JPS62221612A - Production of cosmetic material - Google Patents

Abstract

PURPOSE:Conchiolin, a hard protein in pearl or shells is decomposed with hydrochloric acid, then the acid is removed, the remainder is ultrafiltered to give a cosmetic material of high safety without sensitization. CONSTITUTION:Conchiolin made from pearl oyster, hard-shelled mussel, blue mussel, fresh water pearl oyster, fresh water mussel, preferably pearl oyster or pearl is combined with 2-10% aqueous hydrochloric acid solution to effect hydrolysis at 50-110 deg.C for 5hr to 5 days. The product is dried or evaporated to remove the hydrochloric acid, ultrafiltered to remove high-molecular peptides to collect conchiolin free from sensitizing components. The conchiolin is used to make cosmetics. EFFECT:The product is quite safe, quite free from cosmetic pollution even when it is used for a long period of time.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing cosmetic raw materials, and more specifically to cosmetics made from conchiolin, a hard protein contained in pearls and various shells. It concerns the manufacturing method of raw materials.

Therefore, the present invention plays an important role not only in the technical field of cosmetics, but also in the technical field of the fisheries industry, such as pearl cultivation and various shellfish cultivation, and the technical field of protein chemistry.

(Prior art) Regarding cosmetics that use shells 1, powders such as scrap pearls and Akoya shells have been used on a very small scale at home or as a family tradition, as they have skin conditioning and skin nourishing effects. It just came.

However, by applying a scientific scalpel to these techniques, we were able to determine the true nature of the active ingredients and create a safe cosmetic that will not cause sensitization due to irritation or redness even after long-term use. There has been no industrialization at all.

Furthermore, we have created a cottage industry that not only extracts the decomposition products of conchiolin as an active ingredient, but also removes the sensitizing ingredients that are a source of harmful side effects, producing extremely safe cosmetics that can withstand long-term use. The current state of technology is such that it is not even possible to dream of large-scale factory production.

(Problems to be solved by the invention) Cosmetics made from the decomposition products of conchiolin, an excellent skin-conditioning ingredient found in seashells and pearls, are excellent cosmetics containing natural products, but they do not have long-term effects on the skin. If you use it, it can cause harmful side effects such as skin irritation, itching, and redness.

The present inventor discovered for the first time that it could no longer be used.

The present invention focused on the problem of sensitization of funchiolin, which was discovered for the first time by the present inventor, and was made for the purpose of developing a new and excellent cosmetic raw material that is safe and free of sensitization.

(Means for Solving the Problems) The present invention has been made to achieve the above object, and is applicable to various technologies such as animal experiments and clinical trials that directly use human skin, as well as biochemistry and cosmetic science. As a result of extensive research in the field, we discovered that the cause of sensitization was the polymeric peptides in conchiolin degradation products.

Furthermore, polymer peptides can be added to the conchiolin decomposition products without impairing their excellent cosmetic effects.
As a result of research into industrial methods for removing conchiolin from decomposition products, it was discovered that ultrafiltration is suitable, leading to the completion of the present invention.

That is, the present invention first makes the new discovery that (1) conchiolin decomposition products contain harmful sensitizing substances and cannot be used safely for a long period of time, and (2) that the sensitizing products They further discovered that the chemical substance was a high-molecular peptide, and finally discovered that (3) ultrafiltration was the optimal method for removing this high-molecular peptide.The accumulation of these new discoveries led to the publication of this book. The invention is complete.

The starting material of the present invention is conchiolin. As conchiolin, pearl oyster (Pinctadamartans)
iL), Mytilig coruscum
, Mytilus edulis,
Llyriopsis schleg
elii), crow clam (Cristariapl,
1cata), etc., which are produced from the family Laguineaceae, the family Musselaceae, the family Musselaceae, etc. as raw materials are preferred.

You can freely use products made from other shellfish and commercially available products.
Conchiolin produced from Akoya oyster (pearl oyster) and pearl is particularly suitable since there is no problem in terms of supplying WX material. It is also possible to use crude conchiolin without purification.

Since the active ingredient of the cosmetic raw material according to the present invention is a decomposition product of conchiolin protein (sometimes simply referred to as "conchiolin"), conchiolin is first hydrolyzed. A 0.5-15% hydrochloric acid aqueous solution is used for oil hydrolysis, and the oil is treated for 30 minutes to 10 days while controlling the temperature at 0-130°C.

Of course, the three requirements of hydrochloric acid concentration, hydrolysis temperature, and hydrolysis time must not be set so that conchiolin is completely decomposed into amino acids during hydrolysis.

Preferably, demineralized Akoya shell or pearl Funchiolin is added with a 2 to 10% hydrochloric acid aqueous solution to a concentration of 50 to 110%.
After hydrolysis for 5 hours to 5 days at ℃, the hydrochloric acid is removed.

Conventional methods are used to remove hydrochloric acid, for example,
Freeze-drying or evaporation is preferred.

Further, it is neutralized with an alkali such as ammonia or sodium hydroxide and desalted using a known desalting method.

Also suitable is a method in which amino acids are adsorbed using an ion exchange resin after neutralization with ammonia, and then desorbed with ammonia.

For example, fill a column with Amberlite IR-120H type resin, pass the previously obtained conchiolin hydrolyzate through it, desorb it with an alkali such as N-N1140H, combine the effluents, and add if necessary. Concentrate using conventional methods. In addition, if necessary, it may be dried by evaporation to dryness, freeze-drying, or other appropriate methods, and distilled water may be added at the stage of moving to the next step to prepare a liquid with the desired concentration. good.

In cosmetics, salt can destroy the emulsion of creams, etc., so it is better to have as little salt as possible.
It is preferable that the desalting treatment be completed.

