EP3433349A1 - Enzymatic detergent compositions for the automatic cleaning of surgical and/or medical instruments and/or devices - Google Patents
Enzymatic detergent compositions for the automatic cleaning of surgical and/or medical instruments and/or devicesInfo
- Publication number
- EP3433349A1 EP3433349A1 EP17716972.9A EP17716972A EP3433349A1 EP 3433349 A1 EP3433349 A1 EP 3433349A1 EP 17716972 A EP17716972 A EP 17716972A EP 3433349 A1 EP3433349 A1 EP 3433349A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- detergent composition
- composition
- total weight
- weight relative
- content
- 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.)
- Granted
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 112
- 239000003599 detergent Substances 0.000 title claims abstract description 60
- 238000004140 cleaning Methods 0.000 title claims abstract description 20
- 230000002255 enzymatic effect Effects 0.000 title description 12
- 102000013142 Amylases Human genes 0.000 claims abstract description 19
- 108010065511 Amylases Proteins 0.000 claims abstract description 19
- 239000002738 chelating agent Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004382 Amylase Substances 0.000 claims abstract description 18
- 235000019418 amylase Nutrition 0.000 claims abstract description 18
- 239000004367 Lipase Substances 0.000 claims abstract description 16
- 102000004882 Lipase Human genes 0.000 claims abstract description 16
- 108090001060 Lipase Proteins 0.000 claims abstract description 16
- 108090000787 Subtilisin Proteins 0.000 claims abstract description 16
- 235000019421 lipase Nutrition 0.000 claims abstract description 16
- CIEZZGWIJBXOTE-UHFFFAOYSA-N 2-[bis(carboxymethyl)amino]propanoic acid Chemical compound OC(=O)C(C)N(CC(O)=O)CC(O)=O CIEZZGWIJBXOTE-UHFFFAOYSA-N 0.000 claims abstract description 14
- PQHYOGIRXOKOEJ-UHFFFAOYSA-N 2-(1,2-dicarboxyethylamino)butanedioic acid Chemical compound OC(=O)CC(C(O)=O)NC(C(O)=O)CC(O)=O PQHYOGIRXOKOEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229940080260 iminodisuccinate Drugs 0.000 claims abstract description 8
- 239000002736 nonionic surfactant Substances 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 4
- 238000012360 testing method Methods 0.000 description 15
- 229940088598 enzyme Drugs 0.000 description 14
- 102000004190 Enzymes Human genes 0.000 description 13
- 108090000790 Enzymes Proteins 0.000 description 13
- 230000000694 effects Effects 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 238000004809 thin layer chromatography Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 229920002527 Glycogen Polymers 0.000 description 5
- 229940096919 glycogen Drugs 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 4
- 229960001484 edetic acid Drugs 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000003755 preservative agent Substances 0.000 description 4
- 102000004169 proteins and genes Human genes 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 102000008100 Human Serum Albumin Human genes 0.000 description 3
- 108091006905 Human Serum Albumin Proteins 0.000 description 3
- 108091005804 Peptidases Proteins 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 239000004365 Protease Substances 0.000 description 3
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 3
- -1 alkylenes glycols Chemical class 0.000 description 3
- 230000000845 anti-microbial effect Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 235000019626 lipase activity Nutrition 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 150000003626 triacylglycerols Chemical class 0.000 description 3
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000004599 antimicrobial Substances 0.000 description 2
- 230000003385 bacteriostatic effect Effects 0.000 description 2
- 235000015165 citric acid Nutrition 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 230000000249 desinfective effect Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 239000000174 gluconic acid Substances 0.000 description 2
- 235000012208 gluconic acid Nutrition 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 229920005862 polyol Polymers 0.000 description 2
- 150000003077 polyols Chemical class 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229940100555 2-methyl-4-isothiazolin-3-one Drugs 0.000 description 1
- QFVHZQCOUORWEI-UHFFFAOYSA-N 4-[(4-anilino-5-sulfonaphthalen-1-yl)diazenyl]-5-hydroxynaphthalene-2,7-disulfonic acid Chemical compound C=12C(O)=CC(S(O)(=O)=O)=CC2=CC(S(O)(=O)=O)=CC=1N=NC(C1=CC=CC(=C11)S(O)(=O)=O)=CC=C1NC1=CC=CC=C1 QFVHZQCOUORWEI-UHFFFAOYSA-N 0.000 description 1
- 229940046305 5-bromo-5-nitro-1,3-dioxane Drugs 0.000 description 1
- 108010059892 Cellulase Proteins 0.000 description 1
- 230000010736 Chelating Activity Effects 0.000 description 1
- 238000011537 Coomassie blue staining Methods 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- 229920005682 EO-PO block copolymer Polymers 0.000 description 1
- OHLUUHNLEMFGTQ-UHFFFAOYSA-N N-methylacetamide Chemical compound CNC(C)=O OHLUUHNLEMFGTQ-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 108010077895 Sarcosine Proteins 0.000 description 1
- 241000219289 Silene Species 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 238000003149 assay kit Methods 0.000 description 1
- OGBUMNBNEWYMNJ-UHFFFAOYSA-N batilol Chemical class CCCCCCCCCCCCCCCCCCOCC(O)CO OGBUMNBNEWYMNJ-UHFFFAOYSA-N 0.000 description 1
- 235000019445 benzyl alcohol Nutrition 0.000 description 1
- 229960004217 benzyl alcohol Drugs 0.000 description 1
- XVBRCOKDZVQYAY-UHFFFAOYSA-N bronidox Chemical compound [O-][N+](=O)C1(Br)COCOC1 XVBRCOKDZVQYAY-UHFFFAOYSA-N 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229940106157 cellulase Drugs 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000002538 fungal effect Effects 0.000 description 1
- 230000001408 fungistatic effect Effects 0.000 description 1
- 238000001502 gel electrophoresis Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000003752 hydrotrope Substances 0.000 description 1
- 230000003165 hydrotropic effect Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- BEGLCMHJXHIJLR-UHFFFAOYSA-N methylisothiazolinone Chemical compound CN1SC=CC1=O BEGLCMHJXHIJLR-UHFFFAOYSA-N 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- NJTGANWAUPEOAX-UHFFFAOYSA-N molport-023-220-454 Chemical compound OCC(O)CO.OCC(O)CO NJTGANWAUPEOAX-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 102000013415 peroxidase activity proteins Human genes 0.000 description 1
- 108040007629 peroxidase activity proteins Proteins 0.000 description 1
- 238000002264 polyacrylamide gel electrophoresis Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 238000002731 protein assay Methods 0.000 description 1
- 231100001260 reprotoxic Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- FSYKKLYZXJSNPZ-UHFFFAOYSA-N sarcosine Chemical compound C[NH2+]CC([O-])=O FSYKKLYZXJSNPZ-UHFFFAOYSA-N 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 229960003885 sodium benzoate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- QUCDWLYKDRVKMI-UHFFFAOYSA-M sodium;3,4-dimethylbenzenesulfonate Chemical class [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1C QUCDWLYKDRVKMI-UHFFFAOYSA-M 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000012192 staining solution Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 229940080258 tetrasodium iminodisuccinate Drugs 0.000 description 1
- GYBINGQBXROMRS-UHFFFAOYSA-J tetrasodium;2-(1,2-dicarboxylatoethylamino)butanedioate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CC(C([O-])=O)NC(C([O-])=O)CC([O-])=O GYBINGQBXROMRS-UHFFFAOYSA-J 0.000 description 1
- LBLYYCQCTBFVLH-UHFFFAOYSA-M toluenesulfonate group Chemical group C=1(C(=CC=CC1)S(=O)(=O)[O-])C LBLYYCQCTBFVLH-UHFFFAOYSA-M 0.000 description 1
- 150000003628 tricarboxylic acids Chemical class 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- GDJZZWYLFXAGFH-UHFFFAOYSA-M xylenesulfonate group Chemical group C1(C(C=CC=C1)C)(C)S(=O)(=O)[O-] GDJZZWYLFXAGFH-UHFFFAOYSA-M 0.000 description 1
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
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38627—Preparations containing enzymes, e.g. protease or amylase containing lipase
-
- 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
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/33—Amino carboxylic acids
-
- 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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3245—Aminoacids
-
- 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
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/20—Industrial or commercial equipment, e.g. reactors, tubes or engines
Definitions
- Enzymatic detergent compositions for the automatic cleaning of surgical and / or medical instruments and / or devices.
- the present invention relates to the use of enzymatic detergent compositions for the automatic cleaning of surgical and / or medical instruments and / or devices.
- LFI automatic instrument washer-disinfector cleaning
- NEodisherĀ® SYSTEM ALPHA which consists of two highly concentrated components, namely an enzymatic component, the neodisherĀ® SystemAct, and an alkaline component, the neodisherĀ® SystemClean.
- the enzymatic component contains a subtilisin while the alkaline component contains triethanolamine and methylglycine diacetic acid (MGDA).
- MGDA methylglycine diacetic acid
- the invention thus relates to the use of a concentrated aqueous detergent composition for cleaning surgical and / or medical instruments in a disinfector washer, said concentrated aqueous detergent composition comprising: - a subtilisin,
- a biodegradable chelating agent selected from acid diacetic methylglycine (MGDA) and an iminodisuccinate (IDS) and
- the concentrated detergent composition of the invention does not exhibit the enzymatic stability problems encountered in the prior art enzyme compositions containing alkanolamines.
- the tri-enzymatic cocktail of the concentrated aqueous detergent composition of the The invention will simultaneously hydrolyze the three targets and thereby facilitate detergency.
- the absence of alkanolamine makes it possible to formulate the detergent composition used according to the invention in a very concentrated manner.
- the water content of the concentrated aqueous detergent composition can be reduced to 25% by weight based on the total weight of composition without having to add significant amounts of third-solvent, impact the stability of the enzymes and harm cleaning efficiency.
- the composition used according to the invention advantageously has a subtilisin content of 0.5 to 15% by weight relative to the total weight of the composition, preferably from 1 to 10% by weight relative to the total weight of the composition, preferably from 1 to 5% by weight relative to the total weight of the composition, more preferably from approximately 3% by weight relative to relative to the total weight of the composition.
- the lipase content is advantageously from 0.05 to 2% by weight relative to the total weight of the composition, preferably from 0.5 to 1.5% by weight relative to the total weight of the composition, more preferably from about 1% by weight relative to the total weight of the composition.
