GB2164353A - Process for the preparation of an elixir - Google Patents

Abstract

The preparation of a stabilized quail's egg based elixir of roborating effect having medium alcohol content comprises admixing a sugar with quail's egg powder; admixing with ethanol optionally comprising a conserving agent and/or anti-oxidant; grinding the mixture thus obtained on a fine grinding machine operating with a high revolution number to a particle size below 20 micrones; admixing with a stabilizing agent; diluting with distilled water to the desired concentration and if desired subjecting the mixture to post-homogenization. The advantage of the process is that it enables the preparation of a stabilized quail's egg based elixir without the use of a surfactant.

Description

SPECIFICATION Process for the preparation of an elixir This invention relates to a stabilized quail's egg based elixir of roborating effect and having a medium alcohol content.

Quail's eggs are used for manifold purposes due to the valuable components contained therein. it is known for a long time that various meals can be prepared from quail's eggs. Recently quails's eggs have become widespreadly used in cosmetical industry for the preparation of various cosmetic compositions, e.g. conditioning face-skin packing.

It is known furtheron that quail's egg has a high fat content of about 48-50%. Such substances of a high fat content are generally very poorly wettable by water and for this reason they can be uniformly distributed in aqueous medium only by means of adding various surfactants/wetting agents, dispersing agents/ to the system.

Drinks having roborating effect are generally destined for long-lasting consumption and are administered to the human organism for a longer period of time. Surfactants may be, however, detrimental to the health on lasting consumption. For this reason surfactants are generally not used in the preparation of foodstuffs or drinks for long-lasting consumption. However the processing of quail's egg powder having a high fat content in aqueous medium encounters serious difficulties in the absence of surfactants because of the hydrophobic character of the product.

It has been found that stabilized quail's egg based elixirs of roborating effect and having a medium alcohol content may be readily prepared by eliminating the use of surfactants by admixing a sugar with quail's egg powder; admixing with ethanol optionally comprising a conserving agent and/or antioxidant; grinding the mixture thus obtained on a fine grinding machine operating with a high revolution number to a particle size below 20 micrones; admixing with a stabilising agent; diluting with distilled water to the desired concentration and if desired subjecting the mixture to post-homogenization.

The present invention is based on the recognition that on grinding a mixture of a suitably treated sugar, quail's egg powder and ethanol optionally comprising an anti-oxidant and/or a conserving agent in a micronizing apparatus to a particle size below 20 micrones, a system is formed which is suitable for the preparation of stable compositions not separating into phases, meeting the aesthetic requirements and being suitable for lasting storage.

The above recognition was not aforeseen on the basis of the teaching of the prior art. It is surprising that in the absence of a surfactant from quail's egg powder having a high fat content a product can be prepared which can be readily worked up in aqueous medium and which provides uniform distribution.

In addition, we have found in the course of our experimental work that according to methods which are different from the process of the present invention or comprise only certain elements thereof no product of suitable quality can be obtained.

Thus the said experiments gave the following results: On admixing quail's egg powder with water the powder is not wetted at all. On suspending quail's egg powder in concentrated ethanol a product unsuitable for practical use is obtained due to coagulation. When quail's egg powder is suspended in diluted aqueous ethanol a gelatinous product is obtained which can not be worked-up. On homogenizing a mixture of quail's egg powder and methyl cellulose mucus in a colloidal mill or an ultra turrax the mucus system is decomposed and can no more exhibit the desired stabilizing effect and consequently the product obtained can not be processed. On subjecting to grinding a mixture of quail's egg powder, methyl cellulose and sugar syrup in a colloidal mill the mucus structure of the system is smashed.According to a further test a mixture of methyl cellulose mucus, sugar syrup and quail's egg powder is stirred with a slowly rotating stirrer /50-100 r.p.m./. We completely failed, however, in achieving the desired result. The product obtained separates into several phases, an upper layer gets separated and a product unsuitable for further working-up is formed. The said tests are described in details in Example 2.

