DD284808A5 - METHOD FOR REMOVING GERMINATING - Google Patents

Abstract

A method is described for killing germs, germ products, infectious particles and similar pathogens on solids and in formulations of various compositions and for preserving these formulations. In this method, the solids or the formulations are introduced or filled into a compressed gas container provided with a valve. The container contents are then treated with gas.

Description

2 8 4 8 O 13

description

Method for killing germs

Field of application of the invention

The invention relates to a method for killing germs; Seed products, infectious particles and the like pathogenic agents on solids and in preparations of various compositions and for preserving these preparations, in particular of cosmetic and medical products

Characteristic of the known state of the art

Harmful germs, germs, fungi and the like pathogenic agents can grow on contaminated solids as well as in chemical products such as cosmetics and medicines. The contaminated products can then become harmful products themselves. Cosmetic and medical products are generally good breeding grounds for bacteria, fungi and the like, so it is a requirement to protect these products. There is a risk of increased contamination wherever cleansing, nourishing or conditioning cosmetics, as well as ointments, pastes, creams or emulsions, are stored in tubes, dispensers, cans, bottles and similar packaging and withdrawn from them in small portions for an extended period of time become.

It is therefore undisputed that all these products must be protected against toxic decomposition products, since such products can sometimes lead to significant damage to the health of the consumer.

It is generally the prevailing teaching that such protection is possible only by the addition of chemical preservatives. The prior art knows a multiplicity of chemical

products that fulfill the required task.

However, it is known that preservatives are not safe for the consumer, especially since they can cause allergies. Therefore, regulations have been adopted for the use of preservatives. The formation of allergic reactions in humans by preservatives, however, has a variety of causes, so that even careful and scrupulous tests and approval criteria can not guarantee a complete harmlessness of a preservative. In addition, the variety of contamination possibilities by very different acting pathogens and microorganisms require very different preservatives, so that their variety is easily overlooked.

Finally, it should be noted that a large number of the preservatives used only prevent the germ growth already existing in the product of existing germs, which were introduced for example in the production and bottling, and do not achieve complete killing of the germs

Object of the invention

The object of the invention is to provide a method of the type mentioned, with which not only inhibition of germ growth, but in a simple and economical manner while avoiding residual toxic effects, sterility on solids and in cosmetic and medical products is achieved and obtained remains

Principle of the Invention This object is achieved by a method of the type mentioned, is to introduce the solid preparations or in a valved pressure container or gas filled into this, and then gassed the container contents.

Advantageous developments of the method are characterized in the subclaims.

It was found contrary to the previous opinion of the art that can be dispensed with chemical preservatives in the applications mentioned. Instead of the usual pots, tubes, cans and the like, the cosmetic or medical products are filled in pressure gas containers with known propellants and this product is added to a gas or a gas mixture. Surprisingly, it was found that samples which had been prepared ten years ago were still perfect after removal and had no signs of decomposition. The composition consisted of extreme and easily spoiled substances, namely Frischei. It has been shown that particularly difficult to kill germs can be successfully controlled.

However, it has also been found that with the method according to the invention solids can be sterilized germ-free and thereby easily sterilized. This finding is particularly important for the medical sector, since this poses the problem of contamination of medical instruments and devices. Of these, absolute sterility, ie freedom from proliferation of germs, germinal products and infectious particles is required for each use. The known sterilization methods show sufficient applicability only for the thermostable range. It is autoclaved with tensioned steam at 1 bar pressure and 134 ° C or dry heat at 180 ° C worked. For the thermolabile range, ie ethylene oxide, formaldehyde or radiation sterilization treatment, significant limitations of the applicability due to material incompatibilities, but also in particular due to the human toxicity of the gases used are present.

With the method according to the invention a simple and problemlse sterilization of solids is possible.

embodiment

The invention will be explained in more detail by means of experiments.

First of all, the basic experiment was carried out with extreme and perishable products.

