April 30, 1946. E. LEVIN Re. 22,748 METHOD OF TREATING GRAIN GERM Original Filed Aug. 6, 1936

Reissued Apr. 30, 1946 Re. 22,748 UNITED STATES 22,748PATENT of FICE METHOD of TREATINGGBM CEREAL. GRAN. . . . Erra Levin, Monticello, u. . . . . original No. 2,314,2s2, dated March 16, 1943, Seria No. 94.09, August 8, 1938. Appeation m for reissue October 27, 1943, serial No. 50,866 19 Claims. (C. 99-80). This invention relates to a method of prepar bryo of grain, but it is also present in the ing anti-neuritic products of edible character, germ or of other cereal gr such as such as foods and medicines, and to the products , rye, corn and oats. Heretofore the anti obtained by such method of treatment. neuritic factor in cereal grain germs has been It is known that the so-called possess but slightly utilized due to the fact that germs various properties and are intimately concerned tend to turn rancid on standing. The present with the maintenance of bodily processes, and invention contemplates treating the various cereal thus are inseparably connected with the normal grain germs, and particularly the wheat germ physiology of the animal, including man. Thus and the corn germ, to render them palatable and it is commonly accepted that A functions 10 preservable, thus making the vitamin “B” read to prevent certain types of infections, because its ily available for use as a food or medicine. To absence from the diet results in inflammation of ...this end the oil in the cereal grain germs, particu the eyes, the growth of the animal ceases, and if larly wheat germ and corn germ, is extracted, the condition be not corrected, death usually leaving a wholesome and preservable product. results; the absence of from the diet is 5 Referring again to the cereal grains, it has been likely to result in scurvy and hemorrhages; the shown that exists abundantly in the absence of the vitamin known as water soluble, germ oil of these grains, particularly wheat, corn growth promoting, anti-neutritic vitamin is likely and oats. A further object of the present inven to result in pelagra and neuritis. The existence tion is to remove the oil from these grain germs of an anti-rachtic factor known as vitamin D, 20 without damaging the vitamin E content. whose function, is to preserve the normal depost A further object is to devise a method whereby tion of calcium in the bones, has been shown. cereal grain oil may be removed from the germ Also the existence of vitamin which is concerned without destroying the vitamin B in the new with the maintenance of the function of repro cereal product and to preserve the vitamin Econ duction, has been shown. 25 tent in the germ oil. The present invention is particularly concerned . The problem of how to treat cereal grain germs with the so-called anti-neuritic vitamin and the in such manner that the vitamin B content of the reproductive factor known as vitamin E. It has germs containing them, such as the germs of long been known that yeast contains an abun Wheat, barley, rye, corn and oats, is not destroyed, dance of the anti-neuritic factor. However, yeast 30 has been the subject of intensive and careful in is not we adapted for use in food or as medicine, vestigation but no thoroughly satisfactory solu because of its highly objectionable odor and taste. tion of the problem has heretofore been offered. It is known that the embryo of cereal grains con It has long been thought that the application of tain the anti-neuritic vitamin B1, or B as it is heat readily destroys the anti-neuritic factor... I called in the United States. What was formerly 35 have discovered that by extracting the oil from taken to be the Water soluble, growth-promoting, the grain germ, for example, from the wheat germ anti-neuritic vitamin is not an entity but is con and corn germ, in an acid condition the applica posed of at least seven different factors, among tion of heat during the treatment does not impair which are the anti-neuritic factor and the growth the vitamin B content of the product and the promoting and pelagra preventing factor and the 40, germ oil extracted may be employed as a source anti-paralytic factor B4 hereinafter described. of vitamin E. Moreover, it is possible in this op As yet a uniform terminology for the water solu eration to achieve these results without an ap ble vitamin has not been decided upon. British preciable solvent loss. biologists designate the anti-neuritic factor "Bi' This invention will be readily understood from and the growth promoting factor 'Ba' reserving 5 the following description and the accompanying 'B' to identify the complex of the two factors. drawing, which illustrates more or less diagram in the United States it has been suggested that matically an arrangement of extractor, vapor the term 'B' be restricted to designate the anti izer, condenser, and receiver, which has been neuritic factor and that the term "G" be used to found well suited to the practice of the inven denote the growth promoting factor. In the 50 tion. present application the American terminology Referring to the drawing, 4 indicates an ex will be employed and the term 'B' will be re tractor supporting a removable foraminous basket stricted to refer to the anti-neuritic factor with 5 adapted to contain the cereal germ to be treat which the present invention is concerned. ed, and open and closed steam coils designated The anti-neuritic factor is present in the em 55 by the numerals and 7, respectively, located

