CA2124791C - Encapsulation of liquids in microorganisms - Google Patents
Encapsulation of liquids in microorganismsInfo
- Publication number
- CA2124791C CA2124791C CA 2124791 CA2124791A CA2124791C CA 2124791 C CA2124791 C CA 2124791C CA 2124791 CA2124791 CA 2124791 CA 2124791 A CA2124791 A CA 2124791A CA 2124791 C CA2124791 C CA 2124791C
- Authority
- CA
- Canada
- Prior art keywords
- cells
- micro
- organism
- bleach
- encapsulated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/39—Organic or inorganic per-compounds
- C11D3/3902—Organic or inorganic per-compounds combined with specific additives
- C11D3/3905—Bleach activators or bleach catalysts
- C11D3/3907—Organic compounds
- C11D3/391—Oxygen-containing compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/39—Organic or inorganic per-compounds
- C11D3/3902—Organic or inorganic per-compounds combined with specific additives
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/39—Organic or inorganic per-compounds
- C11D3/3902—Organic or inorganic per-compounds combined with specific additives
- C11D3/3905—Bleach activators or bleach catalysts
- C11D3/3907—Organic compounds
- C11D3/3917—Nitrogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
- C12N1/005—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor after treatment of microbial biomass not covered by C12N1/02 - C12N1/08
Abstract
Yeast or other microorganism cells for use in the encapsulation of liquids (e.g. liquid bleach activators for use in laundry detergent compositions) are deodorised by treatment with a peroxygen bleach, e.g. hydrogen peroxide.
Description
93/11869 ~ 12 4 7 9 L PCl/US92/10391 ENCAPSULATION OF LIQUIDS IN MICROORGANISMS
Field of the Invention The present invention relates to a method of reducing the odour of micro-organism cells. The invention also relates to the use of the resultant deodorised cells in a process for encapsulating a material, in which micro-organism cells are contacted with the said material, which material is in liquid form, whereby the said material is absorbed through the micro-organism cell wall and retained within the micro-organism cells. The invention also relates to liquids that have been encapsulated in that manner.
Backqround to the Invention The encapsulation of materials within micro-organism cells is well known. In EP-B-0,085,805 (Dunlop Limited), a method of encapsulation is described in which the micro-organism is contacted with an organic lipid-extending substance that is a solvent, or a micro-dispersing medium, for the material to be encapsulated, and simultaneously and/or subsequently the micro-organism is contacted with the material to be encapsulated, said material being employed as a solution or micro-dispersion in the organic lipid-extending substance, or in a further organic lipid-extending substance or in a liquid that is miscible with the first-mentioned lipid-extending substance, whereby both the organic lipid-extending substance and the material to be encapsulated are taken into and retained passively within the micro-organism.
Suitable micro-organisms include yeasts and suitable lipid-extending substances include aliphatic alcohols, esters, aromatic hydrocarbons and hydrogenated aromatic hydrocarbons. An example of a material that can be encapsulated is a leuco dye suitable for use in "carbonless"
copy paper. A stated advantage of the method described in that European patent is that, in contrast to certain earlier proposals (cf. US-A-4,001,480 and FR-A-2,179,528), use may be made of micro-organisms having a natural lipid content of less than 40 percent by weight, without the need to employ a plasmolyser.
212~79~
EP-A-0,242,135 (AD2 Limited) discloses a method of producing an encapsulated material by contacting the material in liquid form with a grown intact micro-organism having a microbial lipid content of less than 40 percent by weight. The encapsulatable material must be capable of diffusing into the microbial cell without causing total lysation thereof and the treatment of the micro-organism is carried out in the absence of an organic lipid-extending substance as solvent or microdispersant for the encapsulatable material and in the absence of a plasmolyser.
The material is absorbed by the micro-organism - typically a yeast - by diffusion across the microbial cell wall and is passively retained within the micro-organism. A wide variety of encapsulatable materials are mentioned, including essential oils used as flavours or fragrances, leuco dyes, vitamins, detergents such as lauryl ether sulfate, food colourants, and pesticides and the like.
EP-A-0,414,282 (Quest International) discloses bleach compositions, including laundry detergents, laundry bleaches and dishwashing or scouring products, that contain a perfume whereas EP-A-0,414,283 (Quest International) discloses fabric-softening compositions that contain a perfume. In both cases, the perfume is encapsulated in micro-organism cells according to the conventional methods, as described in US-A-4,00l,480 or EP-A-0,242,135.
