[0001] The invention relates to a self-dissolving capsule for preparation of washing solutions,
containing chemical materials and probiotic microorganisms. Structure - the capsule
is comprised of two or more cavities, wherein one of them is filled with a tablet
composed partially of microorganisms.
[0002] Known household chemistry formulations, appearing on the market in form of capsules
enclosed in self-dissolving films, and formulations containing microorganisms are
mono- and multi-cavity self-dissolving capsules in liquid/liquid, liquid/powder, powder/liquid
phase, used for laundry washing, dishwashing, cleaning of hard surfaces such as floors
or windows (to a small extent). They contain concentrated, active chemical substances.
Whereas the formulations containing microorganisms are products in bottles with an
atomizer (trigger) containing nonionic surfactants of natural origin, soaps of natural
origin and probiotic strains. These formulations are usually very expensive and directed
towards environmentally-friendly households, mainly for cleaning of hard surfaces.
[0003] The object of the invention is improving the available cleaning agents by providing
formulations preventing harmful changes in composition of the microbial flora resulting
from using aggressive detergents as cleaning agents that firstly cause sterilisation
of cleaned surfaces and appliances, which later leads to uncontrolled colonisation
of such ecological niches by undesirable microorganisms. This often leads to arising
of hard to remove, unpleasant odours (biofilms), e.g. in spaces of washing or laundry
washing devices.
[0004] It is especially desired to provide cleaning agents constituting a connection between
the classic cleaning method having a disinfecting character and the cleaning abilities
of useful bacteria.
[0005] Another technological problem directly involving the invention is providing a cleaning
agent of this type in a form fit to apply in currently used washing and laundry washing
appliances, especially in dishwashers and automatic washing machines, which are usually
configured to use a cleaning agent in a form having a particular tablet shape or self-dissolving
capsule containing a cleaning agent. In case of self-dissolving capsules, they are
currently manufactured, generally, with a film dissolving in water, containing polyvinyl
alcohol (PVOH), and the cleaning agent contained within is usually in liquid form.
An appropriate PVOH film is known to people skilled in the art, e.g. from the application
WO2014110356. In case of developing such capsules, it is necessary to achieve compatibility between
the cleaning agent and the polyvinyl film. This means that the liquid part and eventual
tablet part of the capsule should be compatible with the self-dissolving PVOH film.
Moreover, the cleaning agent formula should be stable (not subjected to physicochemical
changes), and the product should be effective at the same time.
[0006] Unexpectedly, the problems mentioned above have been solved by the present invention.
[0007] The invention relates to a self-dissolving capsule for preparation of washing solutions,
characterised in that it contains a washing agents and probiotic microorganisms, wherein
the capsule consists of two separate, sealed cavities, the first of which contains
the washing agent, whereas the second one contains a lyophilised or concentrated liquid
formulation of
Bacillus species probiotic bacteria, forming spores and displaying growth in temperature up
to 65°C, wherein the washing agent is a composition containing the following components:
a nonionic surfactant, a polycarboxylate, an anionic surfactant, a complexing agent
aiding the washing process and providing gloss, plasticisers, a phosphonate, hydrolytic
enzymes, a preservative, a fragrance, functional additives, and water.
[0008] Preferably, the capsule contains probiotic bacteria chosen from the following:
Bacillus subtilis, Bacillus pumilus, Bacillus vallismortis, Bacillus coagulans, Bacillus
lactis, and
Bacillus mojavensis, preferably spores of
Bacillus coagulans PCM 1843 strain.
[0009] Preferably, the washing agent contained in the capsule contains the following: a
nonionic surfactant in amount of 5 to 30 wt%, a polycarboxylate in amount below 7
wt%, an anionic surfactant in amount of 0 to 35 wt%, a complexing agent in amount
of 50 to 75 wt%, a plasticiser in amount below 20 wt%, a phosphonate in amount below
3 wt%, a hydrolytic enzyme in amount below 1 wt%, a preservative in amount below 1
wt%, a fragrance in amount below 1 wt%, a functional additive in amount below 1 wt%,
and water in amount below 4 wt%.
[0010] Preferably, the nonionic surfactant is chosen from the group containing the following:
C12-C14 ethoxylated alcohols, C8 alkyl glucoside, capryl decyl glucoside, alkyldimethylamine
oxide solution, sorbitan sesquioctanoate, alkoxylated fatty alcohol, 2-propylheptanol
ethoxilate, 2-ethylhexyl glucoside, alcohol alkoxylate, C8/10 methyl ester, preferably
chosen from the group containing: C12-C14 ethoxylated alcohols and C8 alkyl glucoside.
[0011] Preferably, the anionic surfactant is chosen from the group containing the following:
sodium p-cumenesulphonate; potassium 4-isopropylbenzenesulphonate; sodium 2-ethylhexyliminodipropionate;
sodium cocopropylenediamine propionate; decyl phosphoric acid; potassium salt, sodium
alkyl sulphate; sodium 2-ethylhexyl sulphate; ABS acid MEA salt; ABS acid TEA salt;
C12-C14 ethoxylated alcohols (1-2.5 EO), sulphates, sodium salts; MEA cocoate; TEA
cocoate, preferably chosen from the group consisting of: ABS acid MEA salt; ABS acid
TEA salt; C12-C14 ethoxylated alcohols (1-2.5 EO), sulphates, sodium salts; MEA cocoate;
TEA cocoate.
[0012] Preferably, the complexing agent is chosen from the group containing the following:
sodium carboxymethyl inulin; tetrasodium EDTA; N,N-bis(carboxymethyl)alanine trisodium
salt; glutamic acid, N,N-diacetic acid tetrasodium salt; sodium citrate, preferably
chosen from the group containing: sodium carboxymethyl inulin; glutamic acid, N,N-diacetic
acid tetrasodium salt.
[0013] Preferably, the polycarboxylate is chosen from the group containing the following:
aqueous solution of partially neutralised polycarboxylic acid (sodium salt); aqueous
solution of a polyacrylic acid sodium salt; preferably is an aqueous solution of partially
neutralised polycarboxylic acid (sodium salt).
[0014] Preferably, the functional additive is chosen from the group containing the following:
vinylpyrrolidone/vinylimidazole copolymer; sodium metasilicate; acylamide carboxylic
acid, alkanolamine salt; PEG-8 GMIS; Fluorescent Brightener 28; Undeceth-5, undecyl
alcohol, sodium lauryl sulphate, caprylyl pyrrolidone.
[0015] Preferably, the plasticiser is chosen from the group containing the following: glycerine,
propylene glycol, and sorbitol.
[0016] Preferably, the phosphonate is chosen from the group containing the following: proprietary
mixture of organophosphonic acid, sodium salts; aqueous solution of aminophosphonic
acid salt.
[0017] Preferably, the preservative is chosen from the group containing the following: 2-bromo-2-nitropropane-1,3-diol,
methylchloroisothiazolinone, methylisothiazolinone; methylisothiazolinone, benzisothiazolinone.
Preferably, the hydrolytic enzyme is chosen from the group containing the following:
protease, lipase, amylase, and cellulase.
[0018] Preferably, a substance from the following table is chosen as a dye, wherein the
particularly preferred substances are underlined.
Dye name |
Dysol Turquoise AXN50 Liquid |
Brilliant Blue E133 |
Violet 656271 |
Dysol Red 4B |
Rhodamine conc. 500% |
Acid Blue FG200% |
Acid Pure Green |
Dysol Light Blue |
Dysol Green |
Sanolin Blue AE90 |
Sanolin Blue NBL |
Puricolor Blue FBL |
Acid Amaranth |
Acid Orange II 143% |
Puricolor Red ARE 14 |
Puricolor Red ARE 52 |
Alizarin Blue RN-200 |
Acid Blue R150% |
Helion Turquoise Blue FGL166 |
SensiRinse Orange |
SensiRinse Green |
SensiRinse Blue |
SensiRinse Yellow |
SensiRinse Red |
SensiRinse Violet |
SensiRinse Black |
Liquitint Bright Yellow HP |
Liquitint Cyan 15HP |
Liquitint Blue HP |
[0019] Preferably, a commercially available substance from the following table is chosen
as a fragrance, wherein the particularly preferred substances are underlined.
