CA1113774A - Method for sterilizing milk - Google Patents
Method for sterilizing milkInfo
- Publication number
- CA1113774A CA1113774A CA304,627A CA304627A CA1113774A CA 1113774 A CA1113774 A CA 1113774A CA 304627 A CA304627 A CA 304627A CA 1113774 A CA1113774 A CA 1113774A
- Authority
- CA
- Canada
- Prior art keywords
- milk
- hydrogen peroxide
- fibers
- treatment
- catalase
- 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
Links
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/358—Inorganic compounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
- A23C3/00—Preservation of milk or milk preparations
- A23C3/08—Preservation of milk or milk preparations by addition of preservatives
- A23C3/085—Inorganic compounds, e.g. lactoperoxidase - H2O2 systems
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
- A23C9/00—Milk preparations; Milk powder or milk powder preparations
- A23C9/12—Fermented milk preparations; Treatment using microorganisms or enzymes
- A23C9/1203—Addition of, or treatment with, enzymes or microorganisms other than lactobacteriaceae
- A23C9/1213—Oxidation or reduction enzymes, e.g. peroxidase, catalase, dehydrogenase
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Dairy Products (AREA)
- Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
- Immobilizing And Processing Of Enzymes And Microorganisms (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE:
Milk is sterilized by a cold treatment with hydrogen peroxide as sterilizing agent and the residual, hydrogen peroxide is subsequently converted to water and oxygen by having the milk flowing through fibers in which a catalase enzyme is occluded. The catalase-occluding fibers can also loosely be added to the milk. This treatment avoids the administration of heat and ensures that no residual hydrogen peroxide is left in milk. The flavor and taste qualities of milk are wholly unaffected by this treatment.
Milk is sterilized by a cold treatment with hydrogen peroxide as sterilizing agent and the residual, hydrogen peroxide is subsequently converted to water and oxygen by having the milk flowing through fibers in which a catalase enzyme is occluded. The catalase-occluding fibers can also loosely be added to the milk. This treatment avoids the administration of heat and ensures that no residual hydrogen peroxide is left in milk. The flavor and taste qualities of milk are wholly unaffected by this treatment.
Description
The present invention relates to a method for sterilizing milk.
Milk gives rise to serious preservation problems, both when it is to be used as such, and when it is to be converted into other produces, such as cheeses, yogurt and the like.
The preservation problems are essentially related to the pollution by bacteria, which, on account of the chemical composition of milk, find therein an excellent culturing medium in which they multiply at a very fast rate. As a matter of fact, milk is a highly valued produce for human feeding but, just for this reason, it is one of the most perishable foodstuffs. Bearing this circumstance in mind, a number of treatments have been studied and applied in the industry, such as sterilization, pasteurization and uperization, which enable milk to keep for average and long periods of time without substantially modifying its nutritional value.
All of these treatments are mainly heat-treatments - and require expensive installations, which are, of necessity, centralized, and often remote from the production centers.
The problem of milk keeping is, at any rate, still - left outstanding in the time span between milking and the heat treatment, that is, during shlpping and storage preliminary to such treatment.
Refrigeration solves this problem only in part, both because it is not always practicable, and because it merely moderates the bacterial growth-rate. It is apparent that the period of time between milking and the heat-treatment must be as short as practicable.
Conversely, there is a sterilization treatment which is extremely simple and cheap and does not require any special installations, and which can be carried out immediately lC~ --2--.- ~ .
1~3774 upon milking. It would suffice to add to the freshly drawn milk hydrogen peroxide in a concentration of from 500 to
Milk gives rise to serious preservation problems, both when it is to be used as such, and when it is to be converted into other produces, such as cheeses, yogurt and the like.
The preservation problems are essentially related to the pollution by bacteria, which, on account of the chemical composition of milk, find therein an excellent culturing medium in which they multiply at a very fast rate. As a matter of fact, milk is a highly valued produce for human feeding but, just for this reason, it is one of the most perishable foodstuffs. Bearing this circumstance in mind, a number of treatments have been studied and applied in the industry, such as sterilization, pasteurization and uperization, which enable milk to keep for average and long periods of time without substantially modifying its nutritional value.
All of these treatments are mainly heat-treatments - and require expensive installations, which are, of necessity, centralized, and often remote from the production centers.