- the content of amylase is advantageously from 0.05 to 2% by weight relative to the total weight of the composition, preferably from 0.5 to 1.5% by weight relative to the total weight of the composition, more preferably from about 1% by weight relative to the total weight of the composition.
- the biodegradable chelating agent is chosen from methylglycine diacetic acid (MGDA) and an iminodisuccinate (IDS), in particular tetrasodium iminodisuccinate.
- MGDA methylglycine diacetic acid
- IDS iminodisuccinate
- the biodegradable chelating agent is methylglycine diacetic acid (MGDA).
- MGDA methylglycine diacetic acid
- the chelating agent used in the present invention not only serves to soften water but also to complex particularly efficiently bi-metal ions and trivalents, in particular Ca 2+ , Fe 3+ , Fe 2+ and Cu 2+ , contained in the protein residues typically found on surgical and / or medical instruments. It seems that these chelating agents sequester these metal ions which destabilizes the tertiary structure of proteins and makes them more easily hydrolyzable.
- the composition used according to the invention advantageously has a content of biodegradable chelating agent of 10 to 50% by weight relative to the total weight of the composition, preferably from 20 to 40% by weight relative to the total weight of the composition, more preferably 25 to 35% by weight relative to the total weight of the composition, more preferably still approximately 30% by weight relative to the total weight of the composition.
- the concentrated aqueous detergent composition is advantageously free from any non-bio-degradable chelating agent, especially ethylene-diamine tetraacetic acid (EDTA), diethylene triamine acid, pentaacetic acid (DTPA), phosphates and polyphosphates.
- EDTA ethylene-diamine tetraacetic acid
- DTPA pentaacetic acid
- phosphates and polyphosphates are advantageously, especially ethylene-diamine tetraacetic acid (EDTA), diethylene triamine acid, pentaacetic acid (DTPA), phosphates and polyphosphates.
- the concentrated aqueous detergent composition is also free of any chelating agent classified as reprotoxic such as nitrilotriacetic acid and its sodium salt (NTA).
- the concentrated aqueous detergent composition is also free of alkali and alkaline earth hydroxides.
- the water content of the concentrated detergent composition used according to the invention is advantageously from 10 to 50% by weight relative to the total weight of the composition, preferably from 15 to 45% by weight relative to the total weight of the composition. more preferably from 20 to 40% by weight relative to the total weight of the composition and more preferably still from 25 to 40% by weight relative to the total weight of the composition.
- the concentrated detergent composition may also contain a third solvent such as a polyol.
- suitable polyols include alkylenes glycols such as ethylene glycol, propylene glycol and glycerine (1,2,3-propanetriol).
- the third-solvent is glycerin.
- Glycerine has the advantage of not only serving as a third-solvent but also stabilizing the enzymes.
- the content of the third-solvent is advantageously from 5 to 50% by weight relative to the total weight of the composition, preferably from 10 to 40% by weight relative to the total weight of the composition, more preferably from 13 to 25% by weight. weight relative to the total weight of the composition.
- the concentrated detergent composition used in accordance with the invention may further comprise one or more nonionic surfactants.
- the nonionic surfactant (s) may, in particular, be chosen from alkoxylated nonionic surfactants and alkylpolyglucosides.
- the alkoxylated nonionic surfactants are advantageously chosen from alkoxylated nonionic surfactants, especially from alkoxylated fatty alcohols, especially ethoxylated and / or propoxylated, and EO-PO block copolymers.
- the nonionic surfactant (s) are chosen from alkylpolyglucosides, preferably it is a C7 alkylpolyglucoside. This alkylpolyglucoside provides the triple advantage of acting as a stabilizer, to provide a favorable wetting effect for detergency and a non-foaming character compatible with an application in washer disinfector.
- the content of nonionic surfactant in the detergent composition used according to the invention is advantageously from 1 to 10, preferably from 2 to 5, more preferably from approximately 3% by weight relative to the total weight of the composition.
- the detergent composition used in accordance with the invention may further comprise an acid or buffer system for adjusting the pH.
- an organic acid is added, chosen from the C 2 -C 6 mono-, di- and tricarboxylic acids, chosen in particular from citric acid, tartaric acid, malic acid, lactic acid, glutaric acid, gluconic acid, glycolic acid, succinic acid and adipic acid.
- Citric acid is particularly preferred. It has the advantage of serving at the same time as complexing agent as well as tartaric acid and gluconic acid.
- the composition will contain no antimicrobial agent, especially no antimicrobial amine, and therefore have no claim for antimicrobial activity at the dose of use.
- the detergent composition used according to the invention may also comprise a preservative agent.
- the preserving agent may be chosen from the usual preserving agents, such as, for example, 5-chloro-5-methyl-4-isothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, p-acid and the like. hydroxybenzoic acid and its methyl esters, 5-bromo-5-nitro-1,3-dioxane and salicylic acid, benzyl alcohol and sodium benzoate. These Preservatives help prevent microbial and fungal contamination by providing a bacteriostatic and fungistatic effect.
- the detergent composition used according to the invention may also comprise a hydrotropic agent.
- This hydrotrope agent may for example be selected from xylene sulfonates, toluenesulfonates, cumenesulfonates, urea, methylacetamide, polyethylene glycol and polypropylene glycol.
- the concentrated detergent composition used according to the invention may further comprise other adjuvants such as, for example, dispersing agents and / or antifoaming agents.
- the dispersing agents may for example be acids of homo-, co- or terpolymers based on acrylic acid or alkali metal salts thereof (polyacrylates).
- the detergent composition is implemented in a washer disinfector (LD) such as an instrument washer-disinfector (LDI) or an endoscope washer-disinfector (LDE).
- LD washer disinfector
- LLI instrument washer-disinfector
- LDE endoscope washer-disinfector
- the term "washer-disinfectorā is to be understood as defined in ISO 15883-1: 2006, namely a machine for cleaning and disinfecting medical devices and all other articles used in the medical, dental, pharmaceutical and veterinary.
- surgical and / or medical instruments as used in the present application is to be broadly understood as referring to medical devices and all other articles used in the medical, dental, pharmaceutical and veterinary environments requiring cleaning. with aqueous detergents before reuse.
- this cleaning is advantageously carried out at a temperature of 20 to 60 Ā° C, preferably 45 to 55 Ā° C, more preferably 50 to 55 Ā° C.
- the cleaning time is advantageously between 20 s and 10 min, preferably between 30 s and 5 min.
- the present invention also relates to the concentrated aqueous detergent composition implemented in the use according to the invention as described above.
- This composition is to be diluted with water, preferably softened, demineralized or osmosis, before use.
- the dilution is generally from 0.03% to 1% (v / v), preferably from 0.1% to 0.6% (v / v), more preferably from 0.2 to 0.4% (v / v). .
- the pH of the diluted ready-to-use composition is advantageously from 8 to 11, preferably from 8.5 to 9.5, more preferably from 8.8 to 9.2, and even more preferably from about 9. determination of the pH of the diluted composition, softened water is used (degree of hardness about 5 Ā° f).
- Figure 1 Photos of the onboard detergency tests for compositions C1, C2 and C3.
- FIG. 1 Evaluation of the activity of subtilisin by gel electrophoresis.
- Figure 3 Evaluation of lipase activity by chromato graphy on thin layer.
- Figure 4 Evaluation of the activity of amylase by thin layer chromatography.
- Table 1 The following three concentrated detergent compositions (Table 1) were evaluated for their ability to effectively clean up residues typically found on surgical and medical instruments. Table 1
- composition Cl The performance of the composition Cl was compared to that of AnisoymeĀ® DLM Maxi (Anios Laboratories, Hellemmes, France), a tri-enzyme detergent containing a protease, a lipase, an amylase and the EDTA chelating agent.
- composition according to the invention allows a more efficient cleaning at low temperatures and dosage. This is all the more surprising since the chelating activity of EDTA is higher than that of MGDA, which would allow a higher cleaning efficiency for ā AniosymeĀ® DLM Maxi.
- composition C1 The respective stabilities of subtilisin, lipase and amylase in the composition C1 were evaluated by the following tests.
- subtilisin contained in the detergent is followed by the technique of polyacrylamide gel electrophoresis, the substrate used is a solution of 0.3% human serum albumin (soil representative of an application in a health facility ).
- FIG. 2 shows four electrophoresis tracks: lane 1 corresponds to the control (human serum albumin (0.3%), non-degraded), lanes 2, 3 and 4 to the composition Cl after manufacture, 3 weeks of storage in a container tightly closed at 30 Ā° C and 7 weeks storage in a tightly closed container at 30 Ā° C respectively. It is found that the enzymatic activity of subtilisin does not degrade for at least 7 weeks.
- the lipase activity was followed by the Thin Layer Chromatography (TLC) technique, the substrate used is a triglyceride and the eluent a mixture of 50 ml of heptane, 20 ml of diethyl ether, 0 5 mL of acetic acid and 1.5 mL of ethanol.
- TLC Thin Layer Chromatography
- Triglyceride-degrading lipase the absence of triglycerides, and the presence of diglycerides and monglycerides demonstrate the enzymatic activity of lipase.
- Figure 3 shows six TLC tracks: lanes 1, 2, 3 correspond to controls (1: triglycerides, 2: diglycerides, 3: monoglycerides), lanes 4, 5 and 6 to composition Cl after manufacture, after 3 weeks storage in a tightly closed container at 30 Ā° C and after 7 weeks of storage in a tightly closed container at 30 Ā° C respectively. It is found that the enzymatic activity of the lipase does not degrade for at least 7 weeks.
- the amylase activity was followed by the Thin Layer Chromatography (TLC) technique, the substrate used is glycogen and the eluent a mixture of 70 mL of ethanol, 1 mL of acetic acid and 29 mL of demineralised water.
- TLC Thin Layer Chromatography
- FIG. 4 shows five TLC tracks: lanes 1 and 2 correspond to the controls (1: glycogen, 2: glucose), lanes 3, 4 and 5 to the Cl composition after manufacture, after 3 weeks of storage in a hermetically sealed container closed at 30 Ā° C and after 7 weeks of storage in a tightly closed container at 30 Ā° C respectively. It is found that the enzymatic activity of the amylase does not degrade for at least 7 weeks.
- composition C1 The influence of the presence of the three subtilisin, lipase and amylase enzymes in the detergent composition was evaluated by comparing the composition C1 to compositions without enzymes (C4), with subtilisin (C5) and with lipase and amylase (C6).