Fragrance name |
Colour Action 9904P |
Spring Scent 7954P |
Olipic 5693P |
Calnival 6364P |
Active Fresh 5215 |
Active Fresh 8360 |
Sensi Fresh 4812 |
Active Fresh 5214 |
Sensi Fresh 0912 |
Air Color 1 (8730006) |
Air Color 2 (8730007) |
Air Color 3 (8730008) |
Air Color 4 (8730012) |
Air White 1 (8730009) |
Air White 2 (8730010) |
Air White 3 (8730011) |
Citrus Clean 3779 |
Citrus Clean 7699 |
Citrus Clean 3070 |
EFFPL 42314 Citrus Fizz |
EFFPL 42318 Platinum Flower |
EFFPL 42341 Platin Freshness |
EFFPL 42342 Aloe&Green Fruits |
EFFPL 42343 Green Tea&Rose |
EFFPL 42344 Pineapple&Tangerine |
EFFPL 42345 Strawberry&Rhubarb |
EFFPL 42346 Apple Garden |
EFFPL 42347 Black Grape |
[0020] The invention relates to a self-dissolving capsule for cleaning soiled hard surfaces
characterised in that, the soiled surface is washed with an aqueous solution obtained
by diluting the capsule of the present invention, defined above, in 2 to 10 litres
of water, wherein the cleaned surface is left to dry, after the washing process.
[0021] The proposed form of application of microorganisms enables isolating the components
acting antagonistically in separate cavities, and thus maintaining their high activity
and effectiveness. Simultaneously, the product protects the microorganisms from the
influence of concentrated materials during the step of enclosing inside the capsule
and under practical conditions (administration routes of biocomponents).
[0022] Product according to the invention contains a tablet, which allows obtaining a maximal
concentration of substances contained therein.
[0023] The application of microorganisms' technology enables introducing microorganisms
along with chemical substances in a single washing bath, also in automatic washing
systems (dishwashers, washing machines), by which they aid the cleaning cycle, and
by colonisation of outlets and surfaces of the device, they promote the hygiene maintenance.
[0024] The natural microbial enzymes carry out decomposition of organic substances, which
provides a possibility of decreasing the amount of chemical substances in the cleaning
agents - environmental aspect.
[0025] The microorganisms aid the cleaning processes by extending the washing cycle. By
colonisation of the washing surface, the 'good microbes' compete with pathogenic microorganisms
present on the washing surface, driving them out and ultimately improving the microflora
of the cleaning surface.
[0026] The embodiments of the invention have been described below, although they should
not be identified with the scope of the invention defined in the attached claims.
[0027] In regard to the classic cleaning, capsules according to the invention have a corresponding
level to that of available traditional products. Their advantage is performing a microbiological
cleaning process. In comparison to products not containing microorganisms, in case
of capsules according to the invention, a biofilm reduction and improvement of bacterial
flora by eliminating pathogenic microorganisms are observed. Applying the capsule
with probiotic on hard surfaces reduced survival of potentially pathogenic Gram+ bacteria
including
Staphylococcus aureus and
Enterococcus faecalis.
[0028] Bacteria inside appliances colonise hard to reach places and elements, and are not
fully washed out during rinsing processes. Capsules according to the invention induce
a change in the flora in direction of eliminating pathogenic microbes.
Example 1. Administration routes of biocomponents
[0029] Following methods of biocomponents application were verified:
- Single-cavity capsule - the formula basis and biocomponents are encapsulated in the
same cavity. The ingredients and the basis are applied jointly from a single cavity.
- Multi-cavity capsule (liquid/liquid) - antagonistic ingredients of the formula are
separated. Ingredients are applied from two cavities.
- Multi-cavity capsule (liquid/tablet) - antagonistic ingredients of the formula are
separated. Ingredients are applied from two cavities.
[0030] For the concept of multi-cavity liquid/tablet and liquid/liquid capsule, two variants
of the test were carried out:
Test package no. 1
[0031] A multi-cavity capsule of self-dissolving film was formed, in liquid/liquid liquid/tablet
(12 mm dimeter) phase according to the following criteria: capsule size 30 mm × 40
mm or approximate, total tablet mass not exceeding 24 g.
Test package no. 2
[0032] A multi-cavity capsule of self-dissolving film was formed, in liquid/liquid liquid/tablet
(16 mm dimeter or approximate) phase according to the following criteria: capsule
size 30 mm × 40 mm or approximate, total tablet mass shout not exceed 24 g.
[0033] At the same time, the cleaning processes efficiency test was performed, as well as
the washing bath parameters and individual formula components influence on stability
and maintaining the activity of biocomponents. For each concept, the possibility of
technological manufacturing of the product and the possibility of placing the recommended
biocomponent dosage inside a capsule were verified.
[0034] Introducing the tablet also provides a possibility of higher concentration of the
compounds, introducing peroxide substances into the formula, mutual separation of
peroxide compound and probiotics, which are negatively affected by them, and possible
introduction of probiotics in pressed form into the product.
Example 2. Technological capacity assessment of individual capsule forms
[0035] Single-cavity capsule - the formula basis and biocomponents are encapsulated in the
same cavity. The components and the basis are applied jointly from a single cavity.
There is no possibility of enclosing the water suspension of biocomponents available
on the market in a self-dissolving film - dissolving of the film occurs.
[0036] In a preferred embodiment, probiotic in powder form should be enclosed in a self-dissolving
film.
1. Multi-cavity capsule (liquid/liquid)
[0037] (Liquid/liquid) capsules using a cavity having 12 mm and 16 mm diameter have been
presented in fig. 1. The smaller cavity (intended for biocomponents) has a volume
of 5 ml, whereas the liquid part (the larger cavity intended for chemical substances)
has a volume of 12 ml. Total mass of the liquid/liquid capsule was about 19 g.
[0038] Due to significant differences in volume, and therefore the dosing time required,
the product is extremely difficult technologically. There is no possibility of enclosing
the water suspension of biocomponents available on the market in a self-dissolving
film - dissolving of the film occurs. The probiotic content contained in the smaller
cavity is too low comparing to that recommended required in a washing bath.
[0039] A multi-cavity liquid/12 mm diameter tablet capsule allows using an about 2 g tablet
and obtaining a liquid part volume of about 12 ml in the first, and 17 ml in the second
case. The total mass of the capsule with a cavity of 12 ml volume is 16 g, and of
the capsule with 17 ml cavity is 21 g.
[0040] Both sachet types fit into the dishwasher detergent cup. The tablet position inside
the capsule is suitable for its shape. The tablet placement in subsequent samples
in relation to the liquid cavity is constant. The film is sealed. The mass in relation
to the assumed capsule size in both cases is below 24 g. The capsule with a cavity
of 17 ml volume looks 'bulgy', the capsule does not touch the table with the whole
surface. Folds are forming around the tablet - further development on flattening them
is required. The cavity having 12 ml volume for the liquid and 12 mm for the tablet
has been assessed as too small to contain the proper biocomponent dose.
[0041] Liquid/tablet (16 mm) capsule: Increasing the tablet diameter allows obtaining a
more stable tablet while cutting the heat-seal. A smaller cavity required for the
tablet/liquid is less cone-like, which positively affects the stage of enclosing the
tablet/liquid in a film. The amount of active substance that can be contained in a
capsule of this form was increased to 3 g and corresponds to the recommended dose.
[0042] As a result of performed tests, a most preferred capsule form was determined: 16
mm (smaller cavity) and 16 ml (cavity with liquid). An exemplary capsule of this type
has been presented in Fig. 2.
[0043] Figures 3-5 illustrate different views of the capsule according to the invention,
having a coating made of PVOH
Example 3. Tested variants of the capsules
[0044] Generally, the capsule is filled with an aqueous solution containing:
nonionic surfactants, polycarboxylates, anionic surfactants, phosphonates, enzymes,
a preservative, a fragrance composition and microorganisms (preferably about 1 wt%).
[0045] Microorganisms are contained in the tablet portion. The capsule is made of a PVOH
self-dissolving film.
[0046] The method of administering the microorganisms in dry form ensures their stability
in the system. Microorganisms contained in the tablet in form of spores are activated
by contact with water.