A problem that arises when using micro-organism cells for encapsulation purposes is that they may have a disagreeable odour and possibly also an unpleasing colour and may therefore diminish the acceptability of the encapsulated products, or compositions containing them, to consumers.
SummarY of the Invention It has now been found that micro-organism cells may be at least partially deodorised by treatment with a peroxygen bleach whilst leaving the cells at least largely intact and hence suitable for encapsulation purposes.
The present invention, in one of its aspects, accordingly provides a method of reducing the odour of micro-organism 212~791 ~3/11869 cells, characterised in that the said cells are treated with a peroxygen bleach.
The invention also provides, in another of its aspects, a process for encapsulating a material in which micro-organism cells are contacted with the said material, which material is in liquid form, whereby the said material is absorbed through the micro-organism cell wall and retained within the micro-organism cells, characterised in that the micro-organism cells are also treated with a peroxygen bleach.
Descri~tion of ExemPlarY Embodiments Although bacteria and algae may be suitable, preferred micro-organisms are fungi, especially filamentous fungi, e.g. Asperglllus niger, and more especially the yeasts.
Examples of yeasts which may be used in the present invention are Lipomyces species, such as L. lipofer and L.
starkeyi, Trichosporon species, such as T. pullulans and T.
cutaneum, Candida species such as C. curvata and C. utilis, Kluvveromyces fragilis and Saccharomyces cerevisiae.
Usually, use will be made of micro-organism cells in grown form, i.e. that have been harvested from a culture medium.
The cells should be intact, that is to say not have undergone any significant lysation, and are preferably of large size, typically with an average diameter for the cell of from 5 to 20 ~m. It is also desirable that the cells should not undergo lysation before or during the encapsulation step.
A micro-organism will normally be chosen that under the conditions of the intended use will disintegrate or undergo sufficient disruption or permit diffusion of its contents so that the encapsulated liquid will be released at the appropriate point of application.
In accordance with this invention, the micro-organism cells are treated with a peroxygen bleach, for example peracids (including so-called 'low-activity' peracids), such as peroxymonosulfuric acid, m-chloroperbenzoic acid, diperisophthalic acid and monoperphthalic acid, and their derivatives, e.g. salts such as potassium monopersulfate 21247~1 4 -("oxone") or magnesium monoperoxyphthalate ("H48").
Compounds that release hydrogen peroxide when dissolved in water come into consideration, especially those that are commercially available; these includes such salts as perborates, notably sodium perborate, and such adducts as percarbonates. At present, however, the preferred peroxygen bleach is hydrogen peroxide (H202).
Although the applicant does not wish to be bound by any theory, it is believed that the peroxygen bleach attacks the amine centres in the micro-organism. Generally, the treatment with the peroxygen bleach should be carried out under conditions that achieve a significant reduction in, or even complete removal of, the characteristic micro-organism odour and/or colour without being so severe as to cause any significant lysation or disruption of the cell walls (which would impair the effectiveness of the micro-organism as an encapsulation material). Generally, the micro-organism is treated with an aqueous solution of the peroxygen bleach, especially one containing the peroxygen bleach at a concentration of from O.Ol to 10%, more preferably from 0.02 to 5% and most preferably from O.l to 2%, w/v. Relative to the weight of micro-organism, the amount of peroxygen bleach is usually 0.02 to 100%, preferably 0.04 to 50% and more preferably O.l to 20% by weight. The solution of peroxygen bleach is preferably prepared in deionised water.
The peroxygen bleach-containing treatment solution is preferably alkaline and will typically contain an alkali -usually an alkali metal or alkaline earth metal hydroxide or carbonate, preferably sodium hydroxide - at a concentration from 0 to 2.0 M, preferably from O.Ol to l.0 M, more preferably from 0.05 to 0.5 M. Simply buffering the solution at high pH may also be considered.
It has also proved advantageous for the peroxygen bleach-containing solution to contain sodium silicate, preferably in an amount from 20 to 60g/l, typically from 30 to 50g/l.
The sodium silicate is useful as a filtering aid, is a source of alkalinity, acts as a defoaming agent and provides some control over heavy metals that might decompose the peroxygen bleach. Of course, other silicates, e.g. other alkali metal silicates, come into consideration for use with or instead of the sodium silicate, as do filtration aids, such as Kieselguhr or Celite~, and chelating agents, such as phosphonates, ethylenediamine tetraacetic acid (EDTA) and sodium tripolyphosphate (STP).
