DE2044534A1 - Oral care products - Google Patents

Description

Colgate-Palmolive Company (US 864 2i2 - prio 6 «10 _o 69

New York, NY ,, V.3t.A. 7218)

$ Park Avenue Hamburg, September 8, 1970

Oral care medium

In recent years, dental and oral hygiene have received increasing attention ₉ and great advances have been made in this area. However, the processes associated with oral hygiene and tooth decay are numerous and complex. There is therefore still an increasing need for dentifrices and oral care products which bring these processes under control or curb Formation of dental plaque, which is a precursor to caries and tartar formation .

Various ways are known for removing plaque from teeth. Among other things, have already been Enzymes like pepsin, amylopepsin, trypsin, and steapsin to aid in the removal of food residues from

109816/2082

₉ 20 * 4534

The teeth are used, however, these love themselves as unwilling to prevent the formation of "n Zonabalag arwiesen" Ea other Snayrao wIb for example the enzymes formed from the microorganisms Aspergilius oryzae and Aepergillue niger were used; " however, they did not show a satisfactory effect in preventing plaque formation

Dental care products with a content of proteolytiachen Enzymes have been developed to catalyze the breakdown of the organic matrix in which dental plaque develops. However, these dentifrices containing proteolytic enzymes are quite inconsistent and its enzymatic action decreases rapidly abο In addition, the enzymes only have a low level Degree of activity and must therefore be in high concentrations and are used relatively frequently during the day ο For this Basically, they are not very suitable for use in normal oral and dental care products »

The present invention is therefore the object based on proposing new enzyme-containing products that improve oral hygiene and have ο a prophylactic effect on the formation of ZaIinbolag » Furthermore, aollen products are proposed which

1098 16/2082 '" ^tL

- j "'

the formation of dental plaque with the usual methods of Prevent oral and dental care. Another object of the invention is to produce inhibiting products without To propose content of protease, which are effective in the removal of dental plaque, but do not damage the flag surfaces, tissue proteins and secretions of the salivary glands «Furthermore, the use should suggested by enzymes for mind hygiene, which are available from more than one source. Finally, oral hygiene products are designed to help prevent the Formation of dental plaque in the form of mouthwashes, toothpastes, tooth tablets, chewing gum and the like to be proposed «

These objects are achieved according to the invention by oral care products which contain an effective amount of invertase an activity of at least about 2000 activity units per mg of nitrogen contained '

The invertase is used in the oral care products according to the invention in an effective amount of at least about 0.05% to about 0.5%. Effective invert preparations have an activity of at least 2000 units of activity per mg nitrogen; for reasons of expediency, however, in general up to

BAD ORiGiNAL

109816/2082

2U4A53A

to about 6000 activity units per mg nitrogen « Preferably the activity is about 4006 activity units per mg nitrogen.

Invertase can be obtained from various sources with a degree of activity sufficient for the use according to the invention

So invertase aue baker's yeast can be obtained in the following wayc (If further information is desired, this can be found in the work "Purification de I ¹ invertase de lavure ^w by EoHo Pieeher and L ₀ Kohtea in Helvetia Chimica Acta, 34, 3o1i23 (151}) _o ) The yeast cells are plasmolyeierty in toluene at a pH value of 5 _S O bie 7 »5 with autolysis of the cells and release of the invertase takes place. 35 parts by volume of picric acid per part by volume of acidified crude extract. The slurry is centrifuged and the precipitate discarded

109816/2082

is then dialyzed against cold water. The dialyzed solution is mixed with alurainium hydroxide of pH 6.0 in an amount of about 1 ng per 12 to 36 activity units of the dialyserfcen solution. The analysis is then carried out for the absorption of the invertase on the Al (OH) for 3 minutes allowed to ^{stand at 0} ° C. and the slurry then centrifuged for 3 minutes. The above liquid is discarded. The precipitate is suspended in as little water as possible by shaking in a vibromixer, and the slurry is mixed with a 4N ammonium lactate / lactic acid buffer system Amount of 5 ml of buffer per g of Al (OH), adjusted to a pH of 2.9. The slurry is then centrifuged and the supernatant liquid decanted and adjusted to pH 4.8 (the precipitate is discarded). The invertase is precipitated with 3 * 5 parts by volume of Aoeton per part by volume of decanted liquid. λ The precipitate is suspended again in water and checked for its activity. The invertase is purified further by adding Al (OH) again, as above, and repeating all the subsequent steps described above.