[0047] The capsule manufacture process proceeds in two steps. The first step is preparing
the tablet. This stage involves the process of ingredient mixing, and next pressing
on the device to a tablet form. The pressing step is carried out under pressure, which
ensures intactness of cell wall structures. The second step involves a process of
forming the capsule, in which the dosing step of the liquid part and tablet incorporation
is achieved at the same time. The process is carried out under strictly controlled
conditions of about 23°C and 45% humidity. Performed tests of film stability confirm
the stability of its structure, and therefore the stability of the capsule under these
formulating conditions.
[0048] Depending on the liquid part composition, the capsule can be applied in appliances
for dishwashing, laundry washing, and, after diluting, also for cleaning other hard
surfaces.
[0049] Various formula compositions were tested:
A dishwasher capsule (comparative example)
nonionic surfactants in amount of 15-30%
polycarboxylates in amount of 5-15%
anionic surfactants in amount of <5%
phosphonates
enzymes
preservative
fragrance composition
microorganisms <1%
[0050] The tablet contained in the capsule displayed a change of parameters - bulging (about
1 mm height change, which consequently results in tearing of the film.
[0051] The liquid part penetrates into the tablet part, which consequently leads to exposure
of the microorganisms on aggressive chemical substances and their elimination.
[0052] A dishwasher capsule with an addition of a peroxide substance (comparative example):
nonionic surfactants in amount of 15-30%
polycarboxylates in amount of 5-15%
anionic surfactants in amount of <5%
peroxide compounds <5%
phosphonates
enzymes
preservative
fragrance composition
microorganisms <1%
[0053] The peroxide substances are desired in the formula systems due to the fact that they
enhance their effectiveness and efficiency. The tests employed sodium percabonate.
However, peroxide substances are highly hygroscopic. One of the stages of forming
the capsule involves binding (gluing) the upper and lower self-dissolving film by
spraying it with water. The tablet with an addition of a peroxide compound displayed
a strong bulging effect and was tearing the film. Product was not stable in time.
The negative effect was observed already 2 weeks after the product manufacture.
[0054] Applying standard materials such as Marlox 154, Not Surf, Rokanol L7W, Rokanol IT
in anionic systems, anionic compound systems with hydrotropes, resulted in lack of
formula stability and their delamination.
[0055] The preferred embodiments of capsules according to the present invention are the
following:
- 1. A capsule for automatic dishwashing. The form of the capsule itself is highly preferred.
It allows application of precisely specified and validated amount of detergent, thus
preventing an excess of chemical agents from being introduced to the environment.
The capsule is characterised by simplicity and quickness of use. It is ready to use
immediately after taking out of the package. The application is performed by placing
the capsule in a dishwasher cup intended for this use and choosing an appropriate
program. The capsule can be used for all washing programs. One capsule is sufficient
and adequate for performing an effective washing process.
- 2. A capsule for automatic laundry washing promoting the maintenance of hygiene of
the appliance. The microorganisms are introduced jointly with the washing agents.
The capsule form is highly preferred. It allows application of precisely specified
and validated amount of detergent, thus preventing an excess of chemical agents from
being introduced to the environment. The capsule is characterised by simplicity and
quickness of use. It is ready to use immediately after taking out of the package.
The application is performed by placing the capsule in the washing machine drum and
choosing an appropriate program. The capsule can be applied in all washing programs.
One capsule is sufficient and adequate for performing an effective washing process
of typically dirty laundry. In case of very dirty laundry, using two capsules is required.
- 3. A capsule for cleaning of hard surfaces. Application is performed by dissolving
a single capsule in about 5 I of water, and subsequent washing of soiled surface.
The process does not require rinsing of the washed surface.
[0056] Tests described in the following example employ the following washing agent formulas:
WASHING GEL
No. |
Formula component |
Content [%] |
Effect on bacteria |
1. |
Alkyl alcohol ethoxylate (C10-C16) |
15-30 |
Bacteriostatic / bactericidal |
2. |
Propylene glycol |
15-30 |
Bacteriostatic / bactericidal |
3. |
Glycerine |
15-30 |
Stabilizes the bacteria / utilized as carbon and energy source |
4. |
Dodecylbenzene sulfonic acid |
15-30 |
Highly bactericidal |
5. |
Water |
< 15 |
In low concentration (9%) increases the effectiveness of bactericidal components |
6. |
Coconut acid |
< 5 |
Bacteriostatic / can be utilized as carbon and energy source |
7. |
Monoethanolamine |
<5 |
Bacteriostatic / bactericidal |
8. |
Proprietary mixture of organophosphonic acid, sodium salts |
< 1 |
Bactericidal |
9. |
Stain remover |
1-5 |
Bacteriostatic / bactericidal |
10. |
Fragrance |
< 1 |
Bacteriostatic |
11. |
Protease |
< 1 |
Bacteriostatic / bactericidal |
12. |
Lipase |
< 1 |
Bacteriostatic / bactericidal |
13. |
Cellulase |
< 1 |
No effect / can be utilized as carbon and energy source |
14. |
EASY WET : Undeceth-5 Undecyl alcohol Sodium lauryl sulphate Caprylyl Pyrrolidone |
< 1 |
Highly bactericidal |
15. |
Vinylpyrrolidone/ Vinylimidazole Copolymer |
< 1 |
No effect |
16. |
Carboxymethyl inulin, sodium salt solution |
< 1 |
Bacteriostatic / bactericidal |
17. |
Dye |
<0.1 |
Bacteriostatic / bactericidal |
18. |
2-Bromo-2-Nitropropane-1,3-Diol Methylchloroisothiazolinone, Methylisothiazolinone |
<0.5 |
Highly bactericidal |
DISHWASHING GEL
No. |
RAW MATERIAL |
Content [%] |
Effect on bacteria |
1. |
Glycerine |
15-30 |
Stabilizes the bacteria / utilized as carbon and energy source |
2. |
Sorbitol |
< 15 |
Stabilizes the bacteria / utilized as carbon and energy source |
3. |
Water |
< 15 |
In low concentration (9%) increases the effectiveness of bactericidal components |
4. |
Propylene glycol |
< 15 |
Bacteriostatic / no effect |
5. |
Sodium citrate |
< 15 |
Can be utilized as carbon and energy source. However it also chelates essential divalent
ions, thus inhibiting survival of bacteria. |
6. |
Polyacrylic acid, partially neutralized, sodium salt in water |
15-30 |
Bacteriostatic |
7. |
Polyacrylic acid, neutralized, sodium salt in water |
15-30 |
Bacteriostatic |
8. |
Monoethanolamine |
5-10 |
Bacteriostatic / bactericidal |
9. |
Alcohols, C12-C14 (even numbers), ethoxylated propoxylated (>2.5 moles EO/PO) |
< 5 |
Bacteriostatic / can be utilized as carbon and energy source |
10. |
Mixture of organophosphonic acid, sodium salt in water |
< 5 |
Bactericidal |
11. |
Protease |
< 5 |
Bacteriostatic / bactericidal |
12. |
Amylase |
< 5 |
No effect / can be utilized as carbon and energy source |
13. |
Polyacrylic acid (carbomer) |
< 5 |
Bacteriostatic |
14. |
Disodium metasilicate |
< 1 |
Bacteriostatic / no effect |
15. |
Fragrance |
< 1 |
Bacteriostatic |
16. |
2-Bromo-2-nitropropane-1,3-diol 2-octyl-2H-isothiazol-3-one |
< 0.5 |
Highly bactericidal |
17. |
Dye |
< 0.1 |
Bacteriostatic / no effect |
Example 4. Influence of physicochemical parameters, changing environment and washing
agent formula components on biocomponent activity in changing environments
[0057] Tests of pH influence on microbial survival in the probiotic were performed. The
maximum survival temperature of microbes isolated from the probiotic was determined
- the maximum temperature growth for probiotics was 58°C, as well as the thermal death
time of the probiotics in temperature of 100°C. Moreover, test of probiotics' survival
in different washing agent formulas were performed. It has been determined that washing
mixture components in high concentrations totally inhibit probiotic growth, displaying
very high bactericidal properties towards them.