The problem of milk keeping is, at any rate, still - left outstanding in the time span between milking and the heat treatment, that is, during shlpping and storage preliminary to such treatment.
Refrigeration solves this problem only in part, both because it is not always practicable, and because it merely moderates the bacterial growth-rate. It is apparent that the period of time between milking and the heat-treatment must be as short as practicable.
Conversely, there is a sterilization treatment which is extremely simple and cheap and does not require any special installations, and which can be carried out immediately lC~ --2--.- ~ .
1~3774 upon milking. It would suffice to add to the freshly drawn milk hydrogen peroxide in a concentration of from 500 to
2,000 ppm (parts per million) to have an absolutely sterile produce without any need of further treatments. In addition, the presence of hydrogen peroxide would keep the produce sterile during shipping and storage, the refrigeration problem and the requirement of minimizing the times taken by these operations being thus offset.
Regrettably enough, this so simple and efficient treatment cannot be carried out because hydrogen peroxide, due to its toxicity, must be driven off, but this cannot be done, in its turn, without adding chemicals which would modify both the chemical and organoleptic properties of the milk.
It has now been ascertained that it is possible to carry out a simple treatment which enables hydrogen peroxide to be converted to water and oxygen and therefore to be eliminated without modifying the chemical composition of milk, --by employing a catalase enæyme immobilized in fibers of a polymeric material according to the procedure disclosed in the Italian Patent 836,462, and permitting this enzyme to exercise its catabylic activity on the residual hydrogen peroxide of the milk for a time sufficient to remove any traces of this residual hydrogen per~xide.
As a matter of fact the enzyme catalase, which catalyzes the conversion of hydrogen peroxide into water and oxygen, can simply be removed, on completion of the reaction, by merely separating the fibers, by which the enzyme is immobil-ized, from milk. It is apparent than, by so doing, the overall treatment of sterilization and driving off of hydrogen peroxide involves, as regards the chemical composition of milk, but a slightest increase of the quantity of water. -
Regrettably enough, this so simple and efficient treatment cannot be carried out because hydrogen peroxide, due to its toxicity, must be driven off, but this cannot be done, in its turn, without adding chemicals which would modify both the chemical and organoleptic properties of the milk.
It has now been ascertained that it is possible to carry out a simple treatment which enables hydrogen peroxide to be converted to water and oxygen and therefore to be eliminated without modifying the chemical composition of milk, --by employing a catalase enæyme immobilized in fibers of a polymeric material according to the procedure disclosed in the Italian Patent 836,462, and permitting this enzyme to exercise its catabylic activity on the residual hydrogen peroxide of the milk for a time sufficient to remove any traces of this residual hydrogen per~xide.
As a matter of fact the enzyme catalase, which catalyzes the conversion of hydrogen peroxide into water and oxygen, can simply be removed, on completion of the reaction, by merely separating the fibers, by which the enzyme is immobil-ized, from milk. It is apparent than, by so doing, the overall treatment of sterilization and driving off of hydrogen peroxide involves, as regards the chemical composition of milk, but a slightest increase of the quantity of water. -
3--.,~ ' .
.
, :
~113774 It is also apparent that such a treatment can be applied to any foodstuff whatsoever which is composed by a solution, or also by a suspension.
At any rate, the invention is illustrated in more detail in the ensuing examples. -75 g (grams) of cellulose triacetate have been dissolved in one litre of methylene chloride at room temperature.
To the polymeric solution, which had been cooled to 1C, there have been added 150 g of a solution of catalase at the concen-tration of 12.5 mg (milligrams) of proteins per ml, equivalent to 625~000 IU/ml in a potassium phosphate 0.01 M, pH 7.0 buffer which contained glycerol (30% wt/wt). By stirring, an emulsion has been obtained which is composed by a fine dispersion of the enzymic solution in the solution of the polymer.
The emulsion has then been extruded through a spinneret immersed in a coagulation bath composed by toluene.
The filament thus formed has been collected on a takeup drum and dried in air to drive off the spinning solvents.
To one litre of milk in which, by the bacterial count made according to the APHA standards (" Standard Methods for the Examination of Dairy Products" , 13th Edition, - American Public Health Association, Inc., New York, 1972?, 120.103 colonies per ml had been found, hydrogen peroxide has been added in a concentration of 1,000 ppm. The milk has been held for one hour at 35C in a closed container.