The activity of the invertase is determined according to the colorimetric Method determined by Sumner using Dinltroealicylic acid to measure the reducing zuoker

109816/2082

2Ü44534

(see JeBo S-umner and 3 "F" Howell, Journal of Biological Chemistry, 108, 3 "51 (1935)). Dia activity of invertase is expressed in units indicating the amount of enzymes which I mg reducing Sucker in 3 Hinuten at 2O ⁰ G and a pH of 4.8 in a 5 # strength Saccharoeelöaung releases "The described by the above- Invertase produced by the method has an activity of about 4000 activity units per mg of nitrogen; of an invertase with this activity, about 0.05 to 0.5 # are generally incorporated into the oral care products according to the invention.

The enzyme preparation can also be prepared from Aspergillua oryzae in the following way * Roux bottles with 70 to 100 ml of Czapek-Dox-Hährlösung sucrose «0 _f 2 $ NaNO ^, 0.15t K ₂ HPO ₄ , 0 _r Q5 # MgSO 0,055c KPl 0.001 # Pe30..7H ₂ 0) are inoculated with spores ui "S at 30 ⁰ C incubated · Mycelkolonien are in general

Harvested within 8 days of vaccination before active sporulation begins. If spores are needed, the mold will! ? to 3 weeks gesuchtat on a solid medium (as above nutrient solution Jedeoh with the addition of 2 ^ agar) and rinsed the spores with water "- wlrä frozen The material and serkleine in a dry ice cooled face *;

109816/2082

Dae product consists at 2O ⁰ C in a flowable Hasse, which still contains some viable cells, which is reflected in the fact that even a low Wachstun takes place when the material two or three days without CHCl, or toluene kept wiröo The suspension is centrifuged and dialyzed the supernatant liquid for 2 days in the presence of toluene against running tap water in a Visking housing made of synthetic cellulose. Dialysis usually produces a fluffy precipitate; this is filtered off, so that a clear, weakly colored extract is obtained o The extract is filtered with suction, dialyzed as above and filtered a second time «

Invertase is manufactured and traded by numerous companies; an example is that under the name "Invertase ¹¹ from Mann Research Laboratory, New York,

YoSt.A., traded product which is reagent grade ™

and has a K value of 15 according to the AOAC method, which corresponds to about 3200 units of activity per mg of N.

It has been found that invertase has the ability improve oral hygiene and prevent plaque from building up on teeth. The process of Dental plaque formation is not known in detail, so

109816/2082 ^ßAD

ο -

de® the theoretical chartering given below not all are to be regarded as binding. Ee is accepted » that plaque on yawn and dentures through the Formation of dextran-like polysaccharides occurs, which by bacteria from sucrose, etch «a Disaccharides are synthesized * Ba bacteria dieae dextran-like polysaccharides not from glucose and / or fructose, the monosaccharide constituents of sucrose, can produce, the formation of τοη dental plaque can thereby be prevented from turning the sucrose into glucose and fructose broken down once the sucrose is broken down to the monosaccharides, find the Bacteria no longer have a usable soil no more plaque can form "

Se has been found to be incorporated into oral care products Invertase in competition with the polysaccharide-forming ones Microorganisms around the available sucrose occurs. Invertase diminishes due to its hydrolytic conversion of sucrose In glucose and fructose the sucrose available for the bacteria SUT synthesis of dextran and thus prevents the formation of dental plaque both in vitro and on the teeth.