According to the process of the present invention as sugar preferably a saccharose syrup partially inverted by warming with an acid can be used. Inversion can be carried out by known methods, preferably under warming at a temperature of about 80"C. As acid inorganic or organic acids, preferably citric acid, can be used in the said inversion step.

The composition obtained by the process of the present invention comprises quail's egg powder /Pulvis ovi gen. Coturnix/ as active ingredient.

Sugar syrup prepared as described above is admixed with quail's egg powder under constant stirring.

Quail's egg powder may be added to the sugar syrup in any conventional apparatus equipped with a stirrer /e.g. Anker-stirrer/. Quail's egg powder may be added in portions and stirring is continued until the unwetted lumps disappear.

The ethanolic solution optionally comprising an anti-oxidant and/or a conserving agent is then added.

The anti-oxidants and conserving agents which may be preferably used in the process of the present invention are discussed later.

The suspension thus formed is introduced into a fine grinding apparatus operating at a high revolution number and ground to a particle size below 20 micrones. The proper particle size is of critical importance because the physico-chemical characteristics of the system thus obtained enable, in the absence of a surfactant, the preparation of a product which has a suitable stability and is not separated into layers.

The lower limit of the particle size interval is of minor importance and is determined by practical and technological factors. Below a certain size-limit namely expensive and specific grinding-micronising equipment is required and the advantage achieved does not justify the costs. Moreover the grinding period required is very long. For practical purposes the preferable lower limit of the particle size interval amounts to 3-5 micrones.

Wet grinding may be carried out in known micronizing equipment, e.g. in colloidal mill or ultra-turrax.

The system obtained after micronization - which comprises particles having a size below 20 micrones, preferably 3-20 micrones - is admixed with a stabilizer. The stabilizing agents which can be preferably used according to the process of the present invention are discussed below.

To the system aroma substances and dyestuffs may be added. As aroma any approved aroma of food industry may be used ie.g. banana aroma'. As dyestuffs any approved dyestuffs of food industry may be applied. One may proceed preferably by taking out a small sample of the mixture, admixing the same with the aroma substance and the solution of the dyestuffs and re-introducing the mixture to the residual mixture.

The mixture thus obtained is diluted to the desired concentration. The ready-for-use elixir comprises preferably 9-12 % by weight of alcohol, 12-25 % by weight of sugar, 4-15 % by weight of quail's egg powder, 0.01-5.0 % by weight of stabilizing agent and 0.01-5.0 % by weight of anti-oxidant and/or conserving agent. After diluting to the desired concentration the mixture may be optionally subjected to post-homogenization. This step may be carried out by methods known per se.

According to the process of the present invention as stabilizing agent any suitable natural macromolecular substance, semi-synthetic macromolecular product, synthetic macromolecular product or inorganic gel-forming substance may be used.

As natural macromolecular substance preferably arabic gum, tragacanth gum, starch, pectine, alginic acid, an alginate, carrageen, agar or gelatine may be used.

As natural macromolecular stabilizing agent particularly 0.01-0.5 % by weight, preferably 0.05-0.1 % by weight, of agar, 0.05-5.0 % by weight, preferably 0.1-1.0 % by weight of sodium alginate; 0.01-3.0 % by weight, preferably 0.1-0.5 % by weight, of carragen; 0.5-2.0 % by weight, preferably 1-1.5 % by weight, of arabic gum; 0.05-2.5 % by weight, preferably 0.1-1.0 % by weight, of pectine; 0.1-5.0 % by weight, preferably 0.5-1.0 % by weight, of tragacanth gum; or 0.01-5.0 % by weight, preferably 0.1-1.0 % by weight, of xanthane gum may be used.

As semi-synthetic macromolecular stabilizing agent preferably methyl cellulose, ethyl cellulose, carboxy methyl cellulose, carboxymethyl cellulose sodium, hydroxypropyl cellulose or alginic acid propyleneglycole ester may be used.