- the degreasing cleansing power of the various compositions was evaluated with respect to English soil according to the ISO 15883 standard which was applied by brush on stainless steel blades (one blade per composition tested) and allowed to dry for one hour at ambient temperature. Then each slide was quenched with stirring (three-dimensional stirrer, 50 rpm) for 15 min at room temperature in one of the four detergent compositions diluted to 0.3% (v / v) in softened water (5%).
- composition Cl The best results were obtained for the composition Cl.
- Residual protein assay using the MicroBCA technique (INTERCHIM UPTIMA MicroBC Assay kit, UP75860A reference) confirms these observations.
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Detergent Compositions (AREA)
Abstract
The invention relates to the use of a concentrated aqueous detergent composition for the cleaning of surgical and/or medical instruments in a washer-disinfector, said concentrated aqueous detergent composition comprising: a subtilisin, a lipase, an amylase, a biodegradable chelating agent selected from among methyl glycine diacetic acid and an iminodisuccinate, and water, said concentrated detergent composition being free of alkanolamine.
Description
Compositions dĆ©tergentes enzymatiques pour le nettoyage automatique d'instruments et/ou appareils chirurgicaux et/ou mĆ©dicaux. Ā Enzymatic detergent compositions for the automatic cleaning of surgical and / or medical instruments and / or devices.
La prƩsente invention concerne l'utilisation de compositions dƩtergentes enzymatiques pour le nettoyage automatique d'instruments et/ou appareils chirurgicaux et/ou mƩdicaux. The present invention relates to the use of enzymatic detergent compositions for the automatic cleaning of surgical and / or medical instruments and / or devices.
En milieu hospitalier, les instruments chirurgicaux sont en gĆ©nĆ©ral soumis Ć un nettoyage automatique en laveur dĆ©sinfecteur d'instruments (LDI) en utilisant des dĆ©tergents fortement alcalins suivi d'une dĆ©sinfection thermique ou chimique. Ces dĆ©tergents ont gĆ©nĆ©ralement un pH supĆ©rieur Ć 12 ce qui les rends trĆØs corrosifs. In hospital settings, surgical instruments are usually subjected to an automatic instrument washer-disinfector cleaning (LDI) using strongly alkaline detergents followed by thermal or chemical disinfection. These detergents generally have a pH greater than 12 which makes them very corrosive.
Pour Ć©viter les dommages causĆ©s par ces dĆ©tergents alcalins, des dĆ©tergents enzymatiques ont Ć©tĆ© proposĆ©s. On connaĆ®t par exemple le MEDICLEANĀ® forte de Dr. Weigert qui fait d'ailleurs l'objet du brevet europĆ©en EP 1 327 674 B l . Ce dĆ©tergent contient de la triĆ©thanolamine, de l'acide nitrilotriacĆ©tique (NTA) comme agent chĆ©latant, des phosphates et une protĆ©ase. La prĆ©sence simultanĆ©e d'une alcanolamine et d'une enzyme dans une mĆŖme composition pose des problĆØmes de stabilitĆ© pour l'enzyme, notamment lorsque la composition est trĆØs concentrĆ©e. To avoid the damage caused by these alkaline detergents, enzymatic detergents have been proposed. We know, for example, the MEDICLEANĀ® forte of Dr. Weigert, which is also the subject of the European patent EP 1,327,674 B1. This detergent contains triethanolamine, nitrilotriacetic acid (NTA) as a chelating agent, phosphates and a protease. The simultaneous presence of an alkanolamine and an enzyme in the same composition poses stability problems for the enzyme, especially when the composition is very concentrated.
C'est pourquoi Dr. Weigert a dĆ©veloppĆ© le neodisherĀ® SYSTEM ALPHA qui est composĆ© de deux composantes trĆØs concentrĆ©s distinctes, Ć savoir une composante enzymatique, le neodisherĀ® SystemAct, et une composante alcaline, le neodisherĀ® SystemClean. La composante enzymatique contient une subtilisine tandis que la composante alcaline contient de la triĆ©thanolamine et de l'acide mĆ©thylglycine diacĆ©tique (MGDA). Ce systĆØme fait d'ailleurs l'objet de la demande de brevet internationale WO2015/043777. That's why Dr. Weigert developed the NEodisherĀ® SYSTEM ALPHA which consists of two highly concentrated components, namely an enzymatic component, the neodisherĀ® SystemAct, and an alkaline component, the neodisherĀ® SystemClean. The enzymatic component contains a subtilisin while the alkaline component contains triethanolamine and methylglycine diacetic acid (MGDA). This system is also the subject of the international patent application WO2015 / 043777.
MĆŖme si ce systĆØme permet de rĆ©soudre les problĆØmes liĆ©s Ć l'instabilitĆ© de l'enzyme en prĆ©sence de fortes concentrations d'agents alcalins comme les alcanolamines, il prĆ©sente un dĆ©savantage majeur en ce qu'il nĆ©cessite
un Ć©quipement spĆ©cifique pour pouvoir alimenter le laveur dĆ©sinfecteur d'instruments avec les deux composantes simultanĆ©ment. Les laveurs dĆ©sinfecteurs d'instruments ne possĆØdent en effet qu'une alimentation de composition dĆ©tergente. Le brevet US 7,723,281 dĆ©crit une composition dĆ©tergente comprenant un systĆØme enzymatique stabilisĆ©. Ce systĆØme enzymatique comprend au moins une enzyme mais peut en comprendre plusieurs, tel qu'une protĆ©ase, une amylase, une lipase, une gluconase, une cellulase, une peroxidase ou un mĆ©lange de celles-ci, ainsi qu'un agent chĆ©latant. Selon la description, l'effet stabilisant est obtenu grĆ¢ce Ć l'incorporation d'une aminĆ©, notamment anti-microbienne, et d'un acide dans un ratio molaire spĆ©cifique. Although this system makes it possible to solve the problems related to the instability of the enzyme in the presence of high concentrations of alkaline agents such as alkanolamines, it presents a major disadvantage in that it requires specific equipment to be able to feed the instrument washer-disinfector with both components simultaneously. Instrument disinfecting washers only have a detergent composition supply. US Patent 7,723,281 discloses a detergent composition comprising a stabilized enzyme system. This enzyme system comprises at least one enzyme but may include several, such as a protease, an amylase, a lipase, a gluconase, a cellulase, a peroxidase or a mixture thereof, as well as a chelating agent. According to the description, the stabilizing effect is obtained thanks to the incorporation of an amine, in particular anti-microbial, and an acid in a specific molar ratio.
Il existe donc toujours un besoin d'un moyen pour nettoyer efficacement les instruments chirurgicaux et mĆ©dicaux en machine sans prĆ©senter les problĆØmes de stabilitĆ© des solutions proposĆ©es dans l'Ć©tat de la technique et sans nĆ©cessiter un appareillage spĆ©cifique pour pouvoir alimenter les machines utilisĆ©es pour le nettoyage. There is therefore still a need for a means for effectively cleaning the surgical and medical instruments in the machine without presenting the stability problems of the solutions proposed in the state of the art and without the need for specific equipment to power the machines used for the cleaning.
Il est du mĆ©rite de la Demanderesse d'avoir trouvĆ© au fruit de nombreuses recherches que ces inconvĆ©nients pouvaient ĆŖtre palliĆ©s en utilisant une composition dĆ©tergente concentrĆ©e qui repose sur la combinaison de trois enzymes et d'un agent chĆ©latant puissant et qui ne contient pas d'alcanolamine. It is the merit of the Applicant to have found in the fruit of much research that these disadvantages could be overcome by using a concentrated detergent composition which is based on the combination of three enzymes and a powerful chelating agent and which does not contain any alkanolamine.
L'invention concerne donc l'utilisation d'une composition dƩtergente aqueuse concentrƩe pour le nettoyage d'instruments chirurgicaux et/ou mƩdicaux en laveur dƩsinfecteur, ladite composition dƩtergente aqueuse concentrƩe comprenant : - une subtilisine, The invention thus relates to the use of a concentrated aqueous detergent composition for cleaning surgical and / or medical instruments in a disinfector washer, said concentrated aqueous detergent composition comprising: - a subtilisin,
une lipase, Ā a lipase,
une amylase, Ā an amylase,
un agent chƩlatant biodƩgradable choisi parmi l'acide
mƩthylglycine diacƩtique (MGDA) et un iminodisuccinate (IDS) et a biodegradable chelating agent selected from acid diacetic methylglycine (MGDA) and an iminodisuccinate (IDS) and
de l'eau, ladite composition dĆ©tergente concentrĆ©e Ć©tant exempte d' alcanolamine. De faƧon tout Ć fait surprenante, cette combinaison spĆ©cifique d'une subtilisine, d'une lipase et d'une amylase avec du MGDA ou de l'IDS permet de s'affranchir de la nĆ©cessitĆ© de l'ajout d' alcanolamine tout en maintenant un nettoyage efficace d'instruments chirurgicaux et/ou mĆ©dicaux souillĆ©s en laveur dĆ©sinfecteur. Ainsi, la composition dĆ©tergente aqueuse concentrĆ©e de l'invention ne prĆ©sente pas les problĆØmes de stabilitĆ© enzymatique rencontrĆ©s dans les compositions enzymatiques de l'art antĆ©rieur contenant des alcanolamines. Ā water, said concentrated detergent composition being free of alkanolamine. Quite surprisingly, this specific combination of a subtilisin, a lipase and an amylase with MGDA or IDS makes it possible to overcome the need for the addition of alkanolamine while maintaining effective cleaning of surgical and / or medical instruments contaminated with a washer disinfector. Thus, the concentrated aqueous detergent composition of the invention does not exhibit the enzymatic stability problems encountered in the prior art enzyme compositions containing alkanolamines.
De plus, Ć©tant donnĆ© que les principaux composants des tissus biologiques qui constituent des souillures majeures des instruments chirurgicaux et mĆ©dicaux sont protĆ©ines, lipides (triglycĆ©rides) et polymĆØres glucidiques (glycogĆØne), le cocktail tri-enzymatique de la composition dĆ©tergente aqueuse concentrĆ©e de l'invention hydrolysera simultanĆ©ment les trois cibles et donc en facilitera la dĆ©tergence. Moreover, since the main components of biological tissues that constitute major stains of surgical and medical instruments are proteins, lipids (triglycerides) and carbohydrate polymers (glycogen), the tri-enzymatic cocktail of the concentrated aqueous detergent composition of the The invention will simultaneously hydrolyze the three targets and thereby facilitate detergency.