The fat phase 70 ° to 80 ° C was added, as usual, hot water:

% By weight of fabric

3.0 paraffin oil

8.0 lanolin anhydricum

3.0 Emuigierwachs

10.0 almond oil sweet

0.2 vitamin A palmitate

49.6 demineralized water, 80 ⁰ C.

In this cooled to 30 ° to 40 ° C cream was prepared on a cold Wpcjö emulsion

10.0 fresh whole egg

'0.0 sunflower oil

0.2 ascorbic acid

5.0 sodium lactate 50%

1.0 perfume oil stirred.

The filling was carried out in aerosol glass bottles in a ratio of 68 g of active ingredient to 7.5 g of LPG as propellant. The liquefied petroleum gas was composed 3: 1 of difluorodichloromethane: butane.

Subsequently, the finished filling active ingredient / LPG with CO _{2 was} applied, up to 10 bar - but also higher. This pressure builds up, depending on the active ingredient composition from strong, so that the statutory requirements can be complied with easily.

2 & 4 8 O 8

This composition was tested for microorganisms by a neutral institute and found the following results:

Enumeration:

bacteria

<10 / g <10 / g <10 / g

These results gave rise to further intensive experiments. The aim was to determine with which combinations of liquid gases, namely butane, dimethyl ether, propane / butane, and CO ₂ , N ₂ , N ₂ O, the system for the most diverse germs has an effect.

The cream with which the experiments were carried out had the following components:

g wt.% of fabric

Fat phase: paraffin oil 2.0 EmuIg! ADULT 3.8 Lanolin anhydricum 1.0 beeswax 1.0 Sunflower oil 20.0 Water phase: demineralized water 70.2 glycerin 2.0

100.0%

As usual for emulsions, the fat phase and the water phase were heated to 80 ° C and then stirred together.

After cooling to about 40 ° C, the emulsion was homogenized.

All other experimental approaches were based on this cream composition. To check the question, to what extent the process kills off and not only a preservation of the micro-organisms, each of the cream 50 g were filled in I00ml cans and this contaminated with the various germs. Thereafter, the cans were hermetically sealed and shaken to achieve uniform mixing. Thereafter, the gases were added to the cans. Of liquefied gases, namely butane, dimethyl ether and optionally propane / butane and mixed gas, in each case an amount of 3.5 g was used. The other gases, namely CO ₂ , N ₂ , N ₂ O, were subjected to a pressure of 12 bar. This pressure was greatly reduced with CO ₂ and N ₂ O after shaking.

In parallel, pure germ material was filled in a nutrient broth in 100 ml cans and fumigated just like the creams. The individual germ species were mixed together.

In the following Tables 1 and 2, the results of the first study have been called "cream" and "broth". - Three different types of germs have been used, which can be found almost everywhere in humans and in their environment:

1. Staphylococcus aureus:

2. Candida albicans:

3. Pseudomonas aeruginosa:

small round spherical bacteria with high resistance to dry environment

thick-walled, gram-positive, non-sporulating non-spore-forming yeasts of oval to roundish shape

Rodent bacteria with high resistance in a moist environment

The fumigation was done as follows:

Pressurizing the cans with only 10 bar compressed air pressurizing the cans only with 12 bar N ₂ pressurizing the cans only with 12 bar N ₂ O combination butane + N ₂ combination butane + N ₂ O combination DME + N ₂ combination DME + N ₂ O

All results of these experiments were unsatisfactory, or showed that a germ reduction with these Mittiin is not successful.

The test results with the effective gases and gas mixtures are summarized in Table 1.

The mixed gas consisted of a mixture of butane and dichlorodifluoromethane in the ratio 1: 3. The numerical values are logarithmic values, i. H. 5.0 means 10 germs per gram of cream, etc.

Contamination occurred on November 14, 1988 with 10 test bacteria per gram of cream, or 10 test bacteria per milliliter of broth. The investigations on microorganisms took place on 19.11.1988, on 28.11.1988, on 27.12.1988 and on 27.07.1989.