As semi-synthetic macromolecular stabilizing agent particularly 0.1-5 % by weight, preferably 0.2-2.0 % by weight, of methyl cellulose; 0.1-5.0 % by weight, preferably 0.1-2.0 % by weight, of carboxymethyl cellulose; 0.1-5.0 % by weight, preferably 0.1-2.0 % by weight of sodium carboxy-methyl cellulose; 0.1-5.0 % by weight, preferably 0.1-2.0 % by weight of hydroxyethyl cellulose; or 0.01-5.0 % by weight, preferably 0.1-1.0 % by weight of alginic acid propylene glycole ester may be used.

As synthetic macromolecular stabilizing agent preferably polyvinyl alcohol, polyvinyl pyrrolidone or a carboxy-vinyl polymer may be used.

As synthetic macromolecular stabilizing agent particularly 0.01-5.0 % by weight, preferably 0.1-1.5 % by weight of polyvinyl alcohol or 0.01-5.0 % by weight, preferably 0.1-1.0 % by weight of polyvinyl pyrrolidone may be applied.

As inorganic gel forming substance preferably bentonite or colloidal magnesium aluminium silicate may be used. Bentonite may be added preferably in an amount of 0.1-5.0 % by weight, preferably 0.5-1.5 % by weight, and colloidal magnesium aluminium silicate may be used in an amount of 0.5-5.0 % by weight, preferably 0.5-1.0 % by weight.

According to a preferred form of realization of the process of the present invention methyl cellulose is used as stabilizing agent, preferably in an amount of 0.5-5.0 % by weight, particularly 0.1-2.0 % by weight, especially 0.5-2.0 % by weight.

In pharmaceutical industry methyl cellulose mucus is generally prepared by pouring hot water onto methyl cellulose powder, allowing to stand for a certain period of time and finally adding cold water /0-5 'CI comprising the conserving agents. The drawback of the said method is that the product obtained often comprises lumps, causes sedimentation and is difficult to be worked up.

It has been found that a readily processible and workable methyl cellulose mucus comprising no lumps can be prepared by adding powdered methyl cellulose to water in small portions and thereafter adding the aqueous solution of the conserving agents comprising glycerol too. As conserving agent preferably methyl andlor propyl p-hydroxy-benzoate may be used.

According to the process of the present invention natural or synthetic anti-oxidants or consErving agents may be used.

As natural anti-oxidant preferably tocoferol, gallic acid, sesamol, coniferyl benzoate, guajaratic acid or dihydro guajaratic acid may be used.

As synthetic anti-oxidant preferably a gallic acid alkyl ester, preferably the ethyl, propyl, octyl, lauryl or cetyl ester, or butyl hydroxy anisole or butyl hydroxy toluene may be applied.

One may particularly preferably use butyl hydroxy toluene, particularly in an amount of 0.005-0.02 % by weight, preferably 0.01 % by weight.

One may furtheron use synergistic agents, preferably esters of ascorbic acid formed with higher aliphatic carboxylic acids /e.g. ascorbyl palmitate/ or phosphoric acid or citric acid. The amount of ascorbic acid esters may be preferably 0.01-0.1 % by weight and that of phosphoric acid or citric acid 0.005-0.20 % by weight, preferably 0.1 % by weight. Phosphoric acid or citric acid may also serve to adjust the pH to the desired value.

As conserving agent preferably a p-hydroxybenzoic acid ester or a mixture of such esters, preferably the methyl, ethyl and/or propyl ester of p-hydroxybenzoic acid, or glycerol, sorbic acid, a sorbate, preferably potassium sorbate or sodium sorbate, or ethanol may be used.

One may proceed preferably by using methyl and/or propyl p-hydroxybenzoate in an amount of 0.051.25 % by weight, preferably 0.08-0.25 % by weight, or glycerol in an amount of 0.5-10 % by weight, preferably 2-5 % by weight; sorbic acid or a sorbate in an amount of 0.01-2.0 % by weight, preferably 0.11.0 % by weight, or sodium benzoate in an amount of 0.01-5.0 % by weight, preferably 0.05-1.0 % by weight.