Normally, up to 250 g, typically 50 to 150 g, of micro-organism is employed per liter of the peroxygen bleach-containing solution. The treatment is conveniently effected by suspending the micro-organism in the treating solution and gently stirring the suspension. Suitable durations for the treatment and suitable temperatures at which it may be carried out can be determined by simple trials; in general, it has been found adequate for the suspension to be stirred for from 5 minutes to 4 hours, preferably from 30 minutes to 2 hours and typically for about 1 hour, at a temperature of from 0~ to 100~C., preferably from 10~ to 50~C. and typically at room temperature. The treated micro-organism is then separated from the treating solution by any convenient method, e.g.
centrifugation, and is generally dried, e.g. by freeze drying, before further use.
Although the primary purpose in treating the micro-organism cells with the peroxygen bleach is to reduce or eliminate any odour of the micro-organism, the treated micro-organism may also be referred to hereinafter as a "bleached" micro-organism; it has been found that the reduction in odour is often accompanied by a lightening of the colour of the micro-organism cell material.
The treated micro-organism may be employed for the encapsulation of a wide variety of encapsulatable materials using any of the methods known in principle from the prior art, e.g. the method described in U.S. Pat. No. 4,001,480, in EP-B-0,085,805 or, preferably, in EP-A-0,242,135.
The material to be encapsulated should be in liquid form under the conditions at which encapsulation is carried out. Materials that are not themselves liquid under those conditions may be used in the form of a solution or micro WO93/11869 PCT/US92/1039' 21217~1 dispersion in a suitable solvent or dispersant, usually a solvent that is immiscible with lipid that may be present in the micro-organism. Suitable solvents include cl - C4 alcohols, e.g. methanol, ethanol or isopropanol, and the solvent may be removed by evaporation after the encapsulation treatment. It is also possible, and sometimes preferred, to carry out the encapsulation process in the presence of water.
Although it is preferred to treat the micro-organisms with the peroxygen bleach before encapsulation is effected, it is possible in principle to effect such treatment during or even after the encapsulation step. Thus, for example, encapsulation could be effected from a system containing both the peroxygen bleach in aqueous solution and the material to be encapsulated, provided that the material to be encapsulated were compatible with that bleach.
The present invention is particularly advantageous in the encapsulation of bleach activators used in cleaning compositions, for example heavy duty or general purpose laundry detergent compositions, bleaching compositions, dishwashing compositions and hard-surface or other cleaning products.
Such bleach activators are commonly susceptible to attack by moisture, leading to hydrolysis or premature perhydrolysis, the products of which are liable to damage other ingredients in the cleaning composition. Suitable bleach activators are disclosed in U.S. Patents No.
4,179,390 (Spadini et al.), No. 4,412,934 (Chung et al.) and No. 4,915,854 (Mao et al.) The present invention is illustrated in and by the following examples.
ExamPle l (a) Yeast Treatment lOOg of baker's yeast (Saccharomyces cerevisiae) were suspended in one litre of a 0.2 molar solution of sodium hydroxide in water containing 40g of sodium silicate.
Hydrogen peroxide was added until its concentration reached l~ w/v and the resultant suspension was then gently stirred 2 1 2 '~7 Q~ ~
V g3/11869 PCT/US92/10391 for one hour at room temperature. The yeast was then removed by centrifugation and freeze dried.
(b) EncaPsulation One part by weight of the bleached yeast obtained according to the above-described treatment (a) was suspended in three parts of water and stirred at 60~C for one hour. 0.6 parts of the material to be encapsulated, namely acetyl triethyl citrate, was then added and the suspension was stirred for 6 hours at 45~C. The yeast cells were then removed by centrifugation and freeze dried. The resultant yeast-encapsulated acetyl triethyl citrate was suitable for incorporation into detergent formulations as a bleach activator.
ExamPle 2 A number of samples of bleached yeast micro-capsules were prepared using the process described above in Example 1 (a) but with certain variations in the yeast concentration, alkalinity, the presence or absence of sodium silicate, and the concentration of hydrogen peroxide. The samples were assessed for yeast odour and for the amount of foaming produced during the hydrogen peroxide treatment. The results are summarised in the following table (in which sample 5 indicates the sample obtained by the process according to Example l(a)).
Table l Sample Yeast Alkalinity Sodium H202 Yeast Foaming Conc. Silicate Odour (g/l) (M) (+/-) (%) (1-5) (1-5) 3 100 2 + 10 4 100 1 +
100 0.2 + 1 1 2 6 100 0.05 + 1 3 5 Kev Odour WO93/11869 PCT/US92/1039' 2~2 179~ 8 1 = Best, i.e. little or no odour 5 = Worst, i.e. odour approximately equal to starting material.