De plus, l'absence d' alcanolamine permet de formuler la composition dĆ©tergente utilisĆ©e conformĆ©ment Ć l'invention de faƧon trĆØs concentrĆ©e. Ainsi, la teneur en eau de la composition dĆ©tergente aqueuse concentrĆ©e peut ĆŖtre rĆ©duite jusqu'Ć 25 % en poids par rapport au poids total de composition sans pour autant devoir ajouter de quantitĆ©s importantes de tiers- solvant, impacter la stabilitĆ© des enzymes et nuire Ć l'efficacitĆ© de nettoyage. In addition, the absence of alkanolamine makes it possible to formulate the detergent composition used according to the invention in a very concentrated manner. Thus, the water content of the concentrated aqueous detergent composition can be reduced to 25% by weight based on the total weight of composition without having to add significant amounts of third-solvent, impact the stability of the enzymes and harm cleaning efficiency.
La composition utilisĆ©e conformĆ©ment Ć l'invention a avantageusement une teneur en subtilisine de 0,5 Ć 15% en poids par rapport au poids total de la composition, de prĆ©fĆ©rence de 1 Ć 10% en poids par rapport au poids total de la composition, de prĆ©fĆ©rence de 1 Ć 5% en poids par rapport au poids total de la composition, plus prĆ©fĆ©rentiellement d'environ 3% en poids par
rapport au poids total de la composition. La teneur en lipase est avantageusement de 0,05 Ć 2% en poids par rapport au poids total de la composition, de prĆ©fĆ©rence de 0,5 Ć 1,5% en poids par rapport au poids total de la composition, plus prĆ©fĆ©rentiellement d'environ 1% en poids par rapport au poids total de la composition. La teneur en amylase est avantageusement de 0,05 Ć 2% en poids par rapport au poids total de la composition, de prĆ©fĆ©rence de 0,5 Ć 1,5% en poids par rapport au poids total de la composition, plus prĆ©fĆ©rentiellement d'environ 1% en poids par rapport au poids total de la composition. The composition used according to the invention advantageously has a subtilisin content of 0.5 to 15% by weight relative to the total weight of the composition, preferably from 1 to 10% by weight relative to the total weight of the composition, preferably from 1 to 5% by weight relative to the total weight of the composition, more preferably from approximately 3% by weight relative to relative to the total weight of the composition. The lipase content is advantageously from 0.05 to 2% by weight relative to the total weight of the composition, preferably from 0.5 to 1.5% by weight relative to the total weight of the composition, more preferably from about 1% by weight relative to the total weight of the composition. The content of amylase is advantageously from 0.05 to 2% by weight relative to the total weight of the composition, preferably from 0.5 to 1.5% by weight relative to the total weight of the composition, more preferably from about 1% by weight relative to the total weight of the composition.
L'agent chĆ©latant biodĆ©gradable est choisi parmi l'acide mĆ©thylglycine diacĆ©tique (MGDA) et un iminodisuccinate (IDS), notamment l'iminodisuccinate tĆ©trasodique. De prĆ©fĆ©rence, l'agent chĆ©latant biodĆ©gradable est de l'acide mĆ©thylglycine diacĆ©tique (MGDA). Sans vouloir ĆŖtre liĆ© par une quelconque thĆ©orie, les inventeurs pensent que l'agent chĆ©latant mis en Åuvre dans la prĆ©sente invention ne sert pas uniquement Ć l'adoucissement de l'eau mais aussi Ć complexer de maniĆØre particuliĆØrement efficace des ions mĆ©talliques bi- et trivalents, notamment Ca2+, Fe3+, Fe2+ et Cu2+, contenus dans les rĆ©sidus protĆ©iques retrouvĆ©s typiquement sur les instruments chirurgicaux et/ou mĆ©dicaux. Il semblerait que ces agents chĆ©latants sĆ©questrent ces ions mĆ©talliques ce qui dĆ©stabilise la structure tertiaire des protĆ©ines et les rends plus facilement hydrolysables. The biodegradable chelating agent is chosen from methylglycine diacetic acid (MGDA) and an iminodisuccinate (IDS), in particular tetrasodium iminodisuccinate. Preferably, the biodegradable chelating agent is methylglycine diacetic acid (MGDA). Without wishing to be bound by any theory, the inventors believe that the chelating agent used in the present invention not only serves to soften water but also to complex particularly efficiently bi-metal ions and trivalents, in particular Ca 2+ , Fe 3+ , Fe 2+ and Cu 2+ , contained in the protein residues typically found on surgical and / or medical instruments. It seems that these chelating agents sequester these metal ions which destabilizes the tertiary structure of proteins and makes them more easily hydrolyzable.
La composition utilisĆ©e conformĆ©ment Ć l'invention a avantageusement une teneur en agent chĆ©latant biodĆ©gradable de 10 Ć 50% en poids par rapport au poids total de la composition, de prĆ©fĆ©rence de 20 Ć 40% en poids par rapport au poids total de la composition, plus prĆ©fĆ©rentiellement de 25 Ć 35% en poids par rapport au poids total de la composition, plus prĆ©fĆ©rentiellement encore d'environ 30% en poids par rapport au poids total de la composition. The composition used according to the invention advantageously has a content of biodegradable chelating agent of 10 to 50% by weight relative to the total weight of the composition, preferably from 20 to 40% by weight relative to the total weight of the composition, more preferably 25 to 35% by weight relative to the total weight of the composition, more preferably still approximately 30% by weight relative to the total weight of the composition.
La composition dĆ©tergente aqueuse concentrĆ©e est avantageusement exempte de tout agent chĆ©latant non bio-dĆ©gradable, notamment d'acide Ć©thylĆØne-diamine-tĆ©traacĆ©tique (EDTA), acide diĆ©thylĆØne-triamine-
pentaacƩtique (DTPA), phosphates et polyphosphates. Avantageusement, la composition dƩtergente aqueuse concentrƩe est Ʃgalement exempte de tout agent chƩlatant classƩ rƩprotoxique tel que l'acide nitrilotriacƩtique et son sel de sodium (NTA). Dans un mode de rƩalisation, la composition dƩtergente aqueuse concentrƩe est Ʃgalement exempte d'hydroxydes alcalins et alcalinoterreux. The concentrated aqueous detergent composition is advantageously free from any non-bio-degradable chelating agent, especially ethylene-diamine tetraacetic acid (EDTA), diethylene triamine acid, pentaacetic acid (DTPA), phosphates and polyphosphates. Advantageously, the concentrated aqueous detergent composition is also free of any chelating agent classified as reprotoxic such as nitrilotriacetic acid and its sodium salt (NTA). In one embodiment, the concentrated aqueous detergent composition is also free of alkali and alkaline earth hydroxides.
La teneur en eau de la composition dĆ©tergente concentrĆ©e utilisĆ©e conformĆ©ment Ć l'invention est avantageusement de 10 Ć 50 % en poids par rapport au poids total de la composition, de prĆ©fĆ©rence de 15 Ć 45 % en poids par rapport au poids total de la composition, plus prĆ©fĆ©rentiellement de 20 Ć 40 % en poids par rapport au poids total de la composition et plus prĆ©fĆ©rentiellement encore de 25 Ć 40% en poids par rapport au poids total de la composition. En plus de l'eau, la composition dĆ©tergente concentrĆ©e peut Ć©galement contenir un tiers- solvant tel un polyol. Des exemples de polyols appropriĆ©s comprennent notamment les alkylĆØnes glycols tels que l'Ć©thylĆØne glycol, le propylĆØne glycol et la glycĆ©rine (1,2,3-propanetriol). De prĆ©fĆ©rence, le tiers-solvant est la glycĆ©rine. La glycĆ©rine a l'avantage de ne pas servir uniquement de tiers-solvant mais de stabiliser Ć©galement les enzymes. The water content of the concentrated detergent composition used according to the invention is advantageously from 10 to 50% by weight relative to the total weight of the composition, preferably from 15 to 45% by weight relative to the total weight of the composition. more preferably from 20 to 40% by weight relative to the total weight of the composition and more preferably still from 25 to 40% by weight relative to the total weight of the composition. In addition to water, the concentrated detergent composition may also contain a third solvent such as a polyol. Examples of suitable polyols include alkylenes glycols such as ethylene glycol, propylene glycol and glycerine (1,2,3-propanetriol). Preferably, the third-solvent is glycerin. Glycerine has the advantage of not only serving as a third-solvent but also stabilizing the enzymes.
La teneur en tiers-solvant est avantageusement de 5 Ć 50 % en poids par rapport au poids total de la composition, de prĆ©fĆ©rence de 10 Ć 40 % en poids par rapport au poids total de la composition, plus prĆ©fĆ©rentiellement de 13 Ć 25 % en poids par rapport au poids total de la composition. The content of the third-solvent is advantageously from 5 to 50% by weight relative to the total weight of the composition, preferably from 10 to 40% by weight relative to the total weight of the composition, more preferably from 13 to 25% by weight. weight relative to the total weight of the composition.
La composition dĆ©tergente concentrĆ©e utilisĆ©e conformĆ©ment Ć l'invention peut en outre comprendre un ou plusieurs tensioactifs non ioniques. Le ou les agents tensioactifs non ioniques peuvent notamment ĆŖtre choisis parmi les tensioactifs non ioniques alcoxylĆ©s et les alkylpolyglucosides. Les tensioactifs non ioniques alcoxylĆ©s sont avantageusement choisis parmi les tensioactifs non ioniques alcoxylĆ©s, notamment parmi les alcools gras alcoxylĆ©s, notamment
Ć©thoxylĆ©s et/ou propoxylĆ©s, et les copolymĆØres blocs EO-PO. Dans un mode de rĆ©alisation prĆ©fĆ©rĆ©, le ou les agents tensioactifs non ioniques sont choisis parmi les alkylpolyglucosides, de prĆ©fĆ©rence il s'agit d'un alkylpolyglucoside en C7. Cet alkylpolyglucoside apporte en effet le triple avantage de jouer un rĆ“le de stabilisant, d'apporter un effet mouillant favorable Ć la dĆ©tergence et un caractĆØre non-moussant compatible avec une application en laveur dĆ©sinfecteur. The concentrated detergent composition used in accordance with the invention may further comprise one or more nonionic surfactants. The nonionic surfactant (s) may, in particular, be chosen from alkoxylated nonionic surfactants and alkylpolyglucosides. The alkoxylated nonionic surfactants are advantageously chosen from alkoxylated nonionic surfactants, especially from alkoxylated fatty alcohols, especially ethoxylated and / or propoxylated, and EO-PO block copolymers. In a preferred embodiment, the nonionic surfactant (s) are chosen from alkylpolyglucosides, preferably it is a C7 alkylpolyglucoside. This alkylpolyglucoside provides the triple advantage of acting as a stabilizer, to provide a favorable wetting effect for detergency and a non-foaming character compatible with an application in washer disinfector.
