IL34205A - Autolysis product of fish and other ichthyological substances and process for its manufacture - Google Patents

Description

Autolysis product of fish and other ichthyologlcal substances and process for its manufacture GEORGES LAMOTTE C:-32514 34205/2 This invention relates to a process for the manufacture of an autolysis product of fish and/or other ichthyological substances (especially crustaceans), and to the said product* Α^.-, Numerous processes for the autolysis of protein substances of fish and the like are already known. However, the conventional processes generally require a very long time to carry out, lead to products which are not constant in quality, and. give relatively low yields because the autolysis is carried to the ammonia stage, with the formation of urea and of ammonia0 Some recent processes are relatively rapid but require the use of antiseptics which are not permitted in human foodstuffs, or are too severe and, whilst yielding free amino acids, destroy all the biological principles which exist in the starting material.

The present invention makes it possible to remedy this disadvantage* It is also known from U.S. Patent Specification 2,560,011 to produce fish meal by treating whole raw fish and/or fish waste with warm water, acidulated to a pH of 3-3·5 by addition of a water soluble acid, at a temperature of about 50 - 80°C for a period of time of half an hour or less than one hour or more, separating the solid residue and drying it. From the filtrate fish glue an4 pure proteins (98% purity) may be recovered by vacuum evaporation or other known means, j 34205/2 f The present Invention consists in a process for the manufacture of an autolysis product of fish and/or other ichthyologlcal substances, which comprises subjecting fish entrails or a mixture of fish and fish entrails and/or other ichthyologioal substances in the ground state to autolysis at an initial pH of at least 4, at sta- ambient temperature or at a temperature not exceeding 60°C, with gentle stirring, stopping the autolysis when the pH has reached about 6.5 and separating the autolysis product formed from the resulting mixture. Known acidic autolysing agents may be used, especially hydrochloric or acetic acid. Preferably the autolysis is carried out at * 0°-60°0., and it may be stopped by allowing the material to cool. The autolysis product may for example be separated from the other materials present by filtration or centrifuging and the residue may, in part or as a whole, be recycled to the autolysis stage .

In this process, the autolysis proceeds rapidly but gently and only to the stage of free aminoacids, and the autolysis product obtained contains not only free aminoacids and possibly a small amount of polypeptides, but also practically all the biological principles existing in the starting material (such as growth factors, the undt factor, the Fischer factor, auxins and the like). On the other hand it does not contain ammoniacal nitrogen.

The autolysis is preferably carried out under an atmosphere of an inert gas, especially carbon dioxide, so as to avoid any contact with air.

Terpenes, especially terpenes extracted from lemon, orange or pineapple juice, may with advantage be added to the material to be autolysed, both as an accelerator of the autolysis and as an antioxidant.

The autolysis product is separated as an aqueous solution, which preferably is concentrated in vacuo at a temperature not exceeding 60°C. until a paste is obtained, or is dried under the same conditions until a powder is obtained.

In one preferred embodiment of the invention, the material to be autolysed is finely ground, its pH is adjusted to about 5 by means of dilute hydrochloric acid or acetic acid, the temperature of the ground material is rapidly raised to about 55°C« under a carbon dioxide atmosphere, this temperature is maintained until the pH has reached about 6.5» and the liquid autolysis product is then separated and the residue recycled to the autolysis stage .

The invention is illustrated by the following Examples:- EXAMPLE 1 1 ton of a mixture of fish entrails and fresh thin fish (for example 20 of entrails and 80% of fish) is finely chopped in a screw grinder.

About litres of concentrated hydrochloric acid diluted with its own weight of water (about litres) is added to the finely ground material to adjust the pH of the mixture to about 5.

This mixture is placed in an autolysis trough made of stainless steel and having a double wall for heating purposes, and is rapidly raised to a temperature of about 55°C. whilst stirring gently to equalise the temperature. The mixture is kept at this temperature, and an atmosphere of carbon dioxide is established in the trough to avoid any contact with air. The course of the autolysis is thus favoured whilst suppressing any danger of putrid fermentation.

The mixture is gently stirred every half hour.

The rise in the pH of the mixture is carefully observed, and when this pH has reached about 6.5 (after 3 to 4- hours' heating) the autolysis is stopped by discontinuing the heating. 600 to 650 litres of a limpid amber-coloured liquid autolysis product, freed of oil and containing the aminoacids and the biological principles, is isolated by centrifuging, and the residual paste containing insoluble polypeptides and undigested material is recycled, after readjusting the pH to about 5> into the autolysis trough, with the addition of entrails and fish to make up a new charge of one ton, as described above.

The liquid autolysis product is obtained in a yield of about 60 to 6 by weight relative to the raw material, and contains about 2% of solids of which about 90% is aminoacids.

This liquid autolysis product can be used as such or concentrated to give a paste or powder which is naturally stable on storage (i.e. without preservative). Thus, a naturally stable paste containing 4-0% of water was obtained by treating the liquid autolysis product in a vacuum concentrator at a temperature of 60°C, as also, using a vacuum drier at the same temperature, was a powder containing 3 of water (by weight). The powder is entirely soluble in water and can be stored perfectly (with neither preservative nor antiseptic); it consists essentially of free aminoacids (in an amount corresponding to 98% by weight of the nitrogen-containing product and to 78% by weight of the powder) , biological principles existing in the starting material (such as growth factors, the undt factor, the Fischer factor, auxins and the like) and small amounts of soluble polypeptides, but is free from ammoniacal nitrogen.