Foaming 1 = Best, i.e. little foaming 5 = Worst, i.e. excessive foaming For the yeast cells to be useful for encapsulation purposes, the cell membrane must be intact. Microscopy showed that this was only the case for Samples 5 and 6.
Sample 5 was preferred to Sample ~, in that it exhi~ited a lower odour and lower foaming.
ExamPle 3 Bleached yeast micro-capsules containing the liquid bleach activator, acetyl triethyl citrate, which micro capsules had been prepared according to the process of Example 1 (b), were blended into a standard detergent composition and stored in sealed cartons under stressed storage conditions (32~C and 80% humidity). For comparison purposes, a similar composition was prepared containing the liquid bleach activator encapsulated in unbleached yeast micro-capsules prepared according to the prior art (EP-A-0,242,135). A
further comparison composition was prepared containing, - instead of the encapsulated liquid bleach activator, a conventional activator, tetraacetyl ethylene diamine (TAED), in particulate form. The comparison compositions were stored in sealed cartons under the stressed storage conditions specified above.
The compositions were sampled after certain periods of time, the samples being analyzed in order to determine how much of the bleach activator (acetyl triethyl citrate or TAED, as the case may be) remained (expressed as a percentage of the original content). Specifically, the analysis was effected by dissolving the sample, analyzing for peracid and comparing that result with the expected result for 100~ active. The results are shown in the following table.
2 1 2 ~ 7 ~ ~
~' ~3/11869 PCT/US92/10391 Table 2 Time Unbleached Bleached TAED
Weeks % remaining % remaininq % remaininq 67 (29) 67 The 5-week result for the bleached capsules is anomalous and is thought to be due to poor dispersion of the product; in particular, caking, which is a problem commonly experienced when using such stressed storage conditions, tends to render dissolution of the product difficult. Overall, the performance of the bleached capsules in preserving the activity of the bleach activator was deemed comparable to the effectiveness of the conventional, unbleached capsules.
It will of course be understood that the present invention has been described above purely by way of example and that modifications of detail can be made within the scope of the lnventlon .
Field of the Invention The present invention relates to a method of reducing the odour of micro-organism cells. The invention also relates to the use of the resultant deodorised cells in a process for encapsulating a material, in which micro-organism cells are contacted with the said material, which material is in liquid form, whereby the said material is absorbed through the micro-organism cell wall and retained within the micro-organism cells. The invention also relates to liquids that have been encapsulated in that manner.
Backqround to the Invention The encapsulation of materials within micro-organism cells is well known. In EP-B-0,085,805 (Dunlop Limited), a method of encapsulation is described in which the micro-organism is contacted with an organic lipid-extending substance that is a solvent, or a micro-dispersing medium, for the material to be encapsulated, and simultaneously and/or subsequently the micro-organism is contacted with the material to be encapsulated, said material being employed as a solution or micro-dispersion in the organic lipid-extending substance, or in a further organic lipid-extending substance or in a liquid that is miscible with the first-mentioned lipid-extending substance, whereby both the organic lipid-extending substance and the material to be encapsulated are taken into and retained passively within the micro-organism.
Suitable micro-organisms include yeasts and suitable lipid-extending substances include aliphatic alcohols, esters, aromatic hydrocarbons and hydrogenated aromatic hydrocarbons. An example of a material that can be encapsulated is a leuco dye suitable for use in "carbonless"
copy paper. A stated advantage of the method described in that European patent is that, in contrast to certain earlier proposals (cf. US-A-4,001,480 and FR-A-2,179,528), use may be made of micro-organisms having a natural lipid content of less than 40 percent by weight, without the need to employ a plasmolyser.
212~79~
EP-A-0,242,135 (AD2 Limited) discloses a method of producing an encapsulated material by contacting the material in liquid form with a grown intact micro-organism having a microbial lipid content of less than 40 percent by weight. The encapsulatable material must be capable of diffusing into the microbial cell without causing total lysation thereof and the treatment of the micro-organism is carried out in the absence of an organic lipid-extending substance as solvent or microdispersant for the encapsulatable material and in the absence of a plasmolyser.
The material is absorbed by the micro-organism - typically a yeast - by diffusion across the microbial cell wall and is passively retained within the micro-organism. A wide variety of encapsulatable materials are mentioned, including essential oils used as flavours or fragrances, leuco dyes, vitamins, detergents such as lauryl ether sulfate, food colourants, and pesticides and the like.