La teneur en tensioactif non ionique dans la composition dĆ©tergente utilisĆ©e conformĆ©ment Ć l'invention est avantageusement de 1 Ć 10 , de prĆ©fĆ©rence de 2 Ć 5 , plus prĆ©fĆ©rentiellement d'environ 3 % en poids par rapport au poids total de la composition. The content of nonionic surfactant in the detergent composition used according to the invention is advantageously from 1 to 10, preferably from 2 to 5, more preferably from approximately 3% by weight relative to the total weight of the composition.
La composition dĆ©tergente utilisĆ©e conformĆ©ment Ć l'invention peut en outre comprendre un acide ou un systĆØme de tampon pour ajuster le pH. De prĆ©fĆ©rence, on ajoute un acide organique, choisi parmi les acides en C2-C6 mono-, di- et tricarboxyliques, notamment choisi parmi l'acide citrique, l'acide tartrique, l'acide malique, l'acide lactique, l'acide glutarique, l'acide gluconique l'acide glycolique, l'acide succinique et l'acide adipique. L'acide citrique est particuliĆØrement prĆ©fĆ©rĆ©. Elle prĆ©sente l'avantage de servir en mĆŖme temps comme agent complexant comme Ć©galement l'acide tartrique et l'acide gluconique. Avantageusement, la composition ne contiendra pas d'agent antimicrobien, notamment pas d' aminĆ© antimicrobienne, et n'aura donc aucune revendication d'activitĆ© antimicrobienne Ć la dose d'emploi. Celle-ci est Ć distinguer d'un effet bactĆ©riostatique qui par contre pourra ĆŖtre recherchĆ©. A cet effet, la composition dĆ©tergente utilisĆ©e conformĆ©ment Ć l'invention peut Ć©galement comprendre un agent conservateur. L'agent conservateur peut ĆŖtre choisi parmi les agents conservateurs habituellement utilisĆ©s, comme par exemple le 5-chloro-5-mĆ©thyl-4-isothiazoline-3-one, le 2-mĆ©thyl-4-isothiazolin3-one, l'acide p-hydroxybenzoĆÆque et ses esters de mĆ©thyl, le 5-bromo-5-nitro-l,3- dioxane et l'acide salicylique, l'alcool benzylique et le benzoate de sodium. Ces
agents conservateurs permettent d'Ʃviter une contamination microbienne et fongique en apportant un effet bactƩriostatique et fongistatique. The detergent composition used in accordance with the invention may further comprise an acid or buffer system for adjusting the pH. Preferably, an organic acid is added, chosen from the C 2 -C 6 mono-, di- and tricarboxylic acids, chosen in particular from citric acid, tartaric acid, malic acid, lactic acid, glutaric acid, gluconic acid, glycolic acid, succinic acid and adipic acid. Citric acid is particularly preferred. It has the advantage of serving at the same time as complexing agent as well as tartaric acid and gluconic acid. Advantageously, the composition will contain no antimicrobial agent, especially no antimicrobial amine, and therefore have no claim for antimicrobial activity at the dose of use. This is to be distinguished from a bacteriostatic effect that can be sought. For this purpose, the detergent composition used according to the invention may also comprise a preservative agent. The preserving agent may be chosen from the usual preserving agents, such as, for example, 5-chloro-5-methyl-4-isothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, p-acid and the like. hydroxybenzoic acid and its methyl esters, 5-bromo-5-nitro-1,3-dioxane and salicylic acid, benzyl alcohol and sodium benzoate. These Preservatives help prevent microbial and fungal contamination by providing a bacteriostatic and fungistatic effect.
La composition dĆ©tergente utilisĆ©e conformĆ©ment Ć l'invention peut Ć©galement comprendre un agent hydrotrope. Cet agent hydrotrope peut par exemple ĆŖtre choisi parmi les xylĆØnesulfonates, les toluĆØnesulfonates, les cumĆØnes sulfonates, l'urĆ©e, le mĆ©thylacĆ©tamide, du polyĆ©thylĆØneglycol et du polypropylĆØneglycol. The detergent composition used according to the invention may also comprise a hydrotropic agent. This hydrotrope agent may for example be selected from xylene sulfonates, toluenesulfonates, cumenesulfonates, urea, methylacetamide, polyethylene glycol and polypropylene glycol.
La composition dĆ©tergente concentrĆ©e utilisĆ©e conformĆ©ment Ć l'invention peut en outre comprendre d'autres adjuvants tels que par exemple des agents dispersants et/ou des agents anti-mousse. Les agents dispersants peuvent par exemple ĆŖtre des acides des homo-, co- ou terpolymĆØres Ć base d'acide acrylique ou des sels de mĆ©taux alcalins de ceux-ci (polyacrylates). The concentrated detergent composition used according to the invention may further comprise other adjuvants such as, for example, dispersing agents and / or antifoaming agents. The dispersing agents may for example be acids of homo-, co- or terpolymers based on acrylic acid or alkali metal salts thereof (polyacrylates).
Dans l'utilisation selon l'invention, la composition dĆ©tergente est mise en Åuvre dans un laveur dĆ©sinfecteur (LD) tel qu'un laveur dĆ©sinfecteur d'instruments (LDI) ou un laveur dĆ©sinfecteur d'endoscope (LDE). Le terme Ā« laveur dĆ©sinfecteur Ā» est Ć comprendre tel qu'il est dĆ©fini dans la norme ISO 15883-1 :2006, Ć savoir une machine destinĆ©e Ć nettoyer et dĆ©sinfecter des dispositifs mĆ©dicaux et tous les autres articles utilisĆ©s dans les milieux mĆ©dical, dentaire, pharmaceutique et vĆ©tĆ©rinaire. Aussi, le terme Ā« instruments chirurgicaux et/ou mĆ©dicaux Ā» tels qu'utilisĆ© dans la prĆ©sente demande est Ć comprendre de faƧon large comme dĆ©signant les dispositifs mĆ©dicaux et tous les autres articles utilisĆ©s dans les milieux mĆ©dical, dentaire, pharmaceutique et vĆ©tĆ©rinaire nĆ©cessitant un nettoyage avec des dĆ©tergents aqueux avant rĆ©utilisation. Dans la prĆ©sente invention, ce nettoyage est avantageusement mise en Åuvre Ć une tempĆ©rature de 20 Ć 60 Ā°C, de prĆ©fĆ©rence de 45 Ć 55 Ā°C, plus prĆ©fĆ©rentiellement de 50 Ć 55 Ā°C. La durĆ©e de nettoyage est avantageusement comprise entre 20 s et 10 min, de prĆ©fĆ©rence entre 30 s et 5 min.
La prĆ©sente invention porte Ć©galement sur la composition dĆ©tergente aqueuse concentrĆ©e mise en Åuvre dans l'utilisation selon l'invention telle que dĆ©crite ci-dessus. Cette composition est Ć diluer avec de l'eau, prĆ©fĆ©rentiellement adoucie, dĆ©minĆ©ralisĆ©e ou osmosĆ©e, avant emploi. La dilution est gĆ©nĆ©ralement de 0,03% Ć 1% (v/v), de prĆ©fĆ©rence de 0, 1% Ć 0.6% (v/v), plus prĆ©fĆ©rentiellement de 0,2 Ć 0,4% (v/v). Le pH de la composition diluĆ©e prĆŖte Ć l'emploi est avantageusement de 8 Ć 11, de prĆ©fĆ©rence de 8,5 Ć 9,5, plus prĆ©fĆ©rentiellement de 8,8 Ć 9,2 et plus prĆ©fĆ©rentiellement encore d'environ 9. Pour la dĆ©termination du pH de la composition diluĆ©e, de l'eau adoucie est utilisĆ©e (degrĆ© de duretĆ© d'environ 5Ā°f). In the use according to the invention, the detergent composition is implemented in a washer disinfector (LD) such as an instrument washer-disinfector (LDI) or an endoscope washer-disinfector (LDE). The term "washer-disinfector" is to be understood as defined in ISO 15883-1: 2006, namely a machine for cleaning and disinfecting medical devices and all other articles used in the medical, dental, pharmaceutical and veterinary. Also, the term "surgical and / or medical instruments" as used in the present application is to be broadly understood as referring to medical devices and all other articles used in the medical, dental, pharmaceutical and veterinary environments requiring cleaning. with aqueous detergents before reuse. In the present invention, this cleaning is advantageously carried out at a temperature of 20 to 60 Ā° C, preferably 45 to 55 Ā° C, more preferably 50 to 55 Ā° C. The cleaning time is advantageously between 20 s and 10 min, preferably between 30 s and 5 min. The present invention also relates to the concentrated aqueous detergent composition implemented in the use according to the invention as described above. This composition is to be diluted with water, preferably softened, demineralized or osmosis, before use. The dilution is generally from 0.03% to 1% (v / v), preferably from 0.1% to 0.6% (v / v), more preferably from 0.2 to 0.4% (v / v). . The pH of the diluted ready-to-use composition is advantageously from 8 to 11, preferably from 8.5 to 9.5, more preferably from 8.8 to 9.2, and even more preferably from about 9. determination of the pH of the diluted composition, softened water is used (degree of hardness about 5 Ā° f).
L'invention sera maintenant dĆ©crite Ć l'aide d'exemples non limitatifs de rĆ©alisation de l'invention. The invention will now be described using non-limiting examples of embodiment of the invention.
FIGURES FIGURES
Figure 1 : Photos des tests de dƩtergence embarquƩ pour les compositions Cl, C2 et C3. Figure 1: Photos of the onboard detergency tests for compositions C1, C2 and C3.