[0058] At the same time, unexpectedly, the tests demonstrated a possibility of survival,
especially in spore form, of chosen
Bacillus sp. bacteria constituting the probiotic during washing process using the washing agent
diluted to the working concentration. For this reason, in the finished product, microbes
should be contained in a separate cavity.
[0059] A summary of preformed tests is presented in the following table.
Table 1. A summary report of thermostability, pH influence and microbial survivability
tests in concentrated washing agents (so called formulas) and washing baths in working
dilutions.
No. |
Tested strain |
pH |
Temperature |
Survivability in the formula |
Survivability in the washing bath |
1 |
Commercial liquid probiotic BadloxR XL100x Ospray Biotechnics Inc. (mixture of Bacillus sp. |
Bacteria incubated in a growth medium, as well as in the tap water, are resistant
to a wide |
Bacteria are highly thermostable, exhibiting cell division up to the temperature of
58°C. In hibernation state |
Death after mixing with tested formulas of washing and cleaning gels. |
Probiotic bacteria used in the temperature range of dishwasher washing and in the
chemical environment generated by the capsules survive a |
|
probiotic strains) |
range of pH, at least 4-10. |
they survive 100°C for over 18h (low percent of living cells). |
|
multiple washing cycle. |
2 |
Commercial probiotic in powder form BPB-100 Ospray Biotechnics Inc. (mixture of Bacillus sp. probiotic strains) |
Bacteria incubated in a growth medium, as well as in the tap water, are resistant
to a wide range of pH, at least 4-10. |
Bacteria are highly thermostable, exhibiting cell division up to the temperature of
58°C. In hibernation state they survive 100°C for over 18h (low percent of living
cells). |
Death after mixing with tested formulas of washing and cleaning gels. |
Probiotic bacteria used in temperature range of dishwasher washing and in the chemical
environment generated by the capsules survive a multiple washing cycle. |
3 |
Bacillus coagulans strain - live bacteria |
The bacterial strain exhibits good survivability in pH 5, 7, and 8, in temperatures
of 30, 40, and 50°C. In temperature of 60°C, a satisfactory survivability was recorded
only in pH 8. Higher temperatures act bactericidally on tested bacteria. |
Test were not performed - bacteria strains died out already in diluted solutions. |
The washing gel exhibits a highly bactericidal effect on tested bacteria strains.
No satisfactory survivability of bacterial cells was observed in any tested conditions
(pH and temperature) in the presence of washing gel. |
|
Polish Collection of Microorganisms, access number PCM 1843 |
4 |
Lactococcus lactis strain- live bacteria |
The bacterial strain exhibits good survivability in pH 5, 7, and 8, in temperatures
of 30, 40, and 50°C. In temperature of 60°C, a satisfactory survivability was recorded
only in pH 8. Higher temperatures act bactericidally on tested bacteria. |
Test were not performed - bacteria strains died out already in diluted solutions. |
The washing gel exhibits a highly bactericidal effect on tested bacteria strains.
No satisfactory survivability of bacterial cells was observed in any tested conditions
(pH and temperature) in the presence of washing gel. |
|
Polish Collection of Microorganisms, access number PCM 476 |
5 |
Bacillus coagulans - spores |
Bacillus coagulans spores are characterised by a good survivability in tested washing and cleaning formulas,
in tested pH and temperature range. |
Not performed |
Tested temperature did not exhibit an inhibiting effect on spore count, except for
the temperature of 100°C. However, even after incubation in temperature of 100°C,
bacterial spores capable of growing were found. |
|
Polish Collection of Microorganisms, access number PCM 1843 |
|
Commercial liquid or solid probiotic (points 1 and 2 in Table 1)
[0060] Stability tests of
Bacillus sp. bacteria in various temperatures and various pH of the laundry washing and washing
bath were performed (concerning pts. 1 and 2 of Table 1).
[0061] The tests involved the following steps:
- preliminary determination of the optimal temperature for liquid and solid probiotic
samples,
- selection of type and nature of microbiological medium (composition and form) - the
growth medium recommended by the manufacturer was chosen (LA) as typically averagely
nutrient-rich medium with average sodium chloride concentration and neutral pH, on
which typically Bacillus sp. genus bacteria exhibit good growth. Firstly, streaking was performed using an
inoculation loop from a 10 microlitre droplet of thoroughly mixed probiotic in order
to isolate the microbial species and strains present therein,
- temperature selection (scale, minimum, maximum, step) - a wide range of temperature
was chosen, starting from room temperature, 30°C and 37°C for mesophiles, 55°C for
thermophiles, and 65°C and 70°C for hyperthermophiles.
[0062] Observed results concerning the optimal temperature for liquid probiotic bacteria
(1) are summarised in the following table.
Temperature |
Growth |
Room temperature |
+ |
30°C |
+++ |
37°C |
+++ |
55°C |
++ |
65°C |
- |
70°C |
- |
[0063] Observed results concerning the optimal temperature for solid probiotic bacteria
(1) are summarised in the following table.
Temperature |
Growth |
Room temperature |
+ |
30°C |
+++ |
37°C |
+++ |
55°C |
++ |
65°C |
- |
70°C |
- |
[0064] A pH influence on survivability of microbes present in probiotics - solid and liquid,
was tested. For this reason a series of liquid growth media was prepared, having an
increasing pH: 5, 6, 7, 8, 9, 10. The probiotic sample was incubated in growth media
prepared in this manner, in room temperature in an increasing pH environment, mixed
in 1:100 ratio. Afterwards, 0.1 ml of such suspension was inoculated, in order to
obtain a bacterial lawn, on a LA growth medium and incubated under optimal conditions
of 37°C for 24 hours. Established incubation times in different pH: 1 hour, 24 h,
48 h, 2 × 48 h (4 days) and 7 days.
[0065] Results: After 4 day incubation in 5-10 pH range, an intense growth was observed
for each of tested pH values for both probiotic samples (liquid 2 and solid) - no
change in relation to 1 hour incubation - tested microbes tolerate a wide range of
growth medium pH: 5, 6, 7, 8, 9, 10, even despite the 100-fold dilution applied.
[0066] Afterwards, a survivability test of the probiotic microbes in concentrated formulas
(washing liquid, laundry washing liquid) was performed.
[0067] In order to carry out the survivability test, 1:10 was arbitrarily chosen as maximal
possible probiotic dilution in the tested medium, which equals a 10% content of the
microbial medium in the tested formula (10+90). Next, two approaches were applied
in order to verify the survivability of the microbes in this environment in comparison
with the double control: a 1:10 dilution of probiotic in the growth medium and an
inoculation immediately after mixing with the tested medium (washing liquid or laundry
washing liquid). The inoculations were performed at time: 0, 1 h, 2 h, 3 h, 6 h, 20
h, accordingly. Two analytical approaches were applied:
A mixture of the probiotic and the tested medium was incubated at time: 0 (inoculated
immediately after mixing), 1 h, 2 h, 3 h, 6 h, 20 h. Each time after the determined
incubation time in the tested medium elapsed, plate inoculations on optimal growth
media were performed in order to obtain the bacterial lawn (0.1 ml) and incubated
at optimal temperature.
[0068] Test results of the influence of washing liquid and laundry washing liquid on microbes
used in the probiotics are presented below:
Incubation time in the tested medium [room temp.] |
Growth intensity on a solid medium - P2 AFTER INCUBATION IN THE WASHING LIQUID |
Growth intensity on a solid medium - P2 AFTER INCUBATION IN THE LAUNDRY WASHING LIQUID |
0 |
no growth |
no growth |
1 h |
no growth |
no growth |
2 h |
no growth |
no growth |
3 h |
no growth |
no growth |
6 h |
no growth |
no growth |
20 h |
no growth |
no growth |
[0069] The obtained results were verified in a subsequent experiment in liquid growth media.
The tested samples were inoculated in liquid growth media by means of an inoculation
loop, thus transporting about 10 microlitres of the tested sample into 5 ml of the
growth medium (1:500 dilution). This approach would enable catching even individual
microbial cells surviving in the laundry washing/washing liquid formula or their spores,
and effective growth under optimal conditions, which would by demonstrated by turbidity
of the liquid growth medium.