EP-A-0,414,282 (Quest International) discloses bleach compositions, including laundry detergents, laundry bleaches and dishwashing or scouring products, that contain a perfume whereas EP-A-0,414,283 (Quest International) discloses fabric-softening compositions that contain a perfume. In both cases, the perfume is encapsulated in micro-organism cells according to the conventional methods, as described in US-A-4,00l,480 or EP-A-0,242,135.
A problem that arises when using micro-organism cells for encapsulation purposes is that they may have a disagreeable odour and possibly also an unpleasing colour and may therefore diminish the acceptability of the encapsulated products, or compositions containing them, to consumers.
SummarY of the Invention It has now been found that micro-organism cells may be at least partially deodorised by treatment with a peroxygen bleach whilst leaving the cells at least largely intact and hence suitable for encapsulation purposes.
The present invention, in one of its aspects, accordingly provides a method of reducing the odour of micro-organism 212~791 ~3/11869 cells, characterised in that the said cells are treated with a peroxygen bleach.
The invention also provides, in another of its aspects, a process for encapsulating a material in which micro-organism cells are contacted with the said material, which material is in liquid form, whereby the said material is absorbed through the micro-organism cell wall and retained within the micro-organism cells, characterised in that the micro-organism cells are also treated with a peroxygen bleach.
Descri~tion of ExemPlarY Embodiments Although bacteria and algae may be suitable, preferred micro-organisms are fungi, especially filamentous fungi, e.g. Asperglllus niger, and more especially the yeasts.
Examples of yeasts which may be used in the present invention are Lipomyces species, such as L. lipofer and L.
starkeyi, Trichosporon species, such as T. pullulans and T.
cutaneum, Candida species such as C. curvata and C. utilis, Kluvveromyces fragilis and Saccharomyces cerevisiae.
Usually, use will be made of micro-organism cells in grown form, i.e. that have been harvested from a culture medium.
The cells should be intact, that is to say not have undergone any significant lysation, and are preferably of large size, typically with an average diameter for the cell of from 5 to 20 ~m. It is also desirable that the cells should not undergo lysation before or during the encapsulation step.
A micro-organism will normally be chosen that under the conditions of the intended use will disintegrate or undergo sufficient disruption or permit diffusion of its contents so that the encapsulated liquid will be released at the appropriate point of application.
In accordance with this invention, the micro-organism cells are treated with a peroxygen bleach, for example peracids (including so-called 'low-activity' peracids), such as peroxymonosulfuric acid, m-chloroperbenzoic acid, diperisophthalic acid and monoperphthalic acid, and their derivatives, e.g. salts such as potassium monopersulfate 21247~1 4 -("oxone") or magnesium monoperoxyphthalate ("H48").
Compounds that release hydrogen peroxide when dissolved in water come into consideration, especially those that are commercially available; these includes such salts as perborates, notably sodium perborate, and such adducts as percarbonates. At present, however, the preferred peroxygen bleach is hydrogen peroxide (H202).
Although the applicant does not wish to be bound by any theory, it is believed that the peroxygen bleach attacks the amine centres in the micro-organism. Generally, the treatment with the peroxygen bleach should be carried out under conditions that achieve a significant reduction in, or even complete removal of, the characteristic micro-organism odour and/or colour without being so severe as to cause any significant lysation or disruption of the cell walls (which would impair the effectiveness of the micro-organism as an encapsulation material). Generally, the micro-organism is treated with an aqueous solution of the peroxygen bleach, especially one containing the peroxygen bleach at a concentration of from O.Ol to 10%, more preferably from 0.02 to 5% and most preferably from O.l to 2%, w/v. Relative to the weight of micro-organism, the amount of peroxygen bleach is usually 0.02 to 100%, preferably 0.04 to 50% and more preferably O.l to 20% by weight. The solution of peroxygen bleach is preferably prepared in deionised water.
The peroxygen bleach-containing treatment solution is preferably alkaline and will typically contain an alkali -usually an alkali metal or alkaline earth metal hydroxide or carbonate, preferably sodium hydroxide - at a concentration from 0 to 2.0 M, preferably from O.Ol to l.0 M, more preferably from 0.05 to 0.5 M. Simply buffering the solution at high pH may also be considered.
It has also proved advantageous for the peroxygen bleach-containing solution to contain sodium silicate, preferably in an amount from 20 to 60g/l, typically from 30 to 50g/l.