Figure 2 : Evaluation de l'activitĆ© de la subtilisine par Ć©lectrophorĆØse sur gel. Figure 2: Evaluation of the activity of subtilisin by gel electrophoresis.
Figure 3 : Evaluation de l'activitƩ de la lipase par chromato graphie sur couche mince. Figure 3: Evaluation of lipase activity by chromato graphy on thin layer.
Figure 4 : Evaluation de l'activitƩ de l'amylase par chromatographie sur couche mince. Figure 4: Evaluation of the activity of amylase by thin layer chromatography.
EXEMPLES EXAMPLES
Les trois compositions dĆ©tergentes concentrĆ©es suivantes (tableau 1) ont Ć©tĆ© Ć©valuĆ©es pour leur capacitĆ© Ć nettoyer efficacement des rĆ©sidus typiquement retrouvĆ© sur des instruments chirurgicaux et mĆ©dicaux.
Tableau 1 The following three concentrated detergent compositions (Table 1) were evaluated for their ability to effectively clean up residues typically found on surgical and medical instruments. Table 1
EXEMPLE 1 : Essais de dƩtergence embarquƩs en laveur dƩsinfecteur MIELE G7836CD EXAMPLE 1: On-board detergency tests in a MIELE G7836CD washer-disinfector
1 ) DĆ©roulement du cycle - Injection du dĆ©tergent Ć 35Ā°C, dilution de 0,3% (v/v) en eau adoucie1) Cycle sequence - Detergent injection at 35 Ā° C, dilution of 0.3% (v / v) in softened water
Lavage avec de l'eau adoucie pendant 3mn Ć 55Ā°C Wash with softened water for 3 minutes at 55 Ā° C
RinƧage avec de l'eau de rĆ©seau froide Ā Rinsing with cold network water
SĆ©chage Ā Drying
2 ) Les diffƩrents tests embarquƩs utilisƩs 2) The different onboard tests used
Simicon (SIMICON PET-K-10 de SIMICON GmbH, Munich,
Allemagne) Simicon (SIMICON PET-K-10 from SIMICON GmbH, Munich, Germany)
Wash check H (Getinge, Sweden) Ā Wash check H (Getinge, Sweden)
- Load Check Browne (Steris, USA) Ā - Load Check Browne (Steris, USA)
Les diffƩrents tests ont ƩtƩ utilisƩs selon les modes d'emplois fournit par le fabricant respectif. The different tests were used according to the instructions provided by the respective manufacturer.
3) RĆ©sultats des essais 3) Test results
Les essais de performance ont montrĆ© que les trois compositions Cl, C2 et C3 donnent des rĆ©sultats tout Ć fait satisfaisants dans les conditions de tests. Les meilleurs rĆ©sultats sont toutefois obtenus avec la composition Cl . Avec cette composition, on ne dĆ©tecte en effet aucune trace sur les trois tests utilisĆ©s (Figure 1). The performance tests showed that the three compositions Cl, C2 and C3 give quite satisfactory results under the test conditions. The best results, however, are obtained with the composition Cl. With this composition, no trace is detected on the three tests used (Figure 1).
Les essais ont Ć©tĆ© rĆ©pĆ©tĆ©s Ć une tempĆ©rature de nettoyage de 40Ā°C et une dilution des compositions Ć 0,5 % (v/v). Les rĆ©sultats obtenus sont comparables Ć ceux obtenus Ć 40Ā°C et confirment donc l'efficacitĆ© des compositions selon l'invention. The tests were repeated at a cleaning temperature of 40 Ā° C. and a dilution of the compositions at 0.5% (v / v). The results obtained are comparable to those obtained at 40 Ā° C and thus confirm the effectiveness of the compositions according to the invention.
EXEMPLE 2 : Essais de dƩtergence comparatifs en laveur dƩsinfecteur MIELE PG 8528 EXAMPLE 2 Comparative Detergent Tests in MIELE PG 8528 Washer Disinfector
La performance de la composition Cl a Ć©tĆ© comparĆ©e Ć celle de l'Anisoyme Ā® DLM Maxi (Laboratoires Anios, Hellemmes, France), un dĆ©tergent trienzymatique contenant une protĆ©ase, une lipase, une amylase et l'agent chĆ©latant EDTA. Le test embarquĆ© utilisĆ© Ć©tait le TOSI AMCOR (rĆ©fĆ©rence 35002577). The performance of the composition Cl was compared to that of AnisoymeĀ® DLM Maxi (Anios Laboratories, Hellemmes, France), a tri-enzyme detergent containing a protease, a lipase, an amylase and the EDTA chelating agent. The embedded test used was the TOSI AMCOR (reference 35002577).
Pour chaque essai, le cycle de traitement se dƩroule comme suit : For each test, the treatment cycle is as follows:
PrƩlavage : eau de rƩseau froide, 1 min, Prewash: cold network water, 1 min,
- Lavage : eau adoucie (5Ā°f), 5 min, tempĆ©rature et dosage selon tableauĀ - Wash: softened water (5 Ā° f), 5 min, temperature and dosage according to table
2 ci-dessous, 2 below,
RinƧage : eau de rĆ©seau froide, 1 min, Ā Rinsing: cold network water, 1 min,
RinƧage final : eau osmosĆ©e Ć 90Ā°C, 1 min avec de Anios RDA Ć 0,05 % (v/v).
Le tableau 2 ci-dessous rĆ©capitule les conditions d'essais rĆ©sultats. Final rinse: water osmosis at 90 Ā° C, 1 min with Anios RDA at 0.05% (v / v). Table 2 below summarizes the results test conditions.
Tableau 2 Ā Table 2
Ces essais montrent que la composition selon l'invention permet un nettoyage plus efficace Ć des tempĆ©ratures et dosage faibles. Ceci est d'autant plus surprenant que l'activitĆ© chĆ©latant de l'EDTA est Ć la base supĆ©rieure Ć celle du MGDA ce qui laisserait attendre une efficacitĆ© de nettoyage supĆ©rieure pour Ī AniosymeĀ® DLM Maxi. These tests show that the composition according to the invention allows a more efficient cleaning at low temperatures and dosage. This is all the more surprising since the chelating activity of EDTA is higher than that of MGDA, which would allow a higher cleaning efficiency for Ī AniosymeĀ® DLM Maxi.
EXEMPLE 3 : Evaluation de l'activitƩ des enzymes dans la composition Cl EXAMPLE 3 Evaluation of the Activity of Enzymes in the Cl Composition
Les stabilitƩs respectives de la subtilisine, de la lipase et de l'amylase dans la composition Cl ont ƩtƩ ƩvaluƩes par les tests suivants. The respective stabilities of subtilisin, lipase and amylase in the composition C1 were evaluated by the following tests.
1 ) ActivitƩ de la subtilisine 1) Activity of subtilisin
L'activitĆ© de la subtilisine contenue dans le dĆ©tergent est suivie par la technique de l'Ć©lectrophorĆØse sur gel de polyacrylamide, le substrat utilisĆ© est une solution de sĆ©rum albumine humaine Ć 0,3% (salissure reprĆ©sentative d'une application en Ć©tablissement de santĆ©). The activity of the subtilisin contained in the detergent is followed by the technique of polyacrylamide gel electrophoresis, the substrate used is a solution of 0.3% human serum albumin (soil representative of an application in a health facility ).
AprĆØs migration, les protĆ©ines et peptides sont rĆ©vĆ©lĆ©s par exposition dans une solution colorante au bleu de Coomassie suivie d'une dĆ©coloration. Une rĆ©vĆ©lation au bleu de Coomassie permet de rĆ©vĆ©ler les produits de dĆ©gradation issus de l'hydrolyse du sĆ©rum albumine humaine.
La Figure 2 montre quatre pistes d'Ć©lectrophorĆØse : la piste 1 correspond au tĆ©moin (sĆ©rum albumine humaine (0,3%) non dĆ©gradĆ©), les pistes 2, 3 et 4 Ć la composition Cl aprĆØs fabrication, 3 semaines de stockage dans un contenant hermĆ©tiquement fermĆ© Ć 30Ā°C et 7 semaine de stockage dans un contenant hermĆ©tiquement fermĆ© Ć 30Ā°C respectivement. On constate que l'activitĆ© enzymatique de la subtilisine ne se dĆ©grade pas pendant au moins 7 semaines. After migration, the proteins and peptides are revealed by exposure in a Coomassie blue staining solution followed by decolorization. A revelation with Coomassie blue reveals the degradation products resulting from the hydrolysis of human serum albumin. FIG. 2 shows four electrophoresis tracks: lane 1 corresponds to the control (human serum albumin (0.3%), non-degraded), lanes 2, 3 and 4 to the composition Cl after manufacture, 3 weeks of storage in a container tightly closed at 30 Ā° C and 7 weeks storage in a tightly closed container at 30 Ā° C respectively. It is found that the enzymatic activity of subtilisin does not degrade for at least 7 weeks.
2 ) ActivitƩ de la lipase 2) Lipase activity
L'activitƩ de la lipase a ƩtƩ suivie par la technique de Chromatographie sur Couche Mince (CCM), le substrat utilisƩ est un triglycƩride et l'Ʃluant un mƩlange de 50 mL d'heptane, de 20 mL d'Ʃther diƩthylique, de 0,5 mL d'acide acƩtique et de 1.5mL d'Ʃthanol. The lipase activity was followed by the Thin Layer Chromatography (TLC) technique, the substrate used is a triglyceride and the eluent a mixture of 50 ml of heptane, 20 ml of diethyl ether, 0 5 mL of acetic acid and 1.5 mL of ethanol.
La lipase dƩgradant les triglycƩrides, l'absence de triglycƩrides, et la prƩsence de diglycƩrides et de monglycƩrides met en Ʃvidence l'activitƩ enzymatique de la lipase. Triglyceride-degrading lipase, the absence of triglycerides, and the presence of diglycerides and monglycerides demonstrate the enzymatic activity of lipase.