[0070] The observed results are presented in the following table:
Incubation time in the tested medium [room temp.] |
Growth intensity in a liquid medium - P2 AFTER INCUBATION IN THE WASHING LIQUID |
Growth intensity in a liquid medium - P2 AFTER INCUBATION IN THE LAUNDRY WASHING LIQUID |
0 |
no growth |
no growth |
1 h |
no growth |
no growth |
2 h |
no growth |
no growth |
3 h |
no growth |
no growth |
6 h |
no growth |
no growth |
20 h |
no growth |
no growth |
[0071] The culture samples in the liquid growth medium were also analysed by a spectrophotometric
method (absorbance change for 600 nm light wavelength). Obtained results confirmed
lack of bacterial growth.
[0072] CONCLUSIONS: The concentrated laundry washing liquid and washing liquid fully eliminate
the microbial growth, displaying very high bactericidal properties.
[0073] Probiotic survivability (pos. 1 and 2) in dilutions used in the washing process.
[0074] In order to perform the survivability test, 3 g weighted amounts of the powder probiotic
(S) were prepared. For effective suspension in the tested medium, the suspension in
tap water was prepared in 1:5 ratio. Whole suspensions were mixed into the previously
prepared working dilutions according to the following scheme:
- 1) 13 ml of washing liquid for 2.5 I
- 2) 13 ml of washing liquid for 5.0 I
- 3) 24 ml of washing liquid for 2.5 I
- 4) 24 ml of laundry washing liquid for 5 I
- 5) 2.5 l of the growth medium - control
- 6) 5.0. l of the growth medium - control
[0075] Next, three experimental approaches were applied, in order to test the microbial
survivability in this environment comparing to a double control of probiotic suspension
in a growth medium, and the inoculation immediately after mixing with the tested medium
(washing liquid or laundry washing liquid). The inoculations were performed at times:
0, 1 h, 2 h, 3 h, 6 h, 24 h, accordingly.
[0076] After mixing the probiotic with the tested working dilution, the mixture was incubated
at time: 0 (inoculation immediately after mixing), 1 h, 2 h, 3 h, 6 h, 24 h. Each
time after the incubation time in the tested medium has elapsed, microbiological inoculations
on a plate (0.1 ml), on optimal growth media were performed, and incubated at optimal
temperature.
[0077] Results of observations concerning the influence of washing liquid and laundry washing
liquid in a working dilution of 13 ml (washing) / 24 ml (laundry washing) for 2.5
or 5.0 l of tap water, determining the microbiological stability (survivability) of
the probiotic compared to the control in the growth medium. The observations are summarised
in the following table.
Incubation time in the tested medium
[room temp.] |
Growth intensity in the liquid growth medium - 3 g of the solid probiotic after mixing
with 13 ml of the washing liquid /2.5 l of water |
Growth intensity in the liquid growth medium - 3 g of the solid probiotic after mixing
with 13 ml of the washing liquid /5 l of water |
Growth intensity in the liquid growth medium - 3 g of the solid probiotic after mixing
with 24 ml of the washing liquid /2.5 l of water |
Growth intensity in the liquid growth medium - 3 g of the solid probiotic after mixing
with 24 ml of the washing liquid /5 l of water |
0 |
+++ |
+++ |
+++ |
+++ |
1 h |
+++ |
+++ |
+++ |
+++ |
2 h |
+++ |
+++ |
+++ |
+++ |
3 h |
+++ |
+++ |
+++ |
+++ |
6 h |
+++ |
+++ |
+++ |
+++ |
24 h |
+++ |
+++ |
+++ |
+++ |
Conclusions:
[0078] All tested dilutions of the washing liquid and the laundry washing liquid allow for
survival of
Bacillus sp. bacteria of the probiotic. Thus, it is possible to apply a combination of washing/laundry
washing liquid and the probiotics, as long as they are physically separated in the
applied package and their release will occur with simultaneous diluting in water.
Test concerning the chosen probiotic strains (see points 3, 4 and 5 in Table 1)
Tests of bacterial stability in various temperatures and various pH of the laundry
washing and washing bath (concerning pts. 3 and 4 of Table 1)
[0079] The tests employed cell suspension of chosen bacteria having a cell count of an order
of 10
6 cells/ml. An appropriate volume of the suspension was taken and transported to a
laundry washing bath with a given pH, prepared beforehand. The final cell count in
the bath was 10
4 cells/ml. Afterwards, the bath along with the cells were placed in a defined temperature
for 30 minutes. After this time, 1 ml of the suspension was taken and a pour plate
prepared, using an earlier developed, best growing mixture as a growth medium.
Table 2.
Lactococcus lactis bacteria cell count after 30 minutes incubation in the laundry washing bath under
the tested conditions.
pH |
Control, without the laundry washing gel |
Tested sample, with the laundry washing gel |
Temperature [°C] |
Temperature [°C] |
30 |
40 |
60 |
30 |
40 |
60 |
5 |
9.7 × 104 |
6.8 × 104 |
0.5 |
0.0 |
0.0 |
0.0 |
7 |
6.8 × 104 |
1.7 × 104 |
0.0 |
0.0 |
0.0 |
0.0 |
8 |
9.6 × 104 |
6.6 × 104 |
1.7 × 104 |
0.0 |
0.0 |
0.0 |
Table 3.
Bacillus coagulans bacteria cell count after 30 minutes incubation in the laundry washing bath under
the tested conditions.
pH |
Control, without the laundry washing gel |
Tested sample, with the laundry washing gel |
Temperature [°C] |
Temperature [°C] |
30 |
40 |
60 |
30 |
40 |
60 |
5 |
7.0 × 104 |
5.0 × 104 |
0,0 |
0.0 |
0.0 |
0.0 |
7 |
11.5 × 104 |
5.7 × 104 |
4,5 |
0.0 |
0.5 |
0.0 |
8 |
8.0 × 104 |
6.2 × 104 |
31 |
2.0 |
0.5 |
0.0 |
Table 4.
Lactococcus lactis bacteria cell count after 30 minutes incubation in the washing bath under the tested
conditions.
pH |
Control, without the washing gel |
Tested sample, with the washing gel |
Temperature [°C] |
Temperature [°C] |
50 |
60 |
70 |
100 |
50 |
60 |
70 |
100 |
5 |
11 |
0.0 |
0.0 |
0.0 |
14.5 |
0.0 |
0.0 |
0.0 |
7 |
3 |
0.0 |
0.0 |
0.0 |
3 |
0.0 |
0.0 |
0.0 |
8 |
7.5 |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
Table 5.
Bacillus coagulans bacteria cell count after 30 minutes incubation in the washing bath under the tested
conditions.
pH |
Control, without the washing gel |
Tested sample, with the washing gel |
Temperature [°C] |
Temperature [°C] |
50 |
60 |
70 |
100 |
50 |
60 |
70 |
100 |
5 |
9.0 × 102 |
1.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
7 |
8.5 × 102 |
1.0 |
0.5 |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
8 |
8.0 × 102 |
0.5 |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
Tests of bacterial stability in various temperatures and various pH of the laundry
washing and washing bath (concerning pt. 5 of Table 1).
[0080]
Table 6.
Bacillus coagulans bacteria spore cell count [spores/ml] after 30 minutes incubation in the laundry
washing bath under the tested conditions.
pH |
Control, without the laundry washing gel |
Tested sample, with the laundry washing gel |
Temperature [°C] |
Temperature [°C] |
30 |
40 |
60 |
30 |
40 |
60 |
5 |
5.5 × 105 |
5.4 × 105 |
7.1 × 105 |
6.9 × 105 |
9.8 × 105 |
10.6 × 105 |
7 |
3.8 × 105 |
5.8 × 105 |
7.0 × 105 |
9.1 × 105 |
10.3 × 105 |
10.4 × 105 |
8 |
6.0 × 105 |
6.8 × 105 |
6.8 × 105 |
8.2 × 105 |
10.2 × 105 |
9.4 × 105 |
Table 7.