Then, to the milk has been added 1 g of the catalase-occluding fiber and the whole has been kept for one hour at 25C with a bland stirring. The fiber has been removed and the bacterial count on the treated milk was nil.
The determination of hydrogen peroxide has been :
~13774 made with the polarograph AMEL* Mod. 463 with mercury drop electrode after having added to 10 mls of milk and equal volume of phosphate buffer 0.05 M, pH 7.0 as the supporting electrolyte and after having reduced the oxygen level by flushing with nitrogen for 5 mins.
The concentration of hydrogen peroxide in the treated milk, calculated with the aid of a calibration curve obtained with milk samples of known H2O2 concentrations, was nil.
20 g of the fiber described in Example 1 have been introduced in a tubular reaction vessel (dia. 12 mm, height 1,000 mm), the temperature of which was thermostatically kept 25C. The fibres were arranged so as to have their axis parallel to the axis of the reactor. The reactor has con-tinuously been fed with 10 litres an * trade mark - /
.~ .
- 4a -i ~,;
~;~
. ' . ' '' ~' ' ' ' -- 1~13774 hour of milk which has been stored at 35C for 12 hrs with 800 ppm of hydrogen peroxide in a sealed container. Prior to the addition of hydrogen peroxide, there had been found, as in Example 1, 150.10 3 bacteria per ml.
After that the milk had flown through the column, no hydrogen peroxide has been found and the bacterial concentration was 7 bacteria per ml.
To a cheese whey having a pH of 6.8 and a bacterial concen-tration of 108.103 bacteria per ml hydrogen peroxide has been ad-ded up to a concentration of 500 ppm. After 12 hours of storage at 35C in closed container the solution has been caused to flow through the reactor described in Example 2 at the rate of flow of 10 litres an hour and no hydrogen peroxide has been found in the eluate. The bacteria in the eluate were 6 per ml.
To one litre of milk hydrogen peroxide has been added at the concentration of 4,500 ppm. To the milk, thermostatically kept at 25C, there have been added 250 mg of a fiber containing catalase occluded therein and prepared according to the procedure detailed in Example 1. After 60 mins the fiber has been withdrawn from the milk and 2,000 ppm of hydrogen peroxide have been found in the milk. After 2 additional hours, during which the milk has still been kept at 25C but out of contact with the fibers, 2,000 ppm of hydrogen peroxide have been found again. Then the fibers have been introduced in the milk mass again and, after 1 hour of reaction, the level of hydrogen peroxide had dropped to 950 ppm. The fiber has been removed from milk once more and, after 2 further hours, 950 ppm of hydrogen peroxide had still be found. These facts are 3 an evidence that the separation of the fibers from milk ensures also the complete removal of the catalase enzyme.
.
, :
~113774 It is also apparent that such a treatment can be applied to any foodstuff whatsoever which is composed by a solution, or also by a suspension.
At any rate, the invention is illustrated in more detail in the ensuing examples. -75 g (grams) of cellulose triacetate have been dissolved in one litre of methylene chloride at room temperature.
To the polymeric solution, which had been cooled to 1C, there have been added 150 g of a solution of catalase at the concen-tration of 12.5 mg (milligrams) of proteins per ml, equivalent to 625~000 IU/ml in a potassium phosphate 0.01 M, pH 7.0 buffer which contained glycerol (30% wt/wt). By stirring, an emulsion has been obtained which is composed by a fine dispersion of the enzymic solution in the solution of the polymer.
The emulsion has then been extruded through a spinneret immersed in a coagulation bath composed by toluene.
The filament thus formed has been collected on a takeup drum and dried in air to drive off the spinning solvents.
To one litre of milk in which, by the bacterial count made according to the APHA standards (" Standard Methods for the Examination of Dairy Products" , 13th Edition, - American Public Health Association, Inc., New York, 1972?, 120.103 colonies per ml had been found, hydrogen peroxide has been added in a concentration of 1,000 ppm. The milk has been held for one hour at 35C in a closed container.
Then, to the milk has been added 1 g of the catalase-occluding fiber and the whole has been kept for one hour at 25C with a bland stirring. The fiber has been removed and the bacterial count on the treated milk was nil.