2 29,748 below the basket. An agitating device (inct means of the pipe, the condenser , and the wa shown) may be employed in the extractor if de ter separator. The last ends of the solvent are sired. The head 8 is securely fastened to the ex completely removed from the grain by a blast tractor by bolts or otherwise, in such manne of live steam which completely vaporizes the oc that it may be readily removed. 5 cluded solvent and whatever water may remain A vapor pipe 9 provided with a valve O leads in the extractor. The water is separated and from the top of the extractor to the upper end withdrawn from the system. of the water-cooled coll of a condenser fl; and The grain germ undergoing treatment, for ex

from the bottom of the coil leads through a sepa ample, wheat germ or corn germ, may be dried in rator 2, a pipe 3 for conducting the condensed O the extractor before removal by the addition of an solvent to a receiver 4 supported in an elevated airline. The solvent collecting in the still is com position above the extractor when supplied with pletely vaporized by the application of additional a vent is for releasing uncondensible gases. closed steam, finishing up with live steam. After At B is shown, leading from the top of the the solvent has been vaporized and more or less separator 2, a valve drain for drawing of the 5 completely passed out of the still, the oil is re watery product of condensation. From the bot moved from the still through the withdrawfall tom of the receiver a pipe T equipped with a line. I prefer to operate my process in a closed shut-off valve leads to the bottom of the ex system in order that the vitamin E in the gerin tractor. oil may not be subjected to oxidation. From the top of the extractor a pipe pro 20 After the Withdrawal of the grain germ and the vided with a check valve 20 and control valve germ oil, the solvent is concentrated in the 2 leads to a vaporizer 22 supported in upright receiver and the apparatus is ready to receive position and having rounded top and bottom. At another charge of grain germ. After extraction, 23 and 24 are shown, respectively, open and the grain germ, such as the wheat germ or cors. closed steam coils preferably located in the bot 25 germ, is light, dry and of a floury consistency tom of the still. A draw-off line for the oil is and has been found to have a high , pro indicated at 25. tein, and water-soluble vitamin content. Among The vapor line 26 leads from the top of the va other things, it is adapted to be used as a supple porizer to the upper end of the water-cooled coil ment to cereal foods, as a liquid extract contain of a condenser f' which is similar in construc 30 ing vitamin B, and may be employed in baking as tion to the condenser f. In like fashion the low a supplement to . The extracted germ oil is er end of the condenser coil leads into the receiv er 4 after passing through the separator f' so a valuable product in that it is rich in vitaxi equipped with a water drain f'. It is preferred that the steaming process in A drain pipe 2, provided with a control valve the extractor be operated under a substantial 2B, is tapped into the bottom of the extractor sub-atmospheric pressure. The degree of vacuum and forms a connection with the pipe 9. will vary during the process according to the sol The operation of this apparatus is as follows: vent used, but it is preferred that the vacuum A charge of cereal grain germ, for example, be such that the temperature in the extractor wheat germ or corn germ, from which it is de 40 does not exceed 160 F. and does not fall below sired to remove a maximum quantity of oil, is 125 F. This temperature range is particularly placed in the foraminous basket and introduced important where the product is to be used as a into the extractor and the head bolted down. flour or in connection with baking. The wheat The solvent is then allowed to flow from the re germ contains a proteolytic enzyme presumably ceiver into the extractor until it is just well be protease, which unless destroyed attacks the low the level of the pipe D. Stean is turned 45 of the flour and causes hard and unsatis on in the closed steam coil and the mixture of factory baked products. This enzyme is not de solvent and grain germ heated. It is desirable stroyed by the extraction temperature even up to to maintain a temperature in the extractor some temperatures of 170 F., presumably because of what below the boiling point of the solvent, pref the absence of moisture. However, in the pres erably below 170 F. The oil readily dissolves in 50 ence of steam the enzyme can be destroyed at the hot solvent and the light solution rises to the the lower temperatures designated. top