Bacillus coagulans bacteria spore cell count [spores/ml] after 30 minutes incubation in the washing
bath under the tested conditions.
pH |
Control, without the washing gel |
Tested sample, with the washing gel |
Temperature [°C] |
Temperature [°C] |
50 |
60 |
70 |
100 |
50 |
60 |
70 |
100 |
5 |
10.1 × 105 |
9.3 × 105 |
8.3 × 105 |
3.0 × 100 |
10.3 × 105 |
10.8 × 105 |
10.0 × 105 |
3.0 × 100 |
7 |
9.0 × 105 |
8.8 × 105 |
8.5 × 105 |
6.5 × 100 |
9.2 × 105 |
10.2 × 105 |
11.3 × 105 |
1.5 × 102 |
8 |
8.7 × 105 |
7.9 × 105 |
8.3 × 105 |
6.7 × 100 |
10.9 × 105 |
8.3 × 105 |
10.0 × 105 |
9.2 × 100 |
[0081] The tests involved:
- proliferation of Bacillus coagulans bacteria,
- formation of spores of these bacteria,
- separation of spores from the vegetative cells,
- freezing and lyophilisation of these spores,
- stability tests of obtained spores in various pH and temperatures, in the washing
and laundry washing formulas (analogically to the laundry washing process: 30, 40,
60 °C; analogically to the washing process in the dishwasher: 50-60-70°C, drying at
about 100°C).
[0082] The tests were performed under the so called dirty conditions, that is with an addition
of 3 g of lecithin for 1 litre of the mixture (the added lecithin simulates the organic
matter load, similarly to the organic contaminations).
[0083] The originally prepared suspension contained 1.5 × 10
7 of bacterial spores. Subsamples were taken from this suspension, and introduced to
the reaction mixtures (washing and laundry washing formulas with various pH values).
[0084] The final spore count in the laundry washing formula was of order 10
5, whereas in the washing formula it was 10
6.
Conclusions:
[0085]
- 1. The chosen bacterial strains can be easily grown in laboratory and semi-industrial
conditions.
- 2. The tested bacterial strains display good survivability in pH 5, 7 and 8 in temperatures
of 30, 40 and 50°C. In temperature of 60°C, a satisfying survivability was recorded
only for pH 8. Higher temperatures are highly bactericidal for tested bacteria.
- 3. The laundry washing gel displays highly bactericidal influence on the tested bacterial
strains. Good survivability of the bacterial cell was not recorded in any of the testing
conditions (pH and temperature), in the presence of the laundry washing gel.
- 4. The washing gel also displays highly bactericidal influence on the tested bacterial
strains. Good survivability of the bacterial cell was not recorded in any of the testing
conditions (pH and temperature), in the presence of the washing gel.
- 5. Solutions of washing and laundry washing gels display high bactericidal influence
on the microbes in the vegetative form.
- 6. Solutions of washing and laundry washing gels do not display a negative influence
on the microbes in spore form.
- 7. The composition may employ Bacillus sp. probiotic strains of Risk Group 1, forming spores, displaying growth in temperature
up to of 65°C.
Example 5. Washing tests
[0086] For the chosen preferred variants of embodiments of the capsule according to the
invention, washing tests were performed.
[0087] An experimental dirty surface was washed with the water solution obtained by dissolving
the capsule according to the invention in a 2 to 10 litres volume of water, wherein
after finishing the washing process, the cleaned surface was left to dry. The tests
were performed in commercially available dishwasher machines.
[0088] Obtained results are summarised in the following table.
Table 8. Washing tests results
Formulation no. |
Probiotic administration |
Classical washing efficiency results |
Survivability of microorganisms after the washing process |
20/2014 |
Probiotic added in powder form to the liquid form |
milk - 52.77% |
According to the survivability tests, the formulation components acted bactericidally
on BPB-100 OSPREY microorganisms |
yolk - 80.00% |
plates/cereal - 72.87% |
8/2015 |
Probiotic in a tablet |
Visual evaluation: |
Applying the washing gel with addition of probiotic to washing the tested surfaces
lowered the survivability of potentially pathogenic G+ bacteria. |
Surface without streaks, dirt, after washing with gloss |
|
Decrease of the cell count of these bacteria was of one order of magnitude. |
13/2015 |
Probiotic in a tablet |
milk - 93.07% |
The probiotics inhabit sides and hard to read areas of the appliances. |
yolk - 52.51% |
plates/cereal - 87.51% |
Tested dilutions of the laundry washing liquid and the washing liquid enable bacterial
survivability. |
36/2015 |
Probiotic in a tablet with an addition of percarbonate |
milk - 89.44% |
The active oxygen displays highly bactericidal influence on microorganisms. |
yolk - 77.8% |
plates/cereal - 72.5% |
46/2015 |
Probiotic in a tablet |
milk - 95.00% |
The probiotics inhabit sides and hard to read areas of the appliances. |
yolk - 78.86% |
plates/cereal - 92.49% |
Tested dilutions of the laundry washing liquid and the washing liquid enable bacterial
survivability. |
167/2016 |
Probiotic in a tablet |
milk - 93.02% |
The probiotics inhabit sides and hard to read areas of the appliances. |
yolk - 79.14% |
plates/cereal - 92.49% |
Tested dilutions of the laundry washing liquid and the washing liquid enable bacterial
survivability. |
[0089] In case of dishwasher products, the washing efficiency was determined by means of
an IKW test. The following criteria of washing efficiency evaluation were assumed:
milk about 90%, yolk about 75%, plates (starch dirt) - about 90%. Survivability of
microorganisms after the washing process, at the level not lower than 80% of the control
amount.
Formulation 20/2014
No. |
LIQUID |
[%] |
1 |
Propylene glycol |
6.98 |
2 |
Sorbitol |
9.60 |
3 |
Glycerine |
32.00 |
4 |
Carbopol |
0.53 |
5 |
Distilled water |
8.21 |
6 |
Sodium citrate |
4.31 |
7 |
Sokalan PA25 |
10.27 |
8 |
Sokalan PA30 |
10.27 |
9 |
Disodium metasilicate |
0.16 |
10 |
Monoethanolamine |
3.69 |
11 |
Cublen A4015 |
1.03 |
12 |
Everlase |
1.31 |
13 |
Termamyl ultra |
1.07 |
14 |
NatSurf |
10.27 |
15 |
Clean Citrus fragrance composition |
0.01 |
16 |
Parmetol N20 |
0.04 |
17 |
Dysol Light Blue (0.5%) dye |
0.26 |
18 |
Badlox® XL100x probiotic |
1.00 |
Formulation 36/2015
No. |
LIQUID |
[%] |
1 |
Propylene glycol |
5.00 |
2 |
Sorbitol |
4.75 |
3 |
Glycerine |
16.90 |
4 |
Carbopol |
0.65 |
5 |
Distilled water |
3.60 |
6 |
Sodium citrate |
6.00 |
7 |
Dissolvine GL47S |
19.00 |
8 |
Sokalan PA25 |
16.00 |
9 |
Sokalan PA30 |
16.00 |
10 |
Disodium metasilicate |