The sodium silicate is useful as a filtering aid, is a source of alkalinity, acts as a defoaming agent and provides some control over heavy metals that might decompose the peroxygen bleach. Of course, other silicates, e.g. other alkali metal silicates, come into consideration for use with or instead of the sodium silicate, as do filtration aids, such as Kieselguhr or Celite~, and chelating agents, such as phosphonates, ethylenediamine tetraacetic acid (EDTA) and sodium tripolyphosphate (STP).
Normally, up to 250 g, typically 50 to 150 g, of micro-organism is employed per liter of the peroxygen bleach-containing solution. The treatment is conveniently effected by suspending the micro-organism in the treating solution and gently stirring the suspension. Suitable durations for the treatment and suitable temperatures at which it may be carried out can be determined by simple trials; in general, it has been found adequate for the suspension to be stirred for from 5 minutes to 4 hours, preferably from 30 minutes to 2 hours and typically for about 1 hour, at a temperature of from 0~ to 100~C., preferably from 10~ to 50~C. and typically at room temperature. The treated micro-organism is then separated from the treating solution by any convenient method, e.g.
centrifugation, and is generally dried, e.g. by freeze drying, before further use.
Although the primary purpose in treating the micro-organism cells with the peroxygen bleach is to reduce or eliminate any odour of the micro-organism, the treated micro-organism may also be referred to hereinafter as a "bleached" micro-organism; it has been found that the reduction in odour is often accompanied by a lightening of the colour of the micro-organism cell material.
The treated micro-organism may be employed for the encapsulation of a wide variety of encapsulatable materials using any of the methods known in principle from the prior art, e.g. the method described in U.S. Pat. No. 4,001,480, in EP-B-0,085,805 or, preferably, in EP-A-0,242,135.
The material to be encapsulated should be in liquid form under the conditions at which encapsulation is carried out. Materials that are not themselves liquid under those conditions may be used in the form of a solution or micro WO93/11869 PCT/US92/1039' 21217~1 dispersion in a suitable solvent or dispersant, usually a solvent that is immiscible with lipid that may be present in the micro-organism. Suitable solvents include cl - C4 alcohols, e.g. methanol, ethanol or isopropanol, and the solvent may be removed by evaporation after the encapsulation treatment. It is also possible, and sometimes preferred, to carry out the encapsulation process in the presence of water.
Although it is preferred to treat the micro-organisms with the peroxygen bleach before encapsulation is effected, it is possible in principle to effect such treatment during or even after the encapsulation step. Thus, for example, encapsulation could be effected from a system containing both the peroxygen bleach in aqueous solution and the material to be encapsulated, provided that the material to be encapsulated were compatible with that bleach.
The present invention is particularly advantageous in the encapsulation of bleach activators used in cleaning compositions, for example heavy duty or general purpose laundry detergent compositions, bleaching compositions, dishwashing compositions and hard-surface or other cleaning products.
Such bleach activators are commonly susceptible to attack by moisture, leading to hydrolysis or premature perhydrolysis, the products of which are liable to damage other ingredients in the cleaning composition. Suitable bleach activators are disclosed in U.S. Patents No.
4,179,390 (Spadini et al.), No. 4,412,934 (Chung et al.) and No. 4,915,854 (Mao et al.) The present invention is illustrated in and by the following examples.
ExamPle l (a) Yeast Treatment lOOg of baker's yeast (Saccharomyces cerevisiae) were suspended in one litre of a 0.2 molar solution of sodium hydroxide in water containing 40g of sodium silicate.
Hydrogen peroxide was added until its concentration reached l~ w/v and the resultant suspension was then gently stirred 2 1 2 '~7 Q~ ~
V g3/11869 PCT/US92/10391 for one hour at room temperature. The yeast was then removed by centrifugation and freeze dried.
(b) EncaPsulation One part by weight of the bleached yeast obtained according to the above-described treatment (a) was suspended in three parts of water and stirred at 60~C for one hour. 0.6 parts of the material to be encapsulated, namely acetyl triethyl citrate, was then added and the suspension was stirred for 6 hours at 45~C. The yeast cells were then removed by centrifugation and freeze dried. The resultant yeast-encapsulated acetyl triethyl citrate was suitable for incorporation into detergent formulations as a bleach activator.
ExamPle 2 A number of samples of bleached yeast micro-capsules were prepared using the process described above in Example 1 (a) but with certain variations in the yeast concentration, alkalinity, the presence or absence of sodium silicate, and the concentration of hydrogen peroxide. The samples were assessed for yeast odour and for the amount of foaming produced during the hydrogen peroxide treatment. The results are summarised in the following table (in which sample 5 indicates the sample obtained by the process according to Example l(a)).