The composition of the aminoacids is as follows: % of total aminoacids Alanine 9.6 Valine 6.8 Iso-leucine 9.4 Glycine 5.9 Leucine 10.2 Threonine 4.3 Proline 4- Serine 6.1 Cysteine 0.9 Methionine 2.9 Phenylalanine 4.8 Aspartic acid 10.7 Glutamic acid 16.1 Tyrosine 0.4 Lysine 5.4 Arginine 1.0 Histidine 0.7 Cystine 0.8 EXAMPLE 2 The process described in Example 1 is repeated, except that the starting material is more coarsely ground material and is acidified to about pH 4.5, and that before raising the temperature, terpenes extracted from lemon or orange essence or pineapple juice are added at the rate of 1 litre per ton of mixture , to act simultaneously as an antioxidant and as an accelerator of the autolysis.

Essentially the same results as in Example 1 are obtained, though starting from a coarser material.

EXAMPLE 3 The process described in Example 1 is repeated up to the end of the autolysis stage. The autolysis is stopped by discontinuing the heating. The contents of the autolysis trough are passed onto a very fine stainless steel sieve of mesh aperture 0.3 mm., the liquid collected is passed onto a vacuum drier kept at 60°C, and a total autolysis product is obtained in the form of a powder comprising about 3% of water and, apart from the aminoacids, containing a very small amount of soluble polypeptides.

The yield is about 20o by weight relative to the starting material .

The autolysis product obtained according to the invention is of special value in human dietetics for treating cases of deficiency (especially hepatic deficiency) and of malnutrition, for improving nitrogen-containing diets and also as a growth factor and as ah activator of biological processes in animal feedstuffs.

Comparative tests carried out on the growth of rats (3 batches of 4- young rats, aged 2 months) were undertaken to determine the respective effect of aminoacids ingested alone , and of the fish autolysis product obtained in Example 1, in comparison and measured relationship to casein.

The first batch received a normal ration plus 1 g. of casein, the second batch a mixture of aminoacids which reproduced the formula of the autolysis product, and the third batch a normal ration plus 0.023 g. of autolysis product. The results are given in the graph of the accompanying Drawing, which shows the weight curves of the tested animals in grams (as the ordinates) as a function of the time in days (as the abscissae). Whilst the rats of the second batch, having received pure aminoacids (curve No. 2) show a slight increase in weight relative to the normal development of the young rats of the first batch (curve No. 1), the ingestion of the corresponding amount of these aminoacids in the form of an autolysis product produces an increase in weight of 38.2% in the rats of the third batch (curve No. 3)· The difference in favour of the autolysis product is presumably due to the presence of various soluble enzymes and of certain factors (e.g. Kundt, Fischer) which have a vigorous effect on the nitrogen metabolism.

It can furthermore be seen from curve No. 3 that discontinuing the autolysis product for ten days (portion AB of this curve) led to a marked slowing down in growth, which resumed immediately when the administration of the daily dose of autolysis product was resumed.

If this interruption had not taken place, the increase in weight of the tested rats would have been more than 50% of the weight of the comparison animals „

Claims (14)

I CLAIM:

1. Process for the manufacture of an autolysis product of fish and/or other ichthyological substances, which comprises subjecting fish entrails or a mixture of fish and fish entrails and/or other ichthyological substances in the ground state to autolysis at an initial least ambrent or higher but not exceedin pH of at -iMgh sHr 4-, at/a temperature ©f-a^-higfeee^-SO C . , with gentle stirring, stopping the autolysis when the pH has reached about 6.5 and separating the autolysis product formed from the resulting mixture.

2. Process according to claim 1, wherein the autolysis is effected at a temperature of 0°-60°C.

3. Process according to claim 1 or 2, wherein the autolysis is carried out under an atmosphere of carbon dioxide or other inert gas.

4. Process according to any one of the preceding claims, wherein terpenes are added to the substance to be autolysed.

5. Process according to claim 4-, wherein terpenes extracted from lemon essence or orange essence or pineapple juice are added.

6. Process according to claim 1, wherein the substance to be autolysed is finely ground, the pH of the ground material is adjusted to about 5 by means of dilute hydrochloric acid or acetic acid, the temperature of the mixture is rapidly raised to about 55 C. , and this temperature is maintained until the pH has reached about 6.5> after which the heating is discontinued and the liquid autolysis product is separated.

7. Process according to any one of the preceding claims, wherein the autolysis product is concentrated in vacuo at a temperature of at highest 60°C. until a paste is obtained.

8. Process according to any one of claims 1-6, wherein the autolysis product is dried in vacuo at a temperature of at highest 60°C. until a powder is obtained.

9. Process for the manufacture of an autolysis product according to claim 1 substantially as hereinbefore described in any one of the Examples.

10. An autolysis product obtained by a process claimed in any one of. claims 1-9·

11. Autolysis product of fish and/or other ichthyological substances, free from oil, in a liquid form, which consists mainly of free aminoacids with or without small amounts of polypeptides, and also contains the biological principles existing in the raw material, but which is free from ammoniacal nitrogen.

12. An autolysis product according to claim 10 or 11 in the form of a paste or a powder.

13. An autolysis product according to any one of claims 10-12, which contains the following free aminoacids: aspartic acid, alanine, arginine, cysteine, cystine, glutamic acid, glycine, histidine, isoleucine, leucine, lysine, methionine, phenylalanine, proline, serine, threo-nine, tyrosine and valine.

14. An autolysis product according to any one of claims 10-13, which is free from antiseptics and preservatives yet is stable on storage. 15· An autolysis product according to any one of claims 10-14, which contains at least 9C% by weight of free aminoacids. For the Mi N ND PA TNE