The elixirs prepared according to the process of the present invention may be used particularly in postillness and post-operation conditions, to strengthen and roborate human organism pulled down by a disease, to improve the health condition of aged people, to improve the stamina of sportsmen and in case of strong diets and slimming cures. The compositions prepared according to the process of the present invention meet aesthetic requirements, posses excellent physical, chemical and microbiological stability and can be stored for a long time.

Further details of the present invention are to be found in the following Examples without limiting the scope of protection to the said Examples.

Example 1 AlPreparation of methyl cellulose mucus Into a 500 ml. flask 220 ml. of water, 24 g of glycerol and a solution of 2.16 ml. of 96 % ethanol, 0.072 g. of propyl p-hydroxybenzoate and 0.168 g. of methyl p-hydroxybenzoate are weighed in and the mixture is allowed to stand under cooling.

In another 500 ml. round-bottomed flask 96 g. of water heated to 80 C are weighed in and 6.0 g. of methyl cellulose are added under constant stirring. The mixture is allowed to stand for half an hour and cooled to 60-65 C. The cooled solution prepared according to the previous paragraph is added to the mixture of water and methyl cellulose under stirring.

Bl Preparation of a sugar syrup To a mixture of 192 g. of sugar and 192 g. of water a solution of 0.96 g. of citric acid in 2.53 g. of water is added under stirring at 80 C. After complete dissolving of the sugar the mixture is heated at 80-85 "C for some minutes and then allowed to cool.

Cl Preparation of the elixir Into an 1500 ml. flask equipped with a stirrer the sugar syrup according to Example 1B is introduced whereupon 48 g. of quail's egg powder are added in portions under constant stirring. The mixture is stirred until the unwetted lumps occasionally present disappear /about 30 minutes.

To the mixture a solution of 0.096 g. of butyl hydroxy toluene, 102 ml. of ethanol and 130 ml. of water are added and the mixture is stirred for some minutes. The suspension is introduced into a colloidal mill /type Cadmach CMCM 5/ and the ground suspension leaving the colloidal mill is added under constant stirring to the methyl cellulose mucus prepared according to A, and pre-weighed into a 1500 ml. flask.

The system is stirred for about an hour, a 40-50 ml. sample is taken out, admixed with 0.68 g. of aroma and an aqueous solution of the dyestuffs and then re-added to the residual mixture in the flask. The system is filled up to 1020 ml. with distilled water and subjected to post-homogenization for half an hour.

The composition of the elixir thus obtained is shown in Table I.

TABLE I Component Amount 9 % Methyl cellulose 1.0 0.5882 Glycerol 4.0 2.3529 p-hydroxybenzoic acid propyl ester 0.012 0.0070 p-hydroxybenzoic acid methyl ester 0.028 0.0152 Quail's egg powder 8.0 4.7058 Saccharose 32.0 18.8235 Citric acid 0.16 0.0941 Butyl hydroxy toluene 0.016 0.0094 Ethanol 17.36 10.2117 Banana aroma 0.136 0.0800 Ariavit tartrazine dyestuff 0.002619 0.0015 Ariavit indigoarmine dyestuff 0.000081 0.000048 Water added to 170.00 100.00 Example 2 Comparative example A 48 g. of quail's egg powder are admixed with about 200 ml. of water. The powd r is not wetted and lumps are swimming on the surface of the water. The mixture thus obtained can not be worked-up in a colloidal mill.

B 48 g. of quail's egg powder are admixed with 100 g. of concentrated /96 %! ethanol. The mixture can not be worked-up because of the coagulation of proteins.

Cl 48 g. of quail's egg powder are admixed with 200 g. of 50 % aqueous ethanol. A gelatinous product is obtained which is unsuitable for processing.