The determination of hydrogen peroxide has been :
~13774 made with the polarograph AMEL* Mod. 463 with mercury drop electrode after having added to 10 mls of milk and equal volume of phosphate buffer 0.05 M, pH 7.0 as the supporting electrolyte and after having reduced the oxygen level by flushing with nitrogen for 5 mins.
The concentration of hydrogen peroxide in the treated milk, calculated with the aid of a calibration curve obtained with milk samples of known H2O2 concentrations, was nil.
20 g of the fiber described in Example 1 have been introduced in a tubular reaction vessel (dia. 12 mm, height 1,000 mm), the temperature of which was thermostatically kept 25C. The fibres were arranged so as to have their axis parallel to the axis of the reactor. The reactor has con-tinuously been fed with 10 litres an * trade mark - /
.~ .
- 4a -i ~,;
~;~
. ' . ' '' ~' ' ' ' -- 1~13774 hour of milk which has been stored at 35C for 12 hrs with 800 ppm of hydrogen peroxide in a sealed container. Prior to the addition of hydrogen peroxide, there had been found, as in Example 1, 150.10 3 bacteria per ml.
After that the milk had flown through the column, no hydrogen peroxide has been found and the bacterial concentration was 7 bacteria per ml.
To a cheese whey having a pH of 6.8 and a bacterial concen-tration of 108.103 bacteria per ml hydrogen peroxide has been ad-ded up to a concentration of 500 ppm. After 12 hours of storage at 35C in closed container the solution has been caused to flow through the reactor described in Example 2 at the rate of flow of 10 litres an hour and no hydrogen peroxide has been found in the eluate. The bacteria in the eluate were 6 per ml.
To one litre of milk hydrogen peroxide has been added at the concentration of 4,500 ppm. To the milk, thermostatically kept at 25C, there have been added 250 mg of a fiber containing catalase occluded therein and prepared according to the procedure detailed in Example 1. After 60 mins the fiber has been withdrawn from the milk and 2,000 ppm of hydrogen peroxide have been found in the milk. After 2 additional hours, during which the milk has still been kept at 25C but out of contact with the fibers, 2,000 ppm of hydrogen peroxide have been found again. Then the fibers have been introduced in the milk mass again and, after 1 hour of reaction, the level of hydrogen peroxide had dropped to 950 ppm. The fiber has been removed from milk once more and, after 2 further hours, 950 ppm of hydrogen peroxide had still be found. These facts are 3 an evidence that the separation of the fibers from milk ensures also the complete removal of the catalase enzyme.
Claims (3)
1. A method for sterilizing milk in the liquid or aqueous suspension condition, comprising the steps of treating the liquid or suspension with hydrogen peroxide and subsequently converting the hydrogen peroxide to water and oxygen by employing a catalase enzyme immobilized in fibers of a polymeric material and permitting said catalase enzyme to exercise its catalytic activity on the residual hydrogen peroxide of said solution or emulsion for a time sufficient to remove any traces of said residual hydrogen peroxide.
2. A method according to claim 1, wherein the fibers in which the catalase enzyme is occluded is placed in the hydrogen-peroxide-containing solution or emulsion and removed therefrom upon completion of the reaction.