0.30 |
11 |
Monoethanolamine |
5.80 |
12 |
Cublen A4015 |
1.50 |
13 |
Marlox |
4.00 |
14 |
Clean Citrus fragrance composition |
0.01 |
15 |
Acticide MBS |
0.09 |
16 |
Dysol Green (0.5%) dye |
0.40 |
No. |
TABLET |
[%] |
1 |
Sodium percarbonate |
50.00 |
2 |
Heavy sodium carbonate |
15.36 |
3 |
Sodium bicarbonate |
7.00 |
4 |
Citric acid |
7.14 |
5 |
Heweten 101 |
4.00 |
6 |
Zinc stearate |
0.5 |
7 |
Cellulose |
4.00 |
8 |
Detergent |
3.00 |
9 |
Polyethylene glycol |
2.00 |
10 |
TAED |
2.00 |
11 |
Heweten 101 |
4.00 |
12 |
BPB-100 probiotic |
1.00 |
Formulation 13/2015
No. |
LIQUID |
[%] |
1 |
Propylene glycol |
6.40 |
2 |
Sorbitol |
9.20 |
3 |
Glycerine |
23.00 |
4 |
Carbopol |
0.80 |
5 |
Distilled water |
8.00 |
6 |
Sodium citrate |
7.00 |
7 |
Sokalan PA25 |
15.00 |
8 |
Sokalan PA30 |
15.00 |
9 |
Disodium metasilicate |
0.30 |
10 |
Monoethanolamine |
5.40 |
11 |
Cublen A4015 |
1.50 |
12 |
Excellenz P100 |
2.20 |
13 |
Effectenz S100 |
1.70 |
14 |
Marlox |
4.00 |
15 |
Fresh Odor fragrance composition |
0.05 |
16 |
Parmetol N20 |
0.05 |
17 |
Dysol Light Blue dye |
0.40 |
No. |
TABLET |
[%] |
1 |
Heavy sodium carbonate |
35.93 |
2 |
Anhydrous sodium sulphate |
21.43 |
3 |
Marvellenz1000/T-blend |
8.00 |
4 |
PROBIOTIC |
7.00 |
5 |
Sodium bicarbonate |
7.00 |
6 |
Citric acid |
7.14 |
7 |
Cellulose |
4.00 |
8 |
Detergent |
3.00 |
9 |
Polyethylene glycol |
2.00 |
10 |
Cellulose |
4.00 |
11 |
Zinc stearate |
0.50 |
Formulation 46/2015
No. |
LIQUID |
[%] |
1 |
Propylene glycol |
6.00 |
2 |
Glycerine |
10.00 |
3 |
Syntapon OD |
2.00 |
4 |
Sokalan PA25 |
22.50 |
5 |
Dissolvine GL47S |
28.00 |
6 |
Monoethanolamine |
5.70 |
7 |
Cublen A4015 |
3.00 |
8 |
Hostacor IT |
2.20 |
9 |
Caflon APG810 |
9.30 |
10 |
AG6202 |
9.30 |
11 |
Carboxyline 25 D Powder |
1.50 |
12 |
Acticide MBS |
0.0944 |
13 |
Citrus Clean 3779 fragrance composition |
0.10 |
14 |
Tap water |
0.30 |
15 |
Liquitint Bright Yellow |
0.0050 |
16 |
Puricolor FBL 5 |
0.0006 |
No. |
TABLET |
[%] |
1 |
Magnesium stearate |
0.50 |
2 |
Sodium sulphate |
32.50 |
3 |
Sodium citrate |
35.00 |
4 |
Sodium bicarbonate |
5.00 |
5 |
Citric acid |
5.00 |
6 |
Arbocel TF 0210 |
4.00 |
7 |
HEWETEN 101 |
4.00 |
8 |
Pluriol E 4000 Powder |
2.00 |
Polyglycol 4000 PS |
9 |
MARVELLENZ 1000 |
8.00 |
T-Blend Evity Blaze/Stainzyme Plus 70/3.6 |
10 |
Purafac LF300 |
3.00 |
11 |
Bacillus coagulans probiotic |
1.00 |
Formulation 167/2016
No. |
LIQUID |
[%] |
1 |
Glutamic acid, N,N-diacetic acid tetrasodium salt |
74.00 |
2 |
Alkyl glucoside |
8.50 |
3 |
Polyacrylic acid, partially neutralized, sodium salt in water |
6.30 |
4 |
Propylene Glycol |
4.30 |
5 |
Glycerine |
3.20 |
6 |
Mixture of organophosphonic acid, sodium salt in water |
2.30 |
7 |
Water |
0.61 |
8 |
Acylamide carboxylic acid, salt |
0.40 |
9 |
Carboxymethyl inulin |
0.25 |
10 |
Preservative: |
0.09 |
1,2-benzisothiazol-3(2H)-one |
2-methyl-2H-isothiazol-3-one |
11 |
Fragrance |
0.05 |
12 |
Dye Blue |
0.00035 |
13 |
Dye Yellow |
0.005 |
No. |
TABLET |
[%] |
1 |
Magnesium stearate |
0.50 |
2 |
Sodium sulphate |
32.50 |
3 |
Sodium citrate |
35.00 |
4 |
Sodium bicarbonate |
5.00 |
5 |
Citric acid |
5.00 |
6 |
Arbocel TF 0210 |
4.00 |
7 |
HEWETEN 101 |
4.00 |
8 |
Pluriol E 4000 Powder |
2.00 |
Polyglycol 4000 PS |
9 |
MARVELLENZ 1000 |
8.00 |
T-Blend Evity Blaze/Stainzyme Plus 70/3.6 |
10 |
Purafac LF300 |
3.00 |
11 |
Bacillus coagulans probiotic |
1.00 |
Formulation 167/2016
No. |
LIQUID |
[%] |
1.0 |
Glycerine |
13.00 |
1.0 |
Propylene glycol |
10.00 |
1.1 |
Distilled water |
6400 |
2.0 |
ABS acid |
20.00 |
3.0 |
Monoethanolamine |
6.8 |
4.0 |
Rokanol L7A |
20 |
6.0 |
Isopropyl alcohol |
2 |
7.0 |
Sensi Rinse 745301 Red Liquid (2,5% r-r) dye |
0.50 |
8.0 |
Fragrance composition |
1.00 |
9.0 |
Parmetol A28 |
0.05 |
No. |
TABLET |
[%] |
1 |
Magnesium stearate |
0,50 |
2 |
Sodium sulphate |
32.50 |
3 |
Sodium citrate |
35.00 |
4 |
Sodium bicarbonate |
5.00 |
5 |
Citric acid |
5.00 |
6 |
Arbocel TF 0210 |
4.00 |
7 |
HEWETEN 101 |
4.00 |
8 |
Pluriol E 4000 Powder |
2.00 |
Polyglycol 4000 PS |
9 |
MARVELLENZ 1000 |
8.00 |
T-Blend Evity Blaze/Stainzyme Plus 70/3.6 |
10 |
Purafac LF300 |
3.00 |
11 |
Bacillus coagulans probiotic |
1.00 |
Example 6. Stability of the liquid part of the formula and its compatibility with
the film
[0090] According to the invention, the capsule is filled with a mixture containing the following:
nonionic surfactants, polycarboxylates, anionic surfactants, complexing compounds,
plasticisers, phosphonates, enzymes, a preservative, a fragrance composition, functional
additives, water, and microorganisms (preferably about 1 wt%). Each group of components
listed above has a certain function on each step of washing process, i.e. wetting
the surface, which allows penetrating the dirt particles and detaching them from the
surface, water softening and removal of metal ions, acting as dispergators of dirt
surrounding the individual dirt particles and preventing their agglomeration, and
preventing the redeposition of dirt, cutting the dirt chains on smaller fragments,
or additives protecting the cleaned surfaces.
[0091] The nonionic surfactants chosen in the first step of the formula development have
not led to obtaining stable systems, they had low effectiveness in the washing process.
Attempts to additionally introduce anionic surfactants into the formula also did not
yield good results. The obtained formulation were characterised by excessively high
foam, which is not recommended for automatic washing systems.
[0092] A compound for wetting the surface was sought that would maintain compatibility with
the other elements of the formula.
[0093] A difficulty in developing a stable formulation of the liquid part of the capsule
was posed by its compatibility with the self-dissolving PVOH (polyvinyl alcohol) film,
having a natural, desired capability of dissolving in water. A system having the water
content in the formulation that would allow maintaining its proper structure at the
product stage and simplicity of dissolving in the washing baths, was searched for.
The research led to reduction of the water content introduced directly to the formula
from 7% to below 4%. Simultaneously, as part of the performed research, a method of
reducing the water content in the formula in a form contained in the materials was
investigated, by means of replacing them with materials having a higher concentration
or introducing thickeners and complexing compounds that bond water.