La Figure 3 montre six pistes de CCM : les pistes 1 , 2, 3 correspondent aux tĆ©moins (1 : triglycĆ©rides, 2 : diglycĆ©rides, 3 : monoglycĆ©rides), les pistes 4, 5 et 6 Ć la composition Cl aprĆØs fabrication, aprĆØs 3 semaines de stockage dans un contenant hermĆ©tiquement fermĆ© Ć 30Ā°C et aprĆØs 7 semaine de stockage dans un contenant hermĆ©tiquement fermĆ© Ć 30Ā°C respectivement. On constate que l'activitĆ© enzymatique de la lipase ne se dĆ©grade pas pendant au moins 7 semaines. Figure 3 shows six TLC tracks: lanes 1, 2, 3 correspond to controls (1: triglycerides, 2: diglycerides, 3: monoglycerides), lanes 4, 5 and 6 to composition Cl after manufacture, after 3 weeks storage in a tightly closed container at 30 Ā° C and after 7 weeks of storage in a tightly closed container at 30 Ā° C respectively. It is found that the enzymatic activity of the lipase does not degrade for at least 7 weeks.
3) ActivitƩ de l 'amylase 3) Activity of amylase
L'activitĆ© de amylase a Ć©tĆ© suivie par la technique de Chromatographie sur Couche Mince (CCM), le substrat utilisĆ© est du glycogĆØne et l'Ć©luant un mĆ©lange de 70 mL d'Ć©thanol, de 1 mL d'acide acĆ©tique et de 29 mL d'eau dĆ©minĆ©ralisĆ©e. The amylase activity was followed by the Thin Layer Chromatography (TLC) technique, the substrate used is glycogen and the eluent a mixture of 70 mL of ethanol, 1 mL of acetic acid and 29 mL of demineralised water.
L' amylase dĆ©gradant le glycogĆØne, l'absence de glycogĆØne et la prĆ©sence de glucose mettent en Ć©vidence l'activitĆ© enzymatique de amylase.
La Figure 4 montre cinq pistes de CCM : les pistes 1 et 2 correspondent aux tĆ©moins (1 : glycogĆØne, 2 : glucose), les pistes 3, 4 et 5 Ć la composition Cl aprĆØs fabrication, aprĆØs 3 semaines de stockage dans un contenant hermĆ©tiquement fermĆ© Ć 30Ā°C et aprĆØs 7 semaine de stockage dans un contenant hermĆ©tiquement fermĆ© Ć 30Ā°C respectivement. On constate que l'activitĆ© enzymatique de l'amylase ne se dĆ©grade pas pendant au moins 7 semaines. The glycogen degrading amylase, the absence of glycogen and the presence of glucose demonstrate the enzymatic activity of amylase. FIG. 4 shows five TLC tracks: lanes 1 and 2 correspond to the controls (1: glycogen, 2: glucose), lanes 3, 4 and 5 to the Cl composition after manufacture, after 3 weeks of storage in a hermetically sealed container closed at 30 Ā° C and after 7 weeks of storage in a tightly closed container at 30 Ā° C respectively. It is found that the enzymatic activity of the amylase does not degrade for at least 7 weeks.
EXEMPLE 4 : Influence des enzymes sur le pouvoir nettoyant dƩgraissant EXAMPLE 4 Influence of Enzymes on the Degreasing Cleansing Power
L'influence de la prĆ©sence des trois enzymes subtilisine, lipase et amylase dans la composition dĆ©tergente a Ć©tĆ© Ć©valuĆ©e en comparant la composition Cl Ć des compositions sans enzymes (C4), avec subtilisine (C5) et avec lipase et amylase (C6). The influence of the presence of the three subtilisin, lipase and amylase enzymes in the detergent composition was evaluated by comparing the composition C1 to compositions without enzymes (C4), with subtilisin (C5) and with lipase and amylase (C6).
Pour ces essais le pouvoir nettoyant dĆ©graissant des diffĆ©rentes compositions a Ć©tĆ© Ć©valuĆ© par rapport Ć de la salissure anglaise selon la norme ISO 15883 qui a Ć©tĆ© appliquĆ©e au pinceau sur des lames en inox (une lame par composition testĆ©e) et laissĆ©e sĆ©cher pendant une heure Ć tempĆ©rature ambiante. Ensuite chaque lame a Ć©tĆ© trempĆ©e sous agitation (agitateur tridimensionnel, 50
rpm) pendant 15 min Ć tempĆ©rature ambiante dans l'une des quatre compositions dĆ©tergente diluĆ©e Ć 0,3 % (v/v) dans de l'eau adoucie (5Ā°f). For these tests, the degreasing cleansing power of the various compositions was evaluated with respect to English soil according to the ISO 15883 standard which was applied by brush on stainless steel blades (one blade per composition tested) and allowed to dry for one hour at ambient temperature. Then each slide was quenched with stirring (three-dimensional stirrer, 50 rpm) for 15 min at room temperature in one of the four detergent compositions diluted to 0.3% (v / v) in softened water (5%).
Les meilleurs rĆ©sultats ont Ć©tĆ© obtenus pour la composition Cl. Les lames traitĆ©es avec les compositions C4, C5 et C6 prĆ©sentaient en effet d'importants rĆ©sidus de salissure anglaise visible Ć l'Åil nu. Le dosage des protĆ©ines rĆ©siduelles par la technique MicroBCA (kit INTERCHIM UPTIMA MicroBC Assay, rĆ©fĆ©rence UP75860A) confirme ces observations.
The best results were obtained for the composition Cl. The slides treated with the compositions C4, C5 and C6 indeed had significant residues of English soil visible to the naked eye. Residual protein assay using the MicroBCA technique (INTERCHIM UPTIMA MicroBC Assay kit, UP75860A reference) confirms these observations.
Claims
1. Utilisation d'une composition dƩtergente aqueuse concentrƩe pour le nettoyage d'instruments chirurgicaux et/ou mƩdicaux en laveur dƩsinfecteur, ladite composition dƩtergente aqueuse concentrƩe comprenant : - une subtilisine, 1. Use of a concentrated aqueous detergent composition for cleaning surgical and / or medical instruments in a washer disinfector, said concentrated aqueous detergent composition comprising: - a subtilisin,
une lipase, Ā a lipase,
une amylase, Ā an amylase,
un agent chĆ©latant biodĆ©gradable choisi parmi l'acide mĆ©thylglycine diacĆ©tique et un iminodisuccinate et Ā a biodegradable chelating agent selected from methylglycine diacetic acid and an iminodisuccinate and
- de l'eau, ladite composition dĆ©tergente concentrĆ©e Ć©tant exempte d'alcanolamine. Ā water, said concentrated detergent composition being free of alkanolamine.
2. Utilisation selon la revendication 1, caractĆ©risĆ©e en ce que la composition dĆ©tergente a une teneur en subtilisine de 0,5 Ć 15% en poids par rapport au poids total de la composition. 2. Use according to claim 1, characterized in that the detergent composition has a subtilisin content of 0.5 to 15% by weight relative to the total weight of the composition.
3. Utilisation selon la revendication 1 ou 2, caractĆ©risĆ©e en ce que la composition dĆ©tergente a une teneur en lipase de 0,05 Ć 2% en poids par rapport au poids total de la composition. 3. Use according to claim 1 or 2, characterized in that the detergent composition has a lipase content of 0.05 to 2% by weight relative to the total weight of the composition.
4. Utilisation selon l'une quelconque des revendications prĆ©cĆ©dentes, caractĆ©risĆ©e en ce que la composition dĆ©tergente a une teneur en amylase de 0,05 Ć 2% en poids par rapport au poids total de la composition. 4. Use according to any one of the preceding claims, characterized in that the detergent composition has an amylase content of 0.05 to 2% by weight relative to the total weight of the composition.
5. Utilisation selon l'une quelconque des revendications prƩcƩdentes, caractƩrisƩe en ce que l'agent chƩlatant biodƩgradable est de l'acide mƩthylglycine diacƩtique. 5. Use according to any one of the preceding claims, characterized in that the biodegradable chelating agent is methylglycine diacetic acid.
6. Utilisation selon l'une quelconque des revendications prĆ©cĆ©dentes, caractĆ©risĆ©e en ce que la composition dĆ©tergente a une teneur en agent chĆ©latant biodĆ©gradable de 10 Ć 50% en poids par rapport au poids total de
la composition. 6. Use according to any one of the preceding claims, characterized in that the detergent composition has a content of biodegradable chelating agent of 10 to 50% by weight relative to the total weight of the composition.
7. Utilisation selon l'une quelconque des revendications prƩcƩdentes, caractƩrisƩe en ce que la composition dƩtergente comprend Ʃgalement de la glycƩrine. 7. Use according to any one of the preceding claims, characterized in that the detergent composition also comprises glycerine.
8. Utilisation selon l'une quelconque des revendications prƩcƩdentes, caractƩrisƩe en ce que la composition dƩtergente comprend Ʃgalement un ou plusieurs tensioactifs non ioniques. 8. Use according to any one of the preceding claims, characterized in that the detergent composition also comprises one or more nonionic surfactants.
9. Utilisation selon l'une quelconque des revendications prĆ©cĆ©dentes, caractĆ©risĆ©e en ce que le nettoyage est effectuĆ© Ć une tempĆ©rature de 20 Ć 60 Ā°C. 9. Use according to any one of the preceding claims, characterized in that the cleaning is carried out at a temperature of 20 to 60 Ā° C.
10. Utilisation selon l'une quelconque des revendications prƩcƩdentes, caractƩrisƩe en ce que la durƩe de nettoyage comprise entre 20 s et 10 min. 10. Use according to any one of the preceding claims, characterized in that the cleaning time between 20 s and 10 min.
11. Composition dƩtergente aqueuse concentrƩe comprenant : - une subtilisine, A concentrated aqueous detergent composition comprising: - a subtilisin,
une lipase, Ā a lipase,
une amylase, Ā an amylase,
un agent chĆ©latant biodĆ©gradable choisi parmi l'acide mĆ©thylglycine diacĆ©tique et un iminodisuccinate et Ā a biodegradable chelating agent selected from methylglycine diacetic acid and an iminodisuccinate and
- de l'eau, ladite composition dĆ©tergente concentrĆ©e Ć©tant exempte d'alcanolamine. Ā water, said concentrated detergent composition being free of alkanolamine.
12. Composition dĆ©tergente selon la revendication 11, caractĆ©risĆ©e en ce qu'elle a une teneur en subtilisine de 0,5 Ć 15% en poids par rapport au poids total de la composition. 12. Detergent composition according to claim 11, characterized in that it has a subtilisin content of 0.5 to 15% by weight relative to the total weight of the composition.
13. Composition dƩtergente selon la revendication 1 1 ou 12,
caractĆ©risĆ©e en ce qu'elle a une teneur en lipase de 0,05 Ć 2% en poids par rapport au poids total de la composition. 13. Detergent composition according to claim 1 1 or 12, characterized in that it has a lipase content of 0.05 to 2% by weight relative to the total weight of the composition.