The conchiolin hydrolyzate desalted in this way is
If necessary, it is concentrated and then ultrafiltered to remove harmful components such as peptides.

Ultrafiltration is performed by a conventional method, preferably under pressure using a commercially available ultrafiltration membrane.

In the present invention, ultrafiltration is performed for the purpose of removing polymer peptides, and the molecular weight cutoff for ultrafiltration is sufficient to remove 6000 or more, but the nominal molecular weight cutoff is 2.
000 ultrafiltration membranes serve this purpose.

For example, ultrafiltration using Am1con membrane or diafil
tration ultrafiltration can be advantageously used.

The liquid that has passed through the ultrafiltration membrane no longer contains sensitizing polymeric peptides.

This can be freely used as a safe cosmetic raw material. If necessary, it may be dried by freeze-drying or the like, or concentrated by vacuum concentration or the like to make it convenient for storage or later use.

The liquid that has passed through the ultrafiltration membrane in this way.

For example, after sterilization, it is filtered, and in the case of a nutritional cream, it is added to the nutritional cream base in an amount of about 1 to 5%.

In the case of nutritional lotion, add 0.2 to an alkaline lotion base.
The desired cosmetic products are manufactured by adding about 4%, and in the case of packs, about 2 to 8% to the pack base. However, the cosmetic raw material according to the present invention has the active ingredient of conchiolin concentrated and harmful sensitizing components have been removed, so it can exert a skin conditioning effect even when used in a small amount, and it can also be used in large quantities. It has no harmful effects and is completely safe for the skin and human body. Therefore, it is not limited to the range of use described above, and can be freely used outside the range.

Next, examples and test examples of the present invention will be described.

Example: To 1 kg of decalcified conchiolin as a dry product, 1.2 Q of 8Q water was added to HCl, the container was sealed, and the mixture was heated and decomposed at 60° C. for 50 hours.

After the decomposition is complete, add ammonia to approximately P11 while measuring the pH.
Add a small amount at a time while stirring thoroughly, and add this to 10
After centrifugation for 1 minute, the mixture was filtered through 3 micron filter paper.

Dilute this 35 times with water and add ρ11 with hydrochloric acid or ammonia.
After setting it to 2.0, 20 of Amberlight IR-1208
After passing through a 0Q column, it was eluted with IN ammonia 600Q.

This liquid was passed through an ultrafiltration membrane P2 (fraction molecule ff12000) manufactured by Romicon and freeze-dried.

In this way, cosmetic raw material 792G made from conchiolin and containing no sensitizing ingredients was obtained.

Test Example 1 The product raw material obtained in the example was used as sample side 1, and as a control, the material obtained by repeating the same operations as in the example except for the ultrafiltration step was used as sample Nα2 for the next visit. The state of molecular distribution was examined using high-performance liquid chromatography.

Column TSK-G2000G 7.5mm x 60
0mm eluent 0.05N phosphoric acid buffer −+ O,
IN Na504 (pH 7,0) Flow bkO, 5mM Detector Ultraviolet absorption 210mm The results are as shown in the drawings; the results for sample Nα1 are shown in FIG. 1, and the results for sample Ha 2 are shown in FIG.

As is clear from these drawings, it can be seen that harmful polymeric parts have been removed in sample Nα1.

Test Example 2 A sensitization test was conducted using the Maximization test method. 10 healthy guinea pigs were used as test animals.
Six groups of mice were prepared, and 2,4-D was used as a positive control.
Using introchlorobenzsne, one group was used for sensitization treatment and the other group was used as a control for induction for three samples: sample Na L, sample Nα2, and positive control.

As a result, the results shown in the following table were obtained.

Measurement time is the time after 24 hour occlusive patch application for induction.

I know it's strong.

(Effect of the invention) According to the present invention, by a very [proper operation].

Sensitizing polymeric peptides are industrially removed from conchiolin cosmetic raw materials (in this regard, test example 1
and 2, it has been clearly demonstrated both chemically and biologically). Therefore, according to the present invention, it is possible to provide cosmetics that are extremely safe and can be used for a long period of time without any cosmetic pollution.

Moreover, despite the removal of sensitizing substances, Conchiolin's inherent skin-conditioning effects are fully maintained without any loss in the cosmetic raw material, and it can be used in various formulations and in various forms. Therefore, according to the present invention, cosmetics effective for early recovery from skin fatigue, pigment bleaching, prevention of skin aging, prevention of stiffness, shine, etc. can be freely prepared. be able to.

Furthermore, conventionally, scrap pearls and Akoya shells after pearl harvesting had no effective use and were discarded, but the present invention opens up a new way of effectively utilizing these waste materials. Furthermore, conchiolin-containing shells other than pearl oysters can be widely used, and the present invention is also extremely superior in terms of effective use of resources.

[Brief explanation of drawings]

FIG. 1 is a liquid chromatogram of a cosmetic raw material according to the present invention, and FIG. 2 is a liquid chromatogram of a substance that was not subjected to ultrafiltration. N119 Toru, oo! ro, oo
5buQQ 6a, 01)
6.7. n. Cut, oo qroo 5o, oo sr,
oo 6o, ac (, g, o. Procedural Amendment July 4, 1986)

Claims (4)

[Claims] (1) A method for producing a cosmetic raw material, which comprises decomposing conchiolin with hydrochloric acid, removing the hydrochloric acid, and then ultrafiltrating it. (2) The manufacturing method according to claim 1, wherein the hydrochloric acid removal step includes desalination after neutralization. (3) The hydrochloric acid removal step is characterized in that the amino acid is adsorbed using an ion exchange resin after being neutralized with an alkali, and then desorbed with an alkali. Production method. (4) The manufacturing method according to claim 1, 2, or 3, characterized in that the molecular weight cut off in the ultrafiltration is 6,000 or less.