contained in the rapeseed oil.
 Furthermore, it has a low a content of oil-soluble metals of Mg (ca.70 ppm
 or less) and Ca (ca.120 ppm or less). As a result, it will be easy to
 further purify the present oil and fat by removing the eluted phosphorous
 component, and the phosphorous content in a drain will advantageously low
 from an environmental point of view as well.
 Since the oil and fat according to the present invention has a total
 phytosterol content of 1000 mg/100 g or more and .beta.-sitosterol content
 of 500 mg/100 g or more, it is expected to show a reducing effect of
 cholesterol in the body.
 As shown by the contents of palmitic acid of 6 wt % or more and linolenic
 acid of 8.5 wt % or less, the oil and fat according to the present
 invention has a high saturated fatty acid content and a low unsaturated
 acid content. As a result, it is more stable against oxidization than the
 conventional rapeseed oil.
 The oil and fat according to the present invention are prepared from the
 material containing the rapeseed germ as a main component by the
 conventional expressing techniques.
 For example, the rapeseed germ is subjected to an oil expressing machine to
 give the expressed oil. Before the expression, the rapeseed germ may be
 heated or its water content may be adjusted appropriately. Furthermore,
 before expression or extraction, it may be subjected to various treatments
 such as flaking, expression with an expander and the like, puffing, and
 roasting.
 On the other hand, the extraction oil is obtained by extracting the
 expression cake with an appropriate solvent such as an organic solvent
 including n-hexane, water, a mixture of water and the organic solvent or
 critical fluid, followed by the concentration of the resulting oil. The
 expression oil and the extraction oil are combined to yield a rapeseed
 germ oil that is the oil and fat according to the present invention.
 The rapeseed germ oil according to the present invention includes also the
 above expression oil and the extraction oil.
 The solvent is removed from the cake obtained in the above expression or
 extraction process by any known methods to give the defatted cake
 according to the present invention.
 The expression cake, defatted cake and protein composition that are
 obtained by the present invention are utilized as materials in various
 applications such as food, fertilizer and feed.
 The present invention will be further described in more detail by referring
 to the following examples, which should not be construed to limit the
 scope of the present invention.
 In the following examples, a water content, an oil content and a T-N
 content are determined by a heat and dry method in accordance with a
 standard oil analysis test (Japan Oil and Fat Chemistry Association), an
 ether extraction method in accordance with the same standard test, and
 Kjeldahl method using KJELTEC AUTO 1030 Analyzer, respectively.

EXAMPLE 1
 The grains of a rapeseed were crudely crushed by using as a crushing
 apparatus "DEHULLING MACHINE TYPE CZ1000" manufactured by TECMACHINE CO.
 (in France) at a rotation rate of 2,800-3,000 rpm and a material feed rate
 of 700-1,000 kg/h.
 The resulting hull and fine fractionicles were then removed from the thus
 crushed rapeseed consisting of the separated hull, germ and fine
 fractionicles by using as a vibrating fluidized bed (a separation taper)
 "FLUID BED SORTER TYPE TLF500" manufactured by TECMACHINE CO. (in France)
 and a light-fraction sucking apparatus.
 Finally, each fraction of 16 mesh (1 mm) or less was separated with a
 sieve, and the composition and yield of each fraction were determined. The
 results are summarized in TABLE 1.
 TABLE 1
 16 mesh 24-32mesh
 (1 mm) or 20 mesh (850 .mu.m (710-
 part less mm) or less 500 .mu.m)
 Germ 38% 76% 95%
 Cotyledon 48% 19% 3%
 Contaminants 14% 4% 1%
 Yield 29% 18% 10%
 The yield of the germ contained in a fraction of 24-32 mesh (710-500 .mu.m)
 was about 83% of a theoretical one.
 The components of the germ contained in each resulting fraction of 16 mesh
 (1 mm) or less, 20 mesh (850 .mu.m mm) or less, and 24-32 mesh (710-500
 .mu.m), and those of the rapeseed (control) were analyzed. The results are
 shown in TABLE 2.
 TABLE 2
 T-N content
 Germ Water Oil T-N in an anhydrous
 Extraction
 Material Content % Content % Content % Content % oil product
 Oil AV
 Rapeseed* Germ 95 5.8 36.9 4.5 8.0
 0.6
 the same as above 76 5.9 38.2 4.4 7.9
 0.3
 the same as above 38 6.3 42.0 3.8 7.4
 0.5
 Rapeseed Oil 12 6.3-6.7 43-45 3.4-3.6 7.4-6.8
 --
 *determined by the present inventors
 As seen from TABLE 2, the rapeseed germ contained in the fraction of 24-32
 mesh has such a high oil content as about 37 wt % that is comparable to
 that in the rapeseed cotyledon (ca. 40 wt %), and it is therefore very
 useful as oil source.
 Furthermore, because the rapeseed germ contained in the fraction of
 24-32mesh has a high protein content ("T-N content".times.6.25) of about
 28 wt %, and a high T-N content in an anhydrous oil product (ca. 50 wt %),
 it is also very useful as protein source.