Di 48 g. of quail's egg powder are admixed with 350 g. of a methyl cellulose mucus prepared according to Example 1Al. The mixture is passed through a colloidal mill or ultra-turrax and thus homogenized. The large shear force smashes the stabilizer system and therefore the product obtained is separated into layers, completely inhomogenous and is completely unsuitable for being placed on the market.

C 48 g. of quail's egg powder, 390 g. of sugar syrup prepared according to Example 18/and 350 g. of methyl cellulose mucus prepared according to Example 1A/ are admixed and passed through a colloidal mill or an ultra-turrax. The properties of the product thus obtained are the same as those of the product prepared according to Example 2D1.

Fi The mixture prepared according to Example 2E/ is stirred with the aid of a slowly rotating stirrer for a long period of time /at least 2 hours, 50-300 r.p.m./. The phases separate and a product being unsuitable for marketing is obtained.

Claims (29)

1. Process for the preparation of a stabilized quail's egg based elixir of roborating effect having medium alcohol content, which comprises admixing a sugar with quail's egg powder; admixing with ethanol optionally comprising a conserving agent and/or anti-oxidant; grinding the mixture thus obtained on a fine grinding machine operating with a high revolution number to a particle size below 20 micrones; admixing with a stabilising agent; diluting with distilled water to the desired concentration and if desired subjecting the mixture to post-homogenization.

2. A process according to Claim 1, which comprises using as sugar component a saccharoze syrup inverted by heating with an acid.

3. A process according to Claim 2, which comprises using citric acid as acid in the inversion step.

4. A process according to any of Claims 1-3, which comprises using sugar in an amount of 15-25 % by weight, preferably 18-20 % by weight, related to the total weight of the composition.

5. A process according to any of Claims 1-4, which comprises using a natural macromolecu ar substance, a semi-synthetic macromolecular product, a synthetic macromolecular product or an inorganic gel-forming agent as stabilizing agent.

6. A process according to Claim 1, which comprises using as natural macromolecular stabilizing agent arabic gum, tragacanth gum, starch, pectine, alginic acid, an alginate, carrageen, agar or gelatine.

7. A process according to Claim 5 or 6, which comprises using as natural macromolecular stabilizing agent 0.01-0.5 % by weight, preferably 0.05-0.1 % by weight, of agar; 0.05-5.0 % by weight, preferably 0.1-1.0 % by weight, of sodium alginate; 0.01-3.0 % by weight, preferably 0.1-0.5 % by weight of carragen; 0.5-2.0 % by weight, preferably 1-1.5 % by weight of arabic gum; 0.05-2.0 % by weight, preferably 0.1-1.0 % by weight of pectine; 0.1-5.0 % by weight, preferably 0.5-1.0 % by weight of tragacanth gum; or 0.01-5.0 % by weight, preferably 0.1-1.0 % by weight of xanthane gum.

8. A process according to Claim 5, which comprises using as semi-synthetic mK cromolecular stabilizing agent methyl cellulose, ethyl cellulose, carboxy methyl cellulose, carboxymeth tl cellulose sodium, hydroxy-propyl cellulose or alginic acid propyleneglycole ester.

9. A process according to Claim 5 or 8, which comprises using as semi-synthet,e macromolecular stabilizing agent 0.1-5 % by weight, preferably 0.2-2.0 % by weight of methyl cellulose; 0.1-5.0 % by weight, preferably 0.1-2.0 % by weight, of carboxymethyl cellulose; 0.1-5.0 % by weight, preferably 0.1-2.0 % by weight of sodium carboxymethyl cellulose; 0.1-5.0 % by weight, preferably 0.1-2.0 h by weight, of hydroxyethyl cellulose; or 0.01-5.0 % by weight, preferably 0.1-1.0 % by weight, of alginic acid propylene glycole ester.

10. A process according to Claim 9, which comprises using as semi-synthetic macromolecular stabilizing agent methyl cellulose.