of the extractor and overflows through the In operating the vacuum extraction the pressure line 9 past the check valve O into the still. As is held at the desired point to give the desired the oil in solution passes out at the top of the temperature until the temperature starts to rise extractor, additional solvent flows in the bot upon substantial elimination of the solvent. At tom. Cereal grain germ, exemplified by wheat that point the pressure is lowered and live steam germ or Corn gerin, contains varying amounts of introduced at approximately the same tempera water, and a solvent having a specific gravity ture range. This operation is then continued un heavier than water is particularly helpful in dis til the product is solvent free. placing water from the germ. 60 By the term 'solvent free' as used herein it is in operation, the still is maintained at ten meant that the product is palatable and shows no peratures higher than the boiling point of the trace of solvent as distinguished by taste or odor. solvent, and when the solution of solvent and oil Where it is not desirable to destroy the proteo enters the still, the solvent is vaporized. The lytic enzyme, temperatures or other conditions check valve prevents the vapors from back-flow 65 may be employed which will preserve the enzyme. ing into the extractor and they rise through pipe Of course, when a vacuum is employed 3 vacuum 2, are condensed in f', and flow into the re pump is added to the apparatus shown in the ceiver, to be put through the system again. drawing. When a maximum amount of oil has been ex As is readily seen, my process is a batch opera tracted and is completely in solution, the liquid 70 tion in a closed system, and has only an imper contents of the extractor are withdrawn through ceptible solvent loss. the drain 2. The valves are then closed and ad While ethylene dichloride is a preferred sol ditional steam applied in the closed steam coil, vent, any petroleum hydrocarbon solvent boiling vaporizing the solvent clinging to the grain below 120° C. and carbon disulfide are suitable germ, returning the solvent to the receiver by 75 for my purpose, if a weak acid is added to the

22,748 3. solvent to maintain an acid condition in the 9 paired and in the same condition as in the nat tractor. It is important that an acid condition ural germ. be maintained during the extraction. The fore 2. The process of making a finished stable, going solvents are inflammable and consequently marketable, non-toxic and palatable dry food particularly desire to employ the various ho product, consisting in extracting from natural rine derivatives of ethane such as dichloroethyl grain germ all of the oil with a heated solvent ene, trichlorol-ethylene, perchlorol-ethylene, therefore at a temperature and acidity to main tetrachlorol-ethane, and Pentachlorol-ethane. tain the vitamin B content unimpaired, and sub These solvents tend to hydrolyze when contacted sequently completely removing the solvent from with the moisture-containing cereal grain Bern O the germl. and it is not necessary to add acid when they are 3. The method as set forth in claim 2 in which employed. It is apparent that the solvent will be the solvent is removed from the germ under sub hydrolyzed from the beginning of the extraction atmospheric pressure and at a temperature of until the solvent is drawn of, that is, from the the order of 125 to 160 F, time the solvent contacts the moisture in the 4. The method as set forth in claim 2 in which grain germ until it is driven of with steam. Ex the solvent is ethylene dichloride. cellent results have also been obtained with car 5. The process of making a finished stable, bon tetrachloride. dry, marketable non-toxic and palatable food The hydrolysis of such a solvent as ethylene dil product consisting of extracting from natural chloride is of material assistance in removing the grain germ all of the oil with a heated solvent of last traces of solvent during the steaming opera the class consisting of chlorine derivatives of tion. the lower molecular weight parafins and sub The treated wheat germs are preferably not sequently completely removing the solvent from completely freed from oil but enough of the oil the germ at a temperature and acidity to main is retained so that the material will not become tain the vitamin B and vitamin B content unin rancid or unpalatable. Inasmuch as the oil con paired. tains some vitamin E and A the retention of it 6. The method as set forth in claim 5 in which in palatable quantitles is desirable. the removal of solvent is accomplished with the The above treatment also may be employed to aid of steam, whereby the solvent is partially adjust the moisture content of the wheat germ. 30 hydrolyzed. In all cases the finished product is thoroughly . A finished stable, marketable, palatable, dry and contains less than 10% of moisture, nor dry food product consisting of wheat germ sub mally about 7%. stantially freed from oil and having substan In some instances, it has been found desirable tially the vitamin B and vitamin B potency