14. Composition dĆ©tergente selon l'une quelconque des revendications 11 Ć 13, caractĆ©risĆ©e en ce qu'elle a une teneur en amylase de 0,05 Ć 2% en poids par rapport au poids total de la composition. 14. Detergent composition according to any one of claims 11 to 13, characterized in that it has an amylase content of 0.05 to 2% by weight relative to the total weight of the composition.
15. Composition dĆ©tergente selon l'une quelconque des revendications 11 Ć 14, caractĆ©risĆ©e en ce que l'agent chĆ©latant biodĆ©gradable est de l'acide mĆ©thylglycine diacĆ©tique. 15. Detergent composition according to any one of claims 11 to 14, characterized in that the biodegradable chelating agent is methylglycine diacetic acid.
16. Composition dĆ©tergente selon l'une quelconque des revendications 11 Ć 15, caractĆ©risĆ©e en ce qu'elle a une teneur en agent chĆ©latant biodĆ©gradable de 10 Ć 50% en poids par rapport au poids total de la composition. 16. Detergent composition according to any one of claims 11 to 15, characterized in that it has a content of biodegradable chelating agent of 10 to 50% by weight relative to the total weight of the composition.
17. Composition dĆ©tergente selon l'une quelconque des revendications 11 Ć 16, caractĆ©risĆ©e en ce qu'elle comprend Ć©galement de la glycĆ©rine. 17. Detergent composition according to any one of claims 11 to 16, characterized in that it also comprises glycerin.
18. Composition dĆ©tergente selon l'une quelconque des revendications 11 Ć 17, caractĆ©risĆ©e en ce qu'elle comprend Ć©galement un ou plusieurs tensioactifs non ioniques.
18. Detergent composition according to any one of claims 11 to 17, characterized in that it also comprises one or more nonionic surfactants.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL17716972T PL3433349T3 (en) | 2016-03-23 | 2017-03-23 | Enzymatic detergent compositions for the automatic cleaning of surgical and/or medical instruments and/or devices |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR1652498A FR3049285B1 (en) | 2016-03-23 | 2016-03-23 | DETERGENT ENZYMATIC COMPOSITIONS FOR THE AUTOMATIC CLEANING OF SURGICAL AND / OR MEDICAL INSTRUMENTS AND / OR DEVICES. |
| PCT/FR2017/050684 WO2017162991A1 (en) | 2016-03-23 | 2017-03-23 | Enzymatic detergent compositions for the automatic cleaning of surgical and/or medical instruments and/or devices |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP3433349A1 true EP3433349A1 (en) | 2019-01-30 |
| EP3433349B1 EP3433349B1 (en) | 2020-04-22 |
Family
ID=56263860
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP17716972.9A Active EP3433349B1 (en) | 2016-03-23 | 2017-03-23 | Enzymatic detergent compositions for the automatic cleaning of surgical and/or medical instruments and/or devices |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP3433349B1 (en) |
| FR (1) | FR3049285B1 (en) |
| PL (1) | PL3433349T3 (en) |
| WO (1) | WO2017162991A1 (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2741355B1 (en) * | 1995-11-17 | 1998-12-31 | Anios Lab Sarl | COMPOSITION FOR THE TREATMENT OF OBJECTS TO BE CLEANED AND / OR DISINFECTED |
| US7491362B1 (en) * | 2008-01-28 | 2009-02-17 | Ecolab Inc. | Multiple enzyme cleaner for surgical instruments and endoscopes |
| US7723281B1 (en) * | 2009-01-20 | 2010-05-25 | Ecolab Inc. | Stable aqueous antimicrobial enzyme compositions comprising a tertiary amine antimicrobial |
| FR2980955B1 (en) * | 2011-10-05 | 2014-12-12 | Anios Lab Sarl | DISINFECTANT AND DETERGENT COMPOSITIONS. |
-
2016
- 2016-03-23 FR FR1652498A patent/FR3049285B1/en active Active
-
2017
- 2017-03-23 PL PL17716972T patent/PL3433349T3/en unknown
- 2017-03-23 WO PCT/FR2017/050684 patent/WO2017162991A1/en active Application Filing
- 2017-03-23 EP EP17716972.9A patent/EP3433349B1/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| WO2017162991A1 (en) | 2017-09-28 |
| FR3049285A1 (en) | 2017-09-29 |
| PL3433349T3 (en) | 2020-10-19 |
| WO2017162991A9 (en) | 2018-10-11 |
| FR3049285B1 (en) | 2018-04-13 |
| EP3433349B1 (en) | 2020-04-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2250246B1 (en) | Multiple enzyme cleaner for surgical instruments and endoscopes | |
| KR100978822B1 (en) | Anticorrosive detergent compositions and their use in cleaning dental and medical devices | |
| JP5407002B2 (en) | Cleaning composition for medical instrument washer | |
| RU2642077C2 (en) | Multi-purpose enzyme detergent and methods of stabilizing applicable solution | |
| EP2526190A2 (en) | Low and high temperature enzymatic system | |
| EP1987125B1 (en) | Liquid detergent composition containing an enzyme | |
| JP6732454B2 (en) | Cleaning disinfectant composition | |
| KR102001696B1 (en) | Liquid cleaning compositions with improved enzyme compatibility and/or stability | |
| CA2231460C (en) | An anionic stabilized enzyme-based clean-in-place system | |
| EP2588420B1 (en) | Descaling of oxalates with acid compositions | |
| CN105907483A (en) | Oxygen-containing multifunctional detergent composition | |
| JP2001501244A (en) | Surface cleaner | |
| KR101900978B1 (en) | Liquid cleaning agent composition | |
| JP7315948B2 (en) | Disinfectant detergent composition | |
| JP2009019130A (en) | Detergent composition and deterging method of dishes using the same | |
| TW201925444A (en) | Surface cleaner and disinfectant composition | |
| EP3924455B1 (en) | High foaming liquid alkaline cleaner concentrate composition | |
| EP3433349B1 (en) | Enzymatic detergent compositions for the automatic cleaning of surgical and/or medical instruments and/or devices | |
| BE1027322B1 (en) | Cleaning and degreasing composition for the treatment of hard surfaces | |
| JPH11302693A (en) | Concentrated detergent composition | |
| CN110546248A (en) | Formulations and methods for cryogenic cleaning of dairy equipment | |
| BE1025146B1 (en) | Composition comprising an enzymatic component and a detergent component | |
| TWI686470B (en) | Moist detergent wipe, use of the moist detergent wipe, and method for cleaning and/or disinfecting an object with a hard surface | |
| WO2022270458A1 (en) | Dish washing method | |
| CN116490596A (en) | Liquid detergent concentrate, ready-to-use application solution, application and cleaning method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: UNKNOWN |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE INTERNATIONAL PUBLICATION HAS BEEN MADE |
|
| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: REQUEST FOR EXAMINATION WAS MADE |
|
| 17P | Request for examination filed |
Effective date: 20180924 |
|
| AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
| AX | Request for extension of the european patent |
Extension state: BA ME |
|
| DAV | Request for validation of the european patent (deleted) | ||
| DAX | Request for extension of the european patent (deleted) | ||
| GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: GRANT OF PATENT IS INTENDED |
|
| INTG | Intention to grant announced |
Effective date: 20191127 |
|
| GRAS | Grant fee paid |
Free format text: ORIGINAL CODE: EPIDOSNIGR3 |
|
| GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE PATENT HAS BEEN GRANTED |
|
| AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
| REG | Reference to a national code |
Ref country code: CH Ref legal event code: EP |
|
| REG | Reference to a national code |
Ref country code: IE Ref legal event code: FG4D Free format text: LANGUAGE OF EP DOCUMENT: FRENCH |
|
| REG | Reference to a national code |
Ref country code: DE Ref legal event code: R096 Ref document number: 602017015228 Country of ref document: DE |
|
| REG | Reference to a national code |
Ref country code: AT Ref legal event code: REF Ref document number: 1260072 Country of ref document: AT Kind code of ref document: T Effective date: 20200515 |
|
| REG | Reference to a national code |
Ref country code: LT Ref legal event code: MG4D |
|
| REG | Reference to a national code |
Ref country code: NL Ref legal event code: MP Effective date: 20200422 |
|
| REG | Reference to a national code |
Ref country code: DE Ref legal event code: R082 Ref document number: 602017015228 Country of ref document: DE Representative=s name: GODEMEYER BLUM LENZE PATENTANWAELTE, PARTNERSC, DE |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IS Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200822 Ref country code: NO Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200722 Ref country code: GR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200723 Ref country code: FI Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 Ref country code: SE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 Ref country code: NL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 Ref country code: PT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200824 Ref country code: LT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 |
|
| REG | Reference to a national code |
Ref country code: AT Ref legal event code: MK05 Ref document number: 1260072 Country of ref document: AT Kind code of ref document: T Effective date: 20200422 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: BG Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200722 Ref country code: RS Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 Ref country code: LV Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 Ref country code: HR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: AL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 |
|
| REG | Reference to a national code |
Ref country code: DE Ref legal event code: R097 Ref document number: 602017015228 Country of ref document: DE |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: AT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 Ref country code: SM Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 Ref country code: EE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 Ref country code: DK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 Ref country code: RO Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 Ref country code: CZ Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 Ref country code: ES Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 |
|
| PLBE | No opposition filed within time limit |
Free format text: ORIGINAL CODE: 0009261 |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT |
|
| 26N | No opposition filed |
Effective date: 20210125 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SI Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MC Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 |
|
| REG | Reference to a national code |
Ref country code: CH Ref legal event code: PL |
|
| REG | Reference to a national code |
Ref country code: BE Ref legal event code: MM Effective date: 20210331 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210323 Ref country code: LI Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210331 Ref country code: LU Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210323 Ref country code: CH Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210331 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: BE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210331 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: CY Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: HU Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO Effective date: 20170323 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 |
|
| PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: DE Payment date: 20231229 Year of fee payment: 8 Ref country code: GB Payment date: 20240108 Year of fee payment: 8 |
|
| PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: PL Payment date: 20240119 Year of fee payment: 8 Ref country code: IT Payment date: 20240212 Year of fee payment: 8 Ref country code: FR Payment date: 20240103 Year of fee payment: 8 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: TR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20200422 |