11. A process according to Claim 10, which comprises using methyl cellulose in an amount of 0.1-5.0 % by weight, preferably 0.1-2.0 % by weight, particularly 0.5 % by weight.

12. A process according to Claim 5, which comprises using as synthetic macromolecular stabilizing agent polyvinyl alcohol, polyvinyl pyrrolidone or a carboxyvinyl polymer.

13. A process according to Claim 5 or 12, which comprises using as synthetic macromolecular stabilizing agent 0.01-5.0 % by weight, preferably 0.1-1.5 % by weight, of polyvinyl alcohol or 0.01-5.0 % by weight, preferably 0.1-1.0 % by weight, of polyvinyl pyrrolidone.

14. A process according to Claim 5, which comprises using as inorganic gel-forming stabilizer bentonite or colloidal magnesium aluminium silicate.

15. A process according to Claim 5 or 14, which comprises using bentonite in an amount of 0.1-5 % by weight, preferably 0.5-1.5 % by weight, or colloidal magnesium aluminium silicate in an amount of 0.1-5.0 % by weight, preferably 0.1-1.0 % by weight.

16. A process according to Claim 1, which comprises using a natural or synthetic anti-oxidant or conserving agent.

17. A process according to Claim 16, which comprises using as natural anti-oxidant tocoferol, gallic acid, sesamol, coniferyl benzoate, guajaratic acid or dihydro guajaratic acid.

18. A process according to Claim 16, which comprises using as synthetic anti-oxidant a gallic acid alkyl ester, preferably the ethyl, propyl, octyl, lauryl or cetyl ester, or butyl hydroxy anisole or butyl hydroxy toluene.

19. A process according to Claim 18, which comprises using butyl hydroxy toluene as synthetic antioxidant.

20. A process according to Claim 19, which comprises using butyl hydroxy toluene in an amount of 0.005-0.02 % by weight, preferably 0.01 % by weight.

21. A process according to Claim 16, which comprises using as anti-oxidant an ascorbic acid ester formed with a higher aliphatic carboxylic acid, preferably ascorbyl palmitate, or phosphoric acid or citric acid.

22. A process according to Claim 21, which comprises using 0.01-0.1 % by weight of an ascorbic acid ester or 0.005-0.20 % by weight, preferably 0.1 % by weight, of citric acid or phosphoric acid.

23. A process according to Claim 16, which comprises using as conserving agent a p-hydroxy-benzoic acid ester or a mixture of such esters, preferably the methyl, ethyl and/or propyl ester of p-hydroxybenzoic acid, or glycerol, sorbic acid, a sorbate, preferably potassium sorbate or sodium sorbate, or ethanol.

24. A process according to Claim 16 or 23, which comprises using methyl and, or propyl p-hydroxybenzoate in an amount of 0.05-1.25 % by weight, preferably 0.08-0.25 % by weight, or glycerol in an amount of 0.5-10 % by weight, preferably 2-5 % by weight; sorbic acid or a sorbate in an amount of 0.012.0 % by weight, preferably 0.1-1.0 % by weight, or sodium benzoate in an amount of 0.01-5.0 % by weight, preferably 0.05-1.0 % by weight.

25. A process according to any of Claims 1-24, which comprises using quail's egg in an amount of 415 % by weight, preferably 4.5-4.7 % by weight.

26. A process according to any of Claims 1-25, which comprises grinding a mixture of saccharose syrup inverted by heating with an acid, quail's egg powder and alcohol comprising a conserving agent and/or an anti-oxidant Ir, a colloidal mill or an ultra-turrax to a particle size between 3 and 20 micrones.

27. A process according to Claim 1 or 26, which comprises preparing the methyl cellulose stabilizing agent by adding methyl cellulose to water and thereafter adding the solution of a conserving agent.

28. A process according to Claim 27, which comprises using methyl or propyl p-hydroxybenzoate as conserving agent.

29. Stabilized quail's egg based elixirs of roborating effect and having a medium alcohol content whenever prepared by the process according to any of Claims 1-28.