109816/2082

lavertase can be used in all products for the oral and Dental care can be used. These products can contain a wide variety of ingredients in appropriate quantities provided that these ingredients do not adversely affect the desired results

The care products according to the invention normally have a pH of about 5 to 9, and preferably about

6 to 7 β If necessary, the pH value can be determined by a "

Buffer system to be maintained «.

If the carrier material consists of a dentifrice, it contains a practically water-insoluble polishing or Abrasives of the type commonly used in toothpastes, chewable tablets and tooth powders. Such abrasives are, for example, dicalcium phosphate, frioalcium phosphate, insoluble sodium metaphosphate, aluminum hydroxy oil, Magnesium oarloid, calcium carbonate, calcium pyrophosphate, Calcium metaphorate, calcium sulfate, bolyethylene methacrylate, bentonite and the like as well suitable mixtures of the same o It can also be abrasive acting resinous substances such as, for example, the SDdenafitäonprodukte of melamine and urea with Formaldehyde should be used «Preferably al» ; .. '■' - to -

10981β / 20β2 bad original

and unlU8llolies Hatriusmetaphoapliat uBd / or

Bibjteat ¥ © rw @ Nä @ t _o las Soklmlimitt®! term as allaini «

especially if

»© laea @ about 20 to *
& about 70

is pleading crowds "

© rteltea is what

g «as« Aj β

It © isa

11/2 θ I.

^BATH ORIGINAL

To use sorbitol »The total liquid arate makes up generally about 20% 75 # of the carrier» Preferably, the toothpastes are also given a gelling agent such as in natural and synthetic gourams or benign substances, ZoBo Irish moss ₉ fragant, sodium carboxymethyl cellulose, polyvinylpyrrolidone, starch and the like generally present in amounts up to about 10 $, and preferably about 2 to 5 O ₉ $ to the Slower. M.

In other mind care products such as mouthwashes and the like If the carrier consists of an aqueous medium, which makes up about 20 to 99 $ of the total product The carrier usually still contains about $ 5 to $ 30 of a non-toxic alcohol such as Ethanol "

In the carrier of the products according to the invention can also organic surface-active substances are used, which ensure thorough and complete distribution of the Support agent according to the invention in .der oral cavity and make the product more cosmetically attractive o This organic surface-active substances can be of an anionic or nonionic naturej preferably used one as a surface-active substance a ^ ensid, which

- 12 -

109816/2082

gives the product cleaning and foaming properties. Suitable surfactants of this type are the water-soluble Salt® higher fatty acid monoglyoerid monosulfates, eg _{o the} sodium acid of the monosulfated monoglyceride of hydrogenated goosefatty acids, higher AXky sulfates, alkylarylaulfonates, higher alkyl sulfoacetates, where fatty acid esters of 1 _s 2-dihydroxypropane sulfonate

f | Fatty acid amides of Taurina, higher fatty acid esters of Isethionic acid and the largely saturated higher aliphatic acylamides of lower aliphatic aminocarboxylic acid compounds " for example those with 12 to 16 carbon atoms in the fatty acid, alkyl or Acyl group, and the like «As examples of the last named amides can N-Lauroylsareo & in and the Sodium, potassium and ethanolamine salts of N ~ lauroyl ~, N-myrietoyl and N-palmitoyl sarcosinate are cited,

oil which should be essentially free of soap or similar higher fatty acid compounds, as these considerably impair the effect of the sarcosines and sarcosinates. The use of the sarcoainate compounds in the oral care products according to the invention is particularly advantageous, since these substances inhibit acid formation in the oral cavity by carbohydrates o persistently and noticeably and reduce the solubility of the tooth enamel in acid solutions

- 13 -

109816/2082

20U53A

Other suitable surface-active substances are the nonionogenic compounds such as, for example, the condensate iona product β of sorbitan monostearate with about 60 times ethylene oxide, the propylene glycol condensates ("Pluronics"), the kbndenaate of higher fatty alcohols such as Tridecy alcohol with ethylene oxide, the condensates of Alkylthiophenols with 10 to 15 ethylene oxide units and the ethylene oxide adducts of monoesters aechawertiger Alcohols and internal ethers thereof such as sorbitan monolaurate, Sorbitol monoolelate and mannitane monopalmitate.

