United States Patent 19 | 1 || 3,966,901 Cullum et al. (45) June 29, 1976 54 DENTIFRICE PREPARATION 58 Field of Search................................. 424/49-52 (75 Inventors: Douglas Charles Cullum, East Molesey, Joan Collinge, Cheadle, 56 References Cited both of England UNITED STATES PATENTS 73 Assignee: Colgate-Palmolive Company, New 3,227,617 lf 1966 Manahan et al...................... 424/52 York, N.Y. 3,227,68 lf 1966 Manahan et al...................... 424/52 33 ()8()29 3f 967 Saunders............................... 424 f52 (22 Filed: Feb. 21, 1975 21 Appl. No. 551,870 Primary Examiner-Lewis Gotts Assistant Examiner-Cary Owens Related U.S. Application Data Attorney, Agent, or Firm-Robert L. Stone; Murray 63 Continuation of Ser. No. 389,628, Aug. 21, 1973, abandoned, which is a continuation of Scr. No. M. Grill; Herbert S. Sylvester 21 (),559, Dec. 21, 1971, abandoned. 57 ABSTRACT 30 Foreign Application Priority Data The present invention relates to a dentifrice prepara Dec. 29, 1970 United Kingdom............... 61 6 1 417() tion containing a water-soluble monofluorophosphate and a polishing material containing at least a major (52 U.S. Cl..................................... 424/52; 424/49; proportion of dimagnesium orthophosphate. 106/62 (51 Int. Cl............................................. A61 K 7/18 4 Claims, No Drawings 3,966,901 1 2 The amount of monoflurophosphate in the dentifrice DENTIFRICE PREPARATION may be varied but should be an effective, non-toxic amount providing about 0.01-1% by weight of fluorine This is a continuation of application Ser. No. 389,628 to the dentifrice. Thus, sodium monofluorophosphate filed Aug. 21, 1973 now abandoned which is a continu is typically used in amounts of about 0.05-7.6% by ation of application Ser. No. 210,559, filed Dec. 21, weight. It is preferred that the sodium monofluorophos 1971, now abandoned. phate salt be no more than about 2%, and usually The present invention relates to a dentifrice prepara within the range of about 0.05% to about 1%, by weight tion containing a water-soluble monofluorophosphate of the dentifrice. and a polishing material containing at least a major 10 The polishing material contains at least a major pro proportion of dimagnesium orthophosphate. portion of dimagnesium orthophosphate, preferably Water soluble monofluorophosphates and particu dimagnesium orthophosphate trihydrate. Other suit larly alkali metal monofluorophosphates such as so able dimagnesium orthophosphates may be used, in dium monofluorophosphate have been disclosed and cluding the heptahydrate. The dimagnesium ortho used as fluorine-providing active ingredients in denti 15 phosphate may be used singly as the sole polishing frice preparations. The polishing agents which may be agent. If desired, it may also be used in combination used for such dentifrices have been the subject of much with other polishing agents as the major ingredient investigation. (more than 50% by weight) of the polishing material. A A dentifrice containing sodium monofluorophos single form of the dimagnesium orthophosphate may be phate and a polishing agent which is principally dical 20 used as well as mixtures of the hydrates in any suitable cium orthophosphate is known to be highly effective in ratio resulting from a blend or formed in situ in the reducing the formation of caries. This dentifrice does manufacture of the dimagnesium orthophosphate. tend to lose a portion of its effectiveness when subject Such all additional polishing agent includes calcium to prolonged aging. It has therefore been most desir carbonate such as natural chalk and precipitated cal able to use it in relatively fresh condition. 25 cium carbonate in minor proportion (i.e. less than 50% It is an advantage of this invention that a dental by weight) of the polishing material. Magnesium car cream is obtained which provides fluorine and is highly bonate may also be used as a minor component of the stable upon prolonged aging. Other advantages will be polishing material, instead of or in addition to calcium apparent from consideration of the following specifica carbonate. These polishing materials are employed in tion. 30 finely powdered form of any suitable particle size for In accordance with certain of its aspects, this inven effective polishing power. tion relates to a dentifrice preparation which comprises In the case of the dimagnesium orthophosphate and a water-soluble monofluorophosphate and compatible alkaline earth metal carbonate (such as calcium car polishing material at least a major part of which is bonate and/or magnesium carbonate) mixtures, the dimagnesium orthophosphate. 