3. A method according to claim 1, wherein the fiber in which the catalase enzyme is occluded is placed in a reactor in which the solution or emulsion is caused to flow after that it has previously been treated with hydrogen peroxide.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IT25625/77A IT1077319B (en) | 1977-07-12 | 1977-07-12 | PROCESS FOR THE STERILIZATION OF MILK AND FOOD PRODUCTS |
| IT25625A/77 | 1977-07-12 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1113774A true CA1113774A (en) | 1981-12-08 |
Family
ID=11217289
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA304,627A Expired CA1113774A (en) | 1977-07-12 | 1978-06-01 | Method for sterilizing milk |
Country Status (19)
| Country | Link |
|---|---|
| JP (1) | JPS5420150A (en) |
| AU (1) | AU522014B2 (en) |
| BE (1) | BE868948A (en) |
| CA (1) | CA1113774A (en) |
| CH (1) | CH627055A5 (en) |
| CS (1) | CS235070B2 (en) |
| DD (1) | DD137661A5 (en) |
| DE (1) | DE2830680A1 (en) |
| FR (1) | FR2397155A1 (en) |
| GB (1) | GB1560209A (en) |
| HU (1) | HU175831B (en) |
| IL (1) | IL54905A (en) |
| IT (1) | IT1077319B (en) |
| LU (1) | LU79942A1 (en) |
| NL (1) | NL7807517A (en) |
| NO (1) | NO782419L (en) |
| SE (1) | SE7807745L (en) |
| SU (1) | SU1122205A3 (en) |
| ZA (1) | ZA783252B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE502211C2 (en) * | 1990-05-10 | 1995-09-18 | Eka Nobel Ab | Methods to counteract microbial growth of thermophilic bacteria and composition thereof |
| DE102004007616B4 (en) * | 2004-02-17 | 2005-12-22 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Process for producing fibers and other shaped articles from cellulose carbamate and / or regenerated cellulose |
| JPWO2023008491A1 (en) * | 2021-07-27 | 2023-02-02 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3282702A (en) * | 1963-07-16 | 1966-11-01 | Union Carbide Corp | Process for removing hydrogen peroxide from liquids |
| IL32406A (en) * | 1968-06-26 | 1973-01-30 | Snam Progetti | Enzyme preparations comprising a solution or dispersion of enzyme occluded in filaments of cellulose esters or synthetic polymers |
| IT1034020B (en) * | 1970-10-17 | 1979-09-10 | Snam Progetti | PROCEDURE FOR THE ENTI-MATIC BREAKDOWN OF LACTOSE IN MILK AND ITS DERIVATIVES AND PRODUCTS OBTAINED |
-
1977
- 1977-07-12 IT IT25625/77A patent/IT1077319B/en active
-
1978
- 1978-05-31 GB GB25019/78A patent/GB1560209A/en not_active Expired
- 1978-06-01 AU AU36785/78A patent/AU522014B2/en not_active Expired
- 1978-06-01 CA CA304,627A patent/CA1113774A/en not_active Expired
- 1978-06-07 ZA ZA00783252A patent/ZA783252B/en unknown
- 1978-06-13 CH CH644678A patent/CH627055A5/en not_active IP Right Cessation
- 1978-06-14 IL IL54905A patent/IL54905A/en unknown
- 1978-07-03 JP JP7983878A patent/JPS5420150A/en active Pending
- 1978-07-07 LU LU79942A patent/LU79942A1/xx unknown
- 1978-07-07 FR FR7820374A patent/FR2397155A1/en active Granted
- 1978-07-10 DD DD78206630A patent/DD137661A5/en unknown
- 1978-07-11 CS CS784644A patent/CS235070B2/en unknown
- 1978-07-11 HU HU78SA3123A patent/HU175831B/en unknown
- 1978-07-11 SE SE7807745A patent/SE7807745L/en unknown
- 1978-07-11 NO NO782419A patent/NO782419L/en unknown
- 1978-07-12 DE DE19782830680 patent/DE2830680A1/en not_active Ceased
- 1978-07-12 SU SU782635401A patent/SU1122205A3/en active
- 1978-07-12 NL NL7807517A patent/NL7807517A/en not_active Application Discontinuation
- 1978-07-12 BE BE189242A patent/BE868948A/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| GB1560209A (en) | 1980-01-30 |
| NL7807517A (en) | 1979-01-16 |
| NO782419L (en) | 1979-01-15 |
| IL54905A (en) | 1983-05-15 |
| AU3678578A (en) | 1979-12-06 |
| FR2397155B1 (en) | 1981-09-11 |
| IT1077319B (en) | 1985-05-04 |
| AU522014B2 (en) | 1982-05-13 |
| BE868948A (en) | 1979-01-12 |
| JPS5420150A (en) | 1979-02-15 |
| LU79942A1 (en) | 1978-12-12 |
| DD137661A5 (en) | 1979-09-19 |
| ZA783252B (en) | 1979-06-27 |
| SE7807745L (en) | 1979-01-13 |
| HU175831B (en) | 1980-10-28 |
| CH627055A5 (en) | 1981-12-31 |
| CS235070B2 (en) | 1985-04-16 |
| FR2397155A1 (en) | 1979-02-09 |
| SU1122205A3 (en) | 1984-10-30 |
| DE2830680A1 (en) | 1979-01-18 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MKEX | Expiry |