Table l Sample Yeast Alkalinity Sodium H202 Yeast Foaming Conc. Silicate Odour (g/l) (M) (+/-) (%) (1-5) (1-5) 3 100 2 + 10 4 100 1 +
100 0.2 + 1 1 2 6 100 0.05 + 1 3 5 Kev Odour WO93/11869 PCT/US92/1039' 2~2 179~ 8 1 = Best, i.e. little or no odour 5 = Worst, i.e. odour approximately equal to starting material.
Foaming 1 = Best, i.e. little foaming 5 = Worst, i.e. excessive foaming For the yeast cells to be useful for encapsulation purposes, the cell membrane must be intact. Microscopy showed that this was only the case for Samples 5 and 6.
Sample 5 was preferred to Sample ~, in that it exhi~ited a lower odour and lower foaming.
ExamPle 3 Bleached yeast micro-capsules containing the liquid bleach activator, acetyl triethyl citrate, which micro capsules had been prepared according to the process of Example 1 (b), were blended into a standard detergent composition and stored in sealed cartons under stressed storage conditions (32~C and 80% humidity). For comparison purposes, a similar composition was prepared containing the liquid bleach activator encapsulated in unbleached yeast micro-capsules prepared according to the prior art (EP-A-0,242,135). A
further comparison composition was prepared containing, - instead of the encapsulated liquid bleach activator, a conventional activator, tetraacetyl ethylene diamine (TAED), in particulate form. The comparison compositions were stored in sealed cartons under the stressed storage conditions specified above.
The compositions were sampled after certain periods of time, the samples being analyzed in order to determine how much of the bleach activator (acetyl triethyl citrate or TAED, as the case may be) remained (expressed as a percentage of the original content). Specifically, the analysis was effected by dissolving the sample, analyzing for peracid and comparing that result with the expected result for 100~ active. The results are shown in the following table.
2 1 2 ~ 7 ~ ~
~' ~3/11869 PCT/US92/10391 Table 2 Time Unbleached Bleached TAED
Weeks % remaining % remaininq % remaininq 67 (29) 67 The 5-week result for the bleached capsules is anomalous and is thought to be due to poor dispersion of the product; in particular, caking, which is a problem commonly experienced when using such stressed storage conditions, tends to render dissolution of the product difficult. Overall, the performance of the bleached capsules in preserving the activity of the bleach activator was deemed comparable to the effectiveness of the conventional, unbleached capsules.
It will of course be understood that the present invention has been described above purely by way of example and that modifications of detail can be made within the scope of the lnventlon .
Claims (6)
1. A method for encapsulating a bleach activator in micro-organism cells for use in laundry compositions, said method comprising the steps of:
(a) deodorizing intact microorganism cells with a peroxygen bleach under conditions whereby the odor of the microorganism cells is reduced while maintaining at least a portion of the deodorized cells intact;
(b) contacting the deodorized microorganism cells from step (a) with a liquid selected from liquid bleach activators and liquids containing solvent and bleach activator under conditions whereby at least a portion of the bleach activator is encapsulated in the intact deodorized microorganism cells; and (c) collecting the microorganism cell-encapsulated bleach activator.
(a) deodorizing intact microorganism cells with a peroxygen bleach under conditions whereby the odor of the microorganism cells is reduced while maintaining at least a portion of the deodorized cells intact;
(b) contacting the deodorized microorganism cells from step (a) with a liquid selected from liquid bleach activators and liquids containing solvent and bleach activator under conditions whereby at least a portion of the bleach activator is encapsulated in the intact deodorized microorganism cells; and (c) collecting the microorganism cell-encapsulated bleach activator.
2. The method according to claim 1 wherein the micro-organism cells are deodorized under alkaline conditions.
3. The method according to claim 2 wherein the deodorization step (a) further comprises silicate.
4. The method according to claim 1 wherein the peroxygen bleach is hydrogen peroxide.
5. The method according to claim 1 wherein the microorganism cells are selected from the group consisting of yeast cells and fungi cells.