DME = dimethyl ether

Table 1

CREAM

Examiner. / germ type

without gas

DUTAN alone + CO2

HISCIIGAS alone + COz

I) M E alone 4 CO2

19.11 Staph Pseud Cand. .88. aureus. aerug. albic. .88. aureus. aerug. albic. 5.0 5.0 '4.0 Λ A A N Y NJ NJ <2 42 42 Λ Ν + C02 42 <2 <2 <2 <2 <2 41 <α 41 5.0 5.0 5.0 1.0 α <1 <1 28. 11 .88 .88. aureus. aerug. albic. values unchanged 4.0 5.0 3.0 <1 .0 27.12 .88 .88. aureus. aerug. albic. values unchanged 42.0 <2.0 <2.0 42.0 42.0 5.0 7.0 6.0 42.0 41.0 <1 .0 3.0 25.07 Staph Pseud Cand. .89. aureus. aerug. albic. .89. aureus. aerug. albic. > 5.0> 6.0> 6.0 <2 <2 42 42 4 42 42 <2 6 3.0 <L2 42 41 4.1 41 41 41 41 - Table 2 BOUILLON Exam date / germ type without gas B U T alone MISCIIGAS alone + CO2 D M alone + E CO2 19.11 Staph Pseud Cand. 7.0) 7.0) 6.0 y for all the qualitative test was positive in 1ml broth 2.8. 1 1 Staph Pseud Cand. > 7.0)> 7.0)> 6.0) 5.0 1.0 27.12 Staph Pseud Cand. > 8.0)> 8.0)> 7.0) > 6.0 ò.ó 25.07 Staph Pseud Cand. > 7.0> 7.0> 7.0 5.0 5.0 7.0 41.0 <1.0 41.0

The tables show that with certain gas combinations an excellent not only bacteriostatic, but also germicidal effect is achieved. This is expressed in particular by the finding in Table 2 "Bouillon", where the combination of DME + CO _{2 could be} shown to be particularly effective.

In the control doses without fumigation, despite a high starting bacterial count during the experimental period of eight months a strong germ growth was observed. This proves that the starting cream itself had no germicidal effect.

The results presented were confirmed by another series of tests in which creams and bouillon were contaminated with graded germ levels - 10 to 10 germs per gram of cream or milliliter of bouillon.

The contamination took place on 16 January 1989, the investigations on microorganisms on 20.01.1989, 25.01.1989 and 17.07.1989. Table 3 and the accompanying figure provide information about the results.

Table 3 CREAM

Exam Date BUTAN DME

Germination without gas alone + CO2 alone + CO2

20.1. 89 6.0 2.0 nn. 1.0 nn. Staph. aureus, 7.0 1111 nn nn. nn. Pseud. aerug. 5.0 3.0 nn. nn nn. Cand. albic. 25.01. 89 4.0 3.0 nn. nn. nn. Staph. aureus 6.0 nn. nn. nn. nn. Pseud. aerug. 7.0 3.0 nn. nn. nn. Cand. albic. 17.7. 89 4.0 nn. nn. nn. nn. Staph. aureus 6.0 5.0 nn. nn. nn. Pseud. aerug. 5.0 4.0 nn. nn. nn. Cand. albic.

nn. = undetectable

Again, the results with broth allow a more differentiated statement. Taking into account the starting bacterial counts (10 to 10), Table 4 "Bouillon" and the accompanying Figures 2, 3 and 4 make it clear that dimethyiether (DME) alone and as a mixture with CO _2, in contrast to the other gases and gas mixtures already 24 hours after fumigation and persistently for more than 6 months

10 germs per ml cause complete germ killing.