of to employ the entire grain as a charge. In the original germ. this case, it is desirable to grind the grain seed 8. The method of treating grain germ to ex before it is inserted in the extractor. tract therefrom substantially all of the oil which The treatment hereinbefore described, when comprises extracting from grain germ substan employed with the preferred solvents, and par tially all of the oll with a heated hydrolyzing ticularly with ethylene di-chloride, extracts the 40 Solvent to form an acid under the conditions of oil from the wheat germ without damaging the the extraction, removing the majority of the sol vitamin B content thereof. This vitamin is vent by drainage, and removing the last traces found in liver and also in wheat germ and is of of solvent in the presence of heated moisture, great value in the treatment of pernicious ane wherein the solvent is hydrolyzed to an acid, nia. When the oil of the wheat germ is ex whereby the entire extraction process is carried tracted with hexane, ether or acetone, the vita Out in an acid environment. min B is dissolved out and lost, whereas in the 9. The method of treating grain germ to ex present method of procedure the vitamin B4 is tract therefrom substantially all of the oil with retained and the finished dry product is as high out affecting its vitamin content, which com as, or higher, in the vitamin than liver. prises extracting from grain germ substantially While I have described in considerable. detail all of the oil with a heated solvent which has the specific form of apparatus which I find well hydrolyzed to form an acid, removing the ma adapted to the carrying out of my process, as jority of the solvent by drainage, and removing well as the details of the particular commercial the last traces of solvent in the presence of process in accordance with the invention, it will heated moisture and under a vacuum at a tem be understood that this is illustrative only and perature substantially below the boiling point of for the purpose of making clear the nature and water, the grain being maintained in an acid mode of applying the invention and that the condition during the entire extraction process. invention is not to be regarded as limited in scope 10. A food product comprising a finished, sta to the illustrative details given, except insofar as ble, marketable, non-toxic, dry, palatable grain such limitation is included within the terms of germ material, substantially free from the oily the accompanying claims, in which it is my in constituents of the grain germ and having the tention to claim all novelty inherent in my inven remaining constituents thereof in unimpared tion as broadly as possible in view of the prior form and having substantially the vitamin B art. potency of the original germ. This application is a continuation-in-part of 11. The method of treating grain germ to ex my copending application, Serial No. 683,085, tract therefrom substantially all of the oil with filled July 31, 1933. out affecting the vitamin content which comprises What I regard as new and desire to secure by extracting from grain germ substantially all of Letters Patent is: 70 the oil with a heated solvent under acid condi 1. A finished stable, marketable, non-toxic and tions and at a temperature above 125 F. and be palatable dry food product with a high content low 160 F, removing the majority of the solvent of vitamin B, consisting of all the constituents by drainage, removing the last traces of solvent of natural grain germ except the oily constit in the presence of heated moisture at a tempera uents thereof and with such constituents unim 7s ture between 125 F. and 160° F, whereby the

4. 99,748 protease in the grain is destroyed, the acid con stantially protease free dry food product having ditions being maintained during the entire ex a high content of vitamin B consisting of all of traction process. the constituents of natural wheat germ except 12. A finished stable, marketable, non-toxic the oily constituents thereof. and palatable, substantially protease-free dry 15. The process as in claim 2 wherein the food product having a high content of vitamin natural grain germ undergoing processing is B, consisting of all of the constituents of nat wheat germ. ural grain germ except the oily constituents 16. The process as in claim 5, wherein the thereof. . natural grain germ undergoing processing is 13. A flour comprising a finished stable, mar 10 wheat germ. ketable, palatable, non-toxic, substantially pro 17. The method as in claim 8, wherein the tease-free food product, having a high content grain germ undergoing treatment is wheat germ. of vitamin B, consisting of all of the constituents 18. The method as in clan 9, wherein the of natural grain germ except the oily constituents grain germ undergoing treatment is wheat germ. thereof. 14. A food product adapted to be used as a 15, 19. The method as in claim 11 wherein the supplement to cereal foods comprising a finished, grain germ undergoing treatment is wheat germ. stable, marketable, non-toxic and palatable, sub aRA. W. N.