35 ratio of these materials is variable and is preferably in The water-soluble monofluorophosphate is prefer the range of about 99:1 to about 65:35 by weight, and ably sodium monofluorophosphate. Sodium mono usually about 25:1 to 3:1, depending upon the particu fluorophosphate (NaPOF) is a water-soluble material lar form of orthophosphate and the particular carbon which releases monofluorophosphate ions in water, and ate used. In general, it is preferred to prepare dental it may be mixed with the polishing material in any 40 creams having 35-60% polishing material with dimag suitable amount. Such dental preparation is compatible nesium orthophosphate as the main polishing ingredi with suitable amounts of surface-active agents, gum, ent and from 0 to 15% calcium carbonate or magne etc., as described. The sodium monofluorophosphate sium carbonate in the dental cream. If desired other as commercially available may vary considerably in polishing materials may be added in suitable amount purity. It may be used in any suitable purity provided 45 such as hydrated alumina, calcium pyrophosphate, that any impurities do not substantially adversely affect tricalcium phosphate, calcium polymetaphosphate and the desired properties. In general, the purity, is desir the like. The total content of polishing agents will be ably at least about 80%. For best results, it should be at usually at least 20%, such as about 20–99% and partic least 85%, and preferably at least 90% by weight of ularly from 20-75%, preferably 35-60%, in toothpastes sodium monofluorophosphate with the balance being 50 and at least 70% in tooth powders. primarily impurities or by-products of manufacture Any suitable surface active or detersive material may such as sodium fluoride, water-soluble sodium phos be included in the dentifrice compositions. Such com phate salt, and the like. Expressed in another way, the patible materials are desirable to provide additional sodium monofluorophosphate employed should have a detersive, foaming and anti-bacterial properties de total fluoride content of about 12%, preferably above 55 pending upon the specific type of surface active mate 12.7%; a content of not more than 1.5%, preferably not rial and are selected similarly. These detergents are more than 1.2% of free sodium fluoride; and a sodium water-soluble organic compounds usually, and may be monofluorophosphate content of at least 12%, prefer anionic, non-ionic or cationic in structure. It is pre ably at least 12.1%, all calculated as fluorine. ferred to use the water-soluble salts of higher fatty acid In addition to sodium monofluorophosphate, other 60 monoglyceride monosulphate detergent (e.g. sodium monofluorophosphate salts which have sufficient water coconut fatty acid monoglyceride monosulphate), solubility for use in the instant invention include cal higher alkyl sulphate (e.g. sodium lauryl sulfate), alkyl cium monofluorophosphate, magnesium monofluoro aryl sulphonate (e.g. sodium dodecyl benzene sulpho phosphate and aluminum monofluorophosphate. The nate) higher fatty acid esters of 1,2-dihydroxy propane term "monofluorophosphate' also includes mono 65 sulphonate (e.g. sodium coconut fatty acid ester of fluoropolyphosphates such as NaPOF, KPOF, 1,2-dihydroxy propane sulphonate), and the like. (NH)POF, Naa KPOF, (NH)NaPOF and LiP In various surface active materials may be used in any OF. suitable amount, generally from about 0.05 to about 3,966,901 3 4 10% by weight, and preferably from about 0.5 to 5% by Other types of dentifrice compositions will be formu weight of the dentifrice composition. lated in known manner also. It is a further embodiment of the present invention to A minor amount of hydrated aluminium oxide may use the substantially saturated higher aliphatic acyl be incorporated in the dentifrice preparation. More amides of lower aliphatic amino carboxylic acid com particularly, a dental cream having improved physical pounds, such as those having 12 to 16 carbons in the properties may be prepared from a mixture of the acyl radical, and as more particularly described in U.S. dimagnesium orthophosphate trihydrate optionally Pat. No. 2,689,170, issued Sept. 14, 1954. The amino with a minor amount of calcium carbonate or magne acid portion is derived generally from the lower ali sium carbonate or dimagnesium orthophosphate hepta phatic saturated monoaminocarboxylic acids having 10 hydrate suspended in a gel comprising water, humec about 2 to 6 carbons, usually the monocarboxylic acid tant and gelling agent, with said monofluorophosphate compounds. Suitable compounds are the fatty acid compound and organic non-soap synthetic detergent, amides of glycine, sarcosine, alanine, 3-amino propa and preferably a minor amount of hydrated aluminium noic acid and valine having about 12 to 16 carbons in oxide. These dental creams exhibit a superior degree of the acyl group. It is preferred to use the N-lauroyl, 15 cosmetic properties and physical stability to aging for myristoyl and palmitoyl sarcoside compounds however long periods of time. The aluminium oxide acts as a for optimum effects. stabilizing and modifying agent so as to eliminate or The amide compounds may be employed in the form inhibit any tendency for separation or "bleeding' of of the free acid or preferably as the water-soluble salts the dental cream in the collapsible tube. thereof, such as the alkali metal, ammonium, amine 20 Suitable examples of hydrated aluminium oxide and alkylolamine salts.