6. A microorganism cell-encapsulated bleach activator composition prepared according to the method of claim 1.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP91870208 | 1991-12-13 | ||
| EP91870208.5 | 1991-12-13 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2124791C true CA2124791C (en) | 1997-10-21 |
Family
ID=8209040
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA 2124791 Expired - Fee Related CA2124791C (en) | 1991-12-13 | 1992-12-01 | Encapsulation of liquids in microorganisms |
Country Status (8)
| Country | Link |
|---|---|
| EP (1) | EP0672113A1 (en) |
| JP (1) | JP3222136B2 (en) |
| CN (1) | CN1074481A (en) |
| CA (1) | CA2124791C (en) |
| MA (1) | MA22732A1 (en) |
| MX (1) | MX9207184A (en) |
| TR (1) | TR27620A (en) |
| WO (1) | WO1993011869A1 (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5713962A (en) * | 1993-06-09 | 1998-02-03 | The Procter & Gamble Company | Process for the bleaching of fabrics |
| ATE169953T1 (en) * | 1993-06-09 | 1998-09-15 | Procter & Gamble | METHOD FOR BLEACHING TISSUES |
| US5905067A (en) * | 1997-02-10 | 1999-05-18 | Procter & Gamble Company | System for delivering hydrophobic liquid bleach activators |
| GB2396107A (en) * | 2002-10-24 | 2004-06-16 | Micap Plc | Micro-organism microcapsules |
| GB2413563A (en) * | 2004-04-27 | 2005-11-02 | Micap Plc | Composition comprising a biocide encapsulated within a fungal cell |
| GB2418654A (en) * | 2004-09-29 | 2006-04-05 | Micap Plc | Microbial encapsulation |
| BR112015020306A2 (en) | 2013-02-25 | 2017-07-18 | Firmenich & Cie | encapsulated plasmolized microorganism particles |
| EP3478089B1 (en) | 2016-06-30 | 2021-11-03 | Firmenich SA | Plated yeast formulations |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR343712A (en) * | 1904-06-04 | 1904-10-13 | Max Elb | Process for removing bitterness from yeast extracts |
| US1056540A (en) * | 1911-10-27 | 1913-03-18 | Alois Zeckendorf | Process of bleaching and conserving yeast. |
| US2031668A (en) * | 1929-04-04 | 1936-02-25 | Gustave T Reich | Art of purifying yeast |
| AT326611B (en) * | 1972-07-31 | 1975-12-29 | Henkel & Cie Gmbh | BLEACHING AID SUITABLE AS A COMPONENT OF POWDERED DETERGENTS AND BLEACHING AGENTS |
| US3951594A (en) * | 1972-11-27 | 1976-04-20 | Pennwalt Corporation | Hydrogen peroxide bleaching solutions and process |
| US4001480A (en) * | 1974-08-16 | 1977-01-04 | Swift & Company | Encapsulation process utilizing microorganisms and products produced thereby |
| US4025453A (en) * | 1976-02-09 | 1977-05-24 | Shell Oil Company | Activated bleaching process and compositions therefor |
| EP0041650A3 (en) * | 1980-06-10 | 1982-05-12 | Provesta Corporation | A method of reducing the nucleic acid level in single cell protein and method for producing a single cell protein product |
| GB8608964D0 (en) * | 1986-04-12 | 1986-05-14 | Pannell N A | Producing microbially encapsulated materials |
| IL95019A0 (en) * | 1989-08-09 | 1991-06-10 | Mycogen Corp | Process for encapsulation of biologicals |
-
1992
- 1992-11-19 TR TR01115/92A patent/TR27620A/en unknown
- 1992-12-01 CA CA 2124791 patent/CA2124791C/en not_active Expired - Fee Related
- 1992-12-01 JP JP51095993A patent/JP3222136B2/en not_active Expired - Fee Related
- 1992-12-01 EP EP93900776A patent/EP0672113A1/en not_active Withdrawn
- 1992-12-01 WO PCT/US1992/010391 patent/WO1993011869A1/en not_active Application Discontinuation
- 1992-12-09 MA MA23022A patent/MA22732A1/en unknown
- 1992-12-11 MX MX9207184A patent/MX9207184A/en unknown
- 1992-12-12 CN CN 92114897 patent/CN1074481A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| EP0672113A4 (en) | 1994-11-28 |
| CN1074481A (en) | 1993-07-21 |
| EP0672113A1 (en) | 1995-09-20 |
| JP3222136B2 (en) | 2001-10-22 |
| MA22732A1 (en) | 1993-07-01 |
| JPH07501944A (en) | 1995-03-02 |
| TR27620A (en) | 1995-06-13 |
| WO1993011869A1 (en) | 1993-06-24 |
| MX9207184A (en) | 1993-07-30 |
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| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| MKLA | Lapsed |