The surfactants are preferably used in amounts of about 0.05 to 5 microns of the carrier.

Various other substances can also be incorporated into the carrier, for example coloring or lightening substances, for example titanium dioxide, Kbaservierungs- ä , ε.Β «. Ifodium benzoate, silicones, chlorophyll compounds, ammonium compounds such as urea, dianmonium phosphate and mixtures thereof, saccharine, alcohol, menthol and other ingredients. These additives are used in the products according to the invention in amounts which have practically no negative influence on the changed properties of the same, and their type and amount are selected according to the type of product intended in each case.

- t4 -

109816/2082

May further ββ zweckiaäiig BBIN the support ₉ to add or antibacterial agents, which are usually in ag®n ffi @ from about 0.01 Me 5 # _t be used vorsugsweise about 0.05 to 1.0 $ of the wearer., Suitable means antibakterieile including the bisphenols imä Bisguaalde such as "for example p« chlorophenyltoguanid,

, 4 ~ chlorine> enzhyärylgu & nyl-

ehlor-2-guanidinobenslmidaaol ₉ 5-amino-1 _f 3-bia (2-ethyl) ~ § ~ ia @ thylhe3Eahydropys "iiaidin, 2, ^2% -Dihydrojcy-

estchlorodiphenylmethane »2,2 · -dihydroxy- and their non-toxic

Furthermore ktanen la! Cragv also arona and sweeteners

la fcEäffltgsaittela ttbllöhen Art T © rwesidet be ii © ja @ a teiu _g i © n S® @ eliim © k and ßerußh der ü®t gmMmtQhtQn Hlohtusig au aoöifiaieren »As B © ie ^ iel @ for g @ © l | p® t @ ZisEtzatoffe dieüer Art

■ _s Ιιβκοη · »

Ils SSUfletoff® © Ignen see

109818/2082

and saccharin »The total amount of flavor and sweet == fabric can be about 0.01 "to 2.0 # of the wearer.

Furthermore, the carrier can also contain a fluorine compound which has an advantageous effect on the care and hygiene of the oral cavity, for example by reducing the solubility of the tooth enamel in acid and protecting the teeth against tooth decay. Suitable fluorine compounds include, for example, sodium fluoride, stannous fluoride, potassium fluoride, potassium stannous fluoride (SnFg ■ «, KF) _P sodium hexafluorostannate, stannous chlorofluoride, sodium fluoroconate and sodium monofluorophosphate ο These compounds, which dissociate in water but are effective in releasing fluorine-containing ions non-toxic amount used - generally in the range - about 0.01 Mb % $> ₉ based on water-soluble fluoro

The invention is further illustrated by the following examples explained, but not limited to the same «Unless otherwise noted, all relate to Quantities based on weight.

- 16 -

BAD ORiGINAL

109816/208 2

2 Ü A A 5 3 4

Toothpastes of the following composition were used Improvement of oral hygiene and prevention of 6 formation Hergesteilts from ^ ahnbelagts

Parts

Glycerin carboxymethyl cellulose Irlachmoos Tetrasodium pyrophosphate sodium likewiseate Saccharin water sodium K-lauroylaarcoßinat Dicalcium phosphate calcium carbonate insoluble sodium metaphogate dye Invertase