Table 4

BOUILLON

Untersuch.-Dat. .89 output ο. gas BUTA N DME + CO2 nn. / germ type 3 germs bacterial count alone + CO2 alone nn. nn. 20.1 2) 8.0 nn. nn. all 8.0 7.0: 6.0 5.0 3.0 4.0 nn. detection limit η η. (Fig. 7.0 6.0 5.0 4.0 : under the η η. .89 4.0 3.0 3 germs 3.0 nn. 25.01 3) 9.0 nn. η η. all 8.0 9.0 9.0 5.0 4.0 nn. nn. nn. (Fig. 7.0 6.0 9.0 5.0 3.0 3.0 3.0 nn. nn. 5.0 9.0 2.0 2.0 nn. nn. .89 4.0 9.0 4 .0 2.0 nn. nn. 3 germs 3.0 3.0 1.0 i7.07 8.0 nn. all , 4) 8.0 8.0 nn. nn. pn. 7.0 8.0 5.0 2.0 nn. (Fig. 6.0 8.0 5.0 nn. nn. 5.0 8.0 nn. nn. nn. 4.0 8.0 nn. 2.0 nn. 3.0 nn. nn.

nn. = undetectable

Figures 2, 3 and 4 illustrate the results particularly clearly.

To further test the effect of the system, the germ spectrum was expanded and introduced some particularly resistant germ species.

In addition to the three germs mentioned above, the following species were used:

Aspergillus niger: black piston mold

Hycobacterium terrae: belonging to the group of tuberculosis bacteria with high environmental resistance ·

Bacillus subtilis: widespread chopsticks

with rapid growth with the ability to sporulate, d. H. resistant survival form.

Bacillus sterothermophilus: also because of the ability

extremely resistant to sporulation, serves as a test germ for autoclaves.

Even for these partially very resistant germ species, a complete kill or at least a reduction of 5 to 6 log steps could be achieved with dimethyl ether or dimethyl ether + CO ₂ .

Significantly lower effects were achieved with butane or butane + CO ₂ .

The results clearly show that the above-mentioned methods make it possible to produce and maintain sterility in cosmetic and medical products without the addition of chemical preservatives.

In further studies, the use of this method of sanitization, i. for the sterilization of solids, in particular of medical instruments and equipment.

Experimental design:

In a - with CO ₂ - vented pressure vessel contaminated tweezers and plastic plates were given with the germs given below and the containers with 3.5 vol .-% or 7! 5 Vol% filled a 0.9% saline solution , Thereafter, the container was pressure-tight and closed

70% of the container volume was filled with the respective liquefied gases.

For the liquefied gases the following combinations were checked again:

Butane alone or with CO ₂ and DME alone or with CO ₂ .

The tweezers and plastic flakes were contaminated with the following seed solutions.

Concentration in g / ml

Germ type: initial germ number:

Staphylococcus aureus 1.0 χ 10

Candida albicans 7 ,; χ 10

Pseudomonas aeruginosa 1.1 χ 10

Aspergillus niger 3.0 χ 10

Bacillus subtilis 1,3 χ

E. CoIi 2.0 χ

Results:

For all investigated gas combinations, a reduction of at least 4 log levels could be observed for all germs.

With the combinations DME + CO ₂ +3.5 V-% NaCl 0.9% and CME + 7.5 V-% NaCl 0.9% -ig no germs could be detected after only 23 hours exposure time.

These results clearly show that for creams and solution. Proven killing of microorganisms and resistant germs can also be achieved by the above method in contaminated solids.

The applied pressures were between 3 and 20 bar.

Claims (6)

1. A method for killing germs, germ products, infectious particles and the like pathogenic agents on solids and in preparations of various compositions and for preserving these preparations, in particular of cosmetic, medical and pharmaceutical products, characterized in that the
Solid or the preparations in one with a valve
provided pressurized gas container or filled in this and then fumigated the container contents. 2. The method according to claim 1, characterized in that one
for gassing butane, mixed gas of butane and dichlorofluoromethane, butane and dimethyl ether, dimethyl ether alone or these
Gases combined with carbon dioxide used. 3. The method according to claim 1 and 2, characterized in that is added in the gasification of preparations liquefied gases in an amount of 5 to 20 wt .-%, based on the weight of the preparation. j 4. The method according to claim 1 and 2, characterized in that the composition is subjected to a pressure of 3 to 20 bar. 5. The method according to claim 1 and 2, characterized in that one or the solid body in the compressed gas tank in the presence of a liquid with liquid gas and fumigated. 6. The method according to claim 5, characterized in that one
with the gas or gas mixture and with a pressure of 3 to
20 bar acted upon.