 EXAMPLE 2
 The expression oil was prepared by expressing the germ contained in each
 fraction of 16 mesh (1 mm) or less, 20 mesh (850 .mu.m mm) or less, and
 24-32 mesh (710-500 .mu.m) obtained in EXAMPLE 1 with an expeller
 apparatus (manufactured by SUEHIRO EPM CO.). On the other hand, the
 extraction oil was prepared by extracting the resulting expression cake
 with n-hexane, followed by pooling and purification. The expression oil
 and the extraction oil were then combined to give the rapeseed germ oil
 that is the oil and fat according to the present invention.
 The analytical results of the resulting rapeseed germ oil are shown in
 TABLE 3, in which "AV" and "POV" mean acid value and peroxide value,
 respectively.
 TABLE 3
 Germ POV Chlorophyll Phosphorous Ca
 Mg Fe Iodine
 Content AV (Meq/Kg) (ppm) (ppm) (ppm)
 (ppm) (ppm) Value
 95% Rapeseed* Germ Oil 0.8 2.4 2.9 190.0 18.9
 12.4 1.2 109
 76% the same as above 1.0 1.0 3.0 211.0 20.3
 16.3 1.2 109
 38% the same as above 1.3 0.6 10.1 451.0 121.1
 70.2 1.8 111
 12% Rapeseed Oil 2.6 0.4 12.4 525.0 203.1
 105.1 3.1 113
 *determined by the present inventors
 The rapeseed germ oil prepared from the rapeseed germ of 24-32 mesh
 (710-500 .mu.m) has a lower chlorophyll content (ca.3 ppm) and a lower
 content of the eluted phosphorous component (ca. 190 ppm)than those
 contained in the rapeseed oil. Further, it has a low content of
 oil-soluble metals of Mg (ca.12 ppm) and Ca (ca.19 ppm). Consequently, it
 will be easy to further purify the present rapeseed germ oil by removing
 the eluted phosphorous component, and as the phosphorous content in a
 drain will be low, which is preferable from an environmental point of view
 as well.
 The chlorophyll content was determined by an absorbance method, and the
 contents of phosphor, magnesium and calcium were determined by ICP
 analysis. The fatty acid compositions of the resulting rapeseed germ oils
 are shown in TABLE 4.
 TABLE 4
 Palmitic Palmitoleic Stearic Oleic Linoleic
 Linolenic Arachidic Eicosenic
 Germ Acid Acid Acid Acid Acid
 Acid Acid Acid
 Content Fatty acid 16:0 16:1 18:0 18:1 18:2
 18:3 20:0 20:1
 95% Rapeseed* Germ Oil 12.0 0.7 2.9 56.8 21.4
 5.3 0.5 0.4
 76% the same as above 10.1 0.8 2.0 57.9 23.3
 5.4 0 0.5
 38% the same as above 6.0 0.8 1.3 60.2 22.6
 8.1 0 1.0
 12% Rapeseed Oil 1-4 0-1 0-2 55-63 18-25
 7-11 0 1-2
 *determined by the present inventors
 As shown by TABLE 4, since the rapeseed germ oil prepared from the rapeseed
 germ of 24-32 mesh (710-500 .mu.m) contains the saturated acid (palmitic
 acid (16:0)) of three times or more (about 12 wt % or more) than the
 rapeseed, while it contains the unsaturated acid (linolenic acid (18:3))
 of about half (about 5.3 wt %) of the rapeseed oil, it has an advantageous
 stability against oxidization.
 The fatty acid contents were determined by methyl esterification-gas
 chromatography in accordance with the standard oil analysis test.
 EXAMPLE 3
 A total and each phytosterol content of the rapeseed germ oil of EXAMPLE 2
 and the rapeseed oil were determined with thin-layer chromatography and
 gas chromatography in accordance with the standard oil analysis test.
 There results are summarized in TABLE 5.
 TABLE 5
 Rapeseed
 Rapeseed Germ Oil Oil
 95% 76% 38% 12%
 Germ Content mg/100 g mg/100 g mg/100 g mg/100 g
 Total 2100 1823 1021 771
 Sterols
 Brassica 140 144 110 102
 sterol
 campesterol 672 585 327 246
 .beta.- 1190 1010 572 386
 sitosterol
 Isofuco 95 84 49 37
 sterol
 The rapeseed germ oil prepared from the rapeseed germ of 24-32 mesh
 (710-500 .mu.m) has the total phytosterol content of about 2,100 mg/100 g
 and the .beta.-sitosterol content of 1,200 mg/100 g, that are about 2.7
 times and three times as much as those of the rapeseed oil, respectively.
 The present rapeseed germ oil is therefore useful as a natural oil having
 a reducing effect of cholesterol in the body.
 EXAMPLE 4
 The defatted rapeseed germ (100 g) obtained during the expression process
 of EXAMPLE 2 was mixed with 1 L of water and extracted with stirring for
 30 min at 50.degree. C. After removal of insoluble materials by
 centrifugation, the extract solution was adjusted to pH 4.5 so as to
 precipitate protein. The resulting precipitate was centrifuged and
 suspended into water, which was then adjusted to pH 7 in order to dissolve
 the precipitate. The resulting solution was then spray dried or
 lyophilized to give 35 g of protein derived from the rapeseed germ.