A. B. C. 25.7 28 _S 5 25.1 0.75 - 1.3 1.3 0.3 - 0.2 0.5 0.2 O ₉ 5 - - 0.2 2O ₉ O 22.0 19.0 1 _S O 1.5 1.0 46.7 15.0 46.7 5.0 - 5 * 0 .at - 30.6 - =. 0.4 - 0.05 0.5 1.0

Example 2

Ss became a mouthwash of the following composition to improve oral hygiene and to prevent plaque formation

- Ί7 -

ORIGINAL

109816/2082

Components ? EijLe

Ethyl alcohol (95 #) 14.8

Sorbitan Monoatearate / Polyoxyäthylon-

Condensate with about 60 moles of ethylene oxide 2.5

Glycerine (99.3 ig) 10.0

Water 71.57

Dye 0.6

Citric acid 0.03

Invertase 0.5

Example 3 There were chewable tablets of the composition Ib ^^ l Improving oral hygiene and preventing education

made of dental plaque}

Components parts Dicalcium phosphate 77.8 Sodium Lauryl Sulphate 0.5 Sodium salt of coconut monoglyceride sulfate

based on hydrogenated coconut oil 1,2

1,6-di-p-chlorophenylbiguanidohexane 0.1 |

Polyethylene Glycol-6000 10.0

Thickness 2.5

Carboxymethyl cellulose 1.25 Silicon dioxide 1.25 Polyvinyl alcohol 2.9

TÄlkum 2.0

Invertase 0.5

As is readily apparent to those skilled in the art, in Modifying the above examples, numerous other products have been made with the advantages of the present invention become ^ 18 -

109816/2082

Claims (1)

2Ü44534 Colgate-Palmolive Company (US 864 212 - prio δο 10.69 New York, N.Yo, YoStoA. 7218) P ate η ta η a P ₁ r tt che Oral care products, characterized in that it an effective amount of invertase having an activity of at least about 2000 activity units per mg Contains nitrogen. 2ο oral care product according to claim 1, characterized in that that it contains an abrasive » 3. Oral care products according to speeches 1 and 2,
characterized in that it is at least about
Oe05 wt. ^ Contains invertaae. 4. Mold care product according to claims 1 Taia 3, characterized in that it contains 0.05 to 0.5 wt. ^ invertase with an activity of about 2000 to
6000 units of activity per mg nitrogen - 19 - 109816/2082 Oral care products according to claims 1 "to 4, characterized in that it is invertase with a Activity of about 4000 units of activity per mg Contains nitrogen. 6 * Oral care product according to claims 1 Ms 5, characterized in that it contains about 20 Ms 75 wt <, # abrasive, the abrasive in one | liquid carrier is suspended and the product represents a toothpaste " ο oral care composition according to claim 6, characterized in that it contains in an amount of about 20 to 75 wt # _e and also about 0.2 to 10 GrQWc ^ a gelling agent, and about 0.05 to 5 Gewo ^ a water soluble organic liquid carrier! © envy contains 8ο oral care product according to claim 7, characterized in that that it as a water-soluble organic surfactant sodium H-lauroyl sarcosinate or liatrium lauryl sulfate contain c jfacapflegeaittel according to claims 6 to 8) characterized by the fact that it is used as an abrasive - 20th 109816/2082 u & ä / o & er insoluble sodium meta * Contains calolumo carbonate 6 bi @ 9 s as 1 09816/2082 15o oral care product according to claim 14, characterized in that it contains about 0.05 to 0.5% by weight of invertase with an activity of about 2000 to 6000 activity units contains per mg nitrogen. 16ο oral care product according to claim 15, characterized in that That it is invertase with an activity of about 4000 activity units per mg of nitrogen contains » 17 »The oral care composition according to claims 13 to 16, characterized 'in that it contains as the alcohol ethanol, the carrier in an amount of about 20 to 99 wt"<f"is present, and the product representing a mouthwash 18o method of improving oral hygiene, thereby characterized in that the oral cavity or the teeth with a care product according to Anapruch 1 bi © 17 treated. 109316/2082