[0094] As part of the development; the next group of compounds found, having influence on
the film structure, were plasticisers. Their amount in the final formulas, in comparison
with the starting formulas, was lowered by about 50% and was on a level <20%. The
starting, high content of plasticisers originated from their additional function as
a solvent, which allowed introducing of thickeners into the formulas. Analysing the
water content and the plasticisers' share in the formulation was an essential element
for capsules functionality of keeping and maintaining its shape and proper properties
during the whole shelf life. Decision not to use the glucose-fructose syrup, as well
as reduction of glycerine and propylene glycol content in the formula, resulted in
an improvement of elasticity and reduction of plasticity of the capsule surface. The
choice of fundamental and auxiliary materials is based, on one hand, on achieving
the desired working properties, and on the other, minimising the amount of bound water
introduced into the formulation, allowed reducing the occurence of substance migration
through the PVOH film, and thus achieving the effect of dry capsule surface. This
was achieved also by applying more concentrated material replacements: replacing the
MGDA compound with the GLDA material - having a higher concentration and fulfilling
a similar function in the formula, reducing the amount of water introduced directly
to the basis. Attempts to apply a thickener that binds water contained in the formulation
were not fully successful, due to the fact that although a stable basis was obtained,
the effect of dry capsule surface was not achieved. Finally, the decision to use a
thickener was revoked. As a result of performed experiments, the following composition
of the optimal formula of the cleaning agent was determined:
|
Washing systems |
Laundry |
Nonionic surfactants |
6.2-10 % |
20-30% |
Complexing materials, aiding the washing process and providing gloss |
50-75% |
3% |
Plasticisers |
<20% |
<20% |
Polycarboxylates |
<7% |
<7% |
Anionic surfactants |
- |
35-30% |
Phosphonates |
<3% |
<3% |
Preservative |
<1% |
<1% |
Fragrance composition |
<1% |
<1% |
Dyes |
<1% |
<1% |
Water |
<4% |
<4% |
Functional additives |
<1% |
<1% |
Enzymes |
- |
<1%** |
Tested formulation systems, content percentage
Formula no. |
6 |
55 |
43 |
46 |
51 |
77 |
128 |
146 |
160 |
Nonionic surfactants |
21.6 |
27 |
3 |
4 |
5 |
0 |
0 |
0 |
15.2 |
Complexing materials, aiding the washing process and providing gloss |
0.15 |
0.15 |
11 |
12.5 |
18.3 |
34.1 |
30 |
35.67 |
28 |
Plasticisers |
27.3 |
16 |
38.9 |
42.5 |
35.5 |
27.75 |
23 |
16 |
16 |
Polycarboxylates |
0.2 |
1.3 |
28 |
26 |
28 |
27 |
32 |
32.33 |
22 |
Anionic surfactants |
17.8 |
27 |
|
|
|
|
8 |
10.63 |
7.49 |
Phosphonates |
0.7 |
0.7 |
2 |
2.15 |
2.2 |
2.15 |
3 |
3 |
3 |
Preservative |
1.2 |
0.09 |
0.09 |
0.09 |
0.09 |
0.09 |
0.09 |
0.09 |
0.09 |
Fragrance composition |
0.05 |
1 |
|
0.01 |
0.01 |
0.01 |
0.01 |
0.01 |
0.01 |
Dyes |
0.28 |
0.01 |
0.4 |
0.46 |
0.4 |
0.5 |
0.51 |
0.38 |
0.32 |
Water |
4.92 |
3.7 |
7 |
6 |
6.6 |
3 |
3 |
1.5 |
0 |
Functional additives |
7.2 |
10.25 |
6.5 |
3.2 |
3.9 |
5.4 |
0.4 |
0.4 |
7.9 |
Enzymes |
0.8 |
0.8 |
3.21 |
3.21 |
|
|
|
|
|
Soaps** |
17.8 |
12 |
|
|
|
|
|
|
|
**concerns the systems for laundry washing |
1. A self-dissolving capsule for preparation of washing solutions, characterised in that it contains a washing agents and probiotic microorganisms, wherein the capsule consists
of two separate, sealed cavities, the first of which contains the washing agent, whereas
the second one contains a lyophilised or concentrated liquid formulation of Bacillus species probiotic bacteria, forming spores and displaying growth in temperature up
to 65°C, wherein the washing agent is a composition containing the following components:
a nonionic surfactant, a polycarboxylate, an anionic surfactant, a complexing agent
aiding the washing process and providing gloss, plasticisers, a phosphonate, hydrolytic
enzymes, a preservative, a fragrance, functional additives, and water.
2. Capsule according to claim 1, characterised in that it contains probiotic bacteria chosen from the following: Bacillus subtilis, Bacillus pumilus, Bacillus vallismortis, Bacillus coagulans, Bacillus
lactis, and Bacillus mojavensis, preferably spores of the Bacillus coagulans PCM 1843 strain.
3. Capsule according to claim 1, characterised in that the washing agent contains the following: a nonionic surfactant in amount of 5 to
30 wt%, a polycarboxylate in amount below 7 wt%, an anionic surfactant in amount of
0 to 35 wt%, a complexing agent in amount of 50 to 75 wt%, a plasticiser in amount
below 20 wt%, a phosphonate in amount below 3 wt%, a hydrolytic enzyme in amount below
1 wt%, a preservative in amount below 1 wt%, a fragrance in amount below 1 wt%, a
functional additive in amount below 1 wt%, and water in amount below 4 wt%.
4. Capsule according to claim 1, characterised in that the nonionic surfactant is chosen from the group containing the following: C12-C14
ethoxylated alcohols, C8 alkyl glucoside, capryl decyl glucoside, alkyldimethylamine
oxide solution, sorbitan sesquioctanoate, alkoxylated fatty alcohol, 2-propylheptanol
ethoxilate, 2-ethylhexyl glucoside, alcohol alkoxylate, C8/10 methyl ester, preferably
chosen from the group containing: C12-C14 ethoxylated alcohols and C8 alkyl glucoside.
5. Capsule according to claim 1, characterised in that the anionic surfactant is chosen from the group containing the following: sodium
p-cumenesulphonate; potassium 4-isopropylbenzenesulphonate; sodium 2-ethylhexyliminodipropionate;
sodium cocopropylenediamine propionate; decyl phosphoric acid; potassium salt, sodium
alkyl sulphate; sodium 2-ethylhexyl sulphate; ABS acid MEA salt; ABS acid TEA salt;
C12-C14 ethoxylated alcohols (1-2.5 EO), sulphates, sodium salts; MEA cocoate; TEA
cocoate, preferably chosen from the group consisting of: ABS acid MEA salt; ABS acid
TEA salt; C12-C14 ethoxylated alcohols (1-2.5 EO), sulphates, sodium salts; MEA cocoate;
TEA cocoate.
6. Capsule according to claim 1, characterised in that the complexing agent is chosen from the group containing the following: sodium carboxymethyl
inulin; tetrasodium EDTA; N,N-bis(carboxymethyl)alanine trisodium salt; glutamic acid,
N,N-diacetic acid tetrasodium salt; sodium citrate, preferably chosen from the group
containing: sodium carboxymethyl inulin; glutamic acid, N,N-diacetic acid tetrasodium
salt.
7. Capsule according to claim 1, characterised in that the polycarboxylate is chosen from the group containing the following: aqueous solution
of partially neutralised polycarboxylic acid (sodium salt); aqueous solution of a
polyacrylic acid sodium salt; preferably is an aqueous solution of partially neutralised
polycarboxylic acid (sodium salt).
8. Capsule according to claim 1, characterised in that the functional additive is chosen from the group containing the following: vinylpyrrolidone/vinylimidazole
copolymer; sodium metasilicate; acylamide carboxylic acid, alkanolamine salt; PEG-8
GMIS; Fluorescent Brightener 28; Undeceth-5, undecyl alcohol, sodium lauryl sulphate,
caprylyl pyrrolidone.
9. Capsule according to claim 1, characterised in that the plasticiser is chosen from the group containing the following: glycerine, propylene
glycol, and sorbitol.
10. Capsule according to claim 1, characterised in that the phosphonate is chosen from the group containing the following: proprietary mixture
of organophosphonic acid, sodium salts; aqueous solution of aminophosphonic acid salt.
11. Capsule according to claim 1, characterised in that the preservative is chosen from the group containing the following: 2-bromo-2-nitropropane-1,3-diol,
methylchloroisothiazolinone, methylisothiazolinone; methylisothiazolinone, benzisothiazolinone.
12. Capsule according to claim 1, characterised in that the hydrolytic enzyme is chosen from the group containing the following: protease,
lipase, amylase, and cellulase.
13. A method for cleaning soiled surfaces, characterised in that the soiled surface is washed with an aqueous solution obtained by dissolving the
self-dissolving capsule defined in claims 1-12 in 2 to 10 litres volume of water,
wherein, after finishing the washing process, the cleaned surface is left to dry.