7.4.

4 Manufacture of toothpastes Toothpaste can be manufactured via two separate distinct batch processes, both of which are, in principle, three-step methods. Continuous or semi-continuous variations of these methods can be found among the larger manufacturers. A brief outline of the fundamental batch processes are given below: General method A Stage 1 is to carefully blend all powder components of the toothpaste together, including the gelling agents, abrasives and thickening agents: l(a-f) Abrasives 4(a-f) Gelling agents 8 and 9 Powdered Therapeutic Agents 5a Sweetener 7(a-f) Whitener/Colours This blend is essential to avoid aggregation of the gelling agent.

Stage 2 is then to mix this blend with all the aqueous and liquid components of the paste (humectants, water) in a heavy-duty mixer: 3(a-d) Humectants 10 Purified Water Following complete swelling of the gelling agent a homogeneous paste will be obtained. General method B In stage 1 of this process, the gelling agent is fully hydrated in the presence of sufficient water and heat if necessary. In addition all soluble salts may be added: 3(a-d) Humectants 4(a-f) Gelling Agents 8 and 9 Powdered Therapeutic Agents 10 Purified Water Several processing variations may be used, especially in the hydration of the gel, but generally the manufacturer of the gelling agents recommend either (a) dispersion in the non-aqueous portion of the humectant system (glycerin or propylene glycol) before addition of the free water and the ingredients added in solution in order to ensure good hydration and prevent gel lump formation; or (b) continually hydrating the gelling agent by pulling small amounts of the powder into a stream of cold water. Stage 2 of the process is to mix the fully dispersed gel and the powders together also in a duty mixer: l(a-f) Abrasives 5(a) Sweetener 7(a-f) Whitener/Colours Following complete mixing a homogeneous paste will be obtained. Addition of flavour and surfactants In stage 3 the homogeneous paste obtained from either process must then be mixed with both the surfactant and the flavour under vacuum. This is essential in order to de-aerate the product at the final stage, otherwise a cosmetically unacceptable 'mousse'-type consistency will be produced. These are often added as late as possible in the manufacture because mixing the surface-active agent will create foaming and air entrapment if caution is not taken. Equally mixing under vacuum with the flavour added could cause unnecessary loss of some flavour components that can be up to 25% of the total raw material cost of the toothpaste.

When manufactured, appropriate analytical tests must be carried out to verify that the concentration of therapeutic ingredients is within acceptable ranges. Finally, microbial testing is necessary to confirm the quality of the product, specifically that it is not contaminated and that it prevents the growth of microorganisms. 7.5 TOOTHPASTE FORMULATIONS 7.5.1 Anti-cavity (fluoride) Early in the last century, epidemiological studies showed that people living in areas with naturally fluoridated water (optimal <lppm), had significantly lower levels of dental caries compared to those living in a non-fluoridated region (Mellberg and Ripa, 1973). This led manufacturers in the 1950s to add 'fluoride' to a toothpaste in order to add the anti-cavity benefit of fluoride to the cleaning effect of toothbrushing. Extensive clinical trials have been carried out since then, testing various formulation options, in co-operation with both the dental profession and academic researchers. These typically show that correctly formulated toothpastes with 1000ppm F~ can give caries reduction in the range of 10-30% after three years. This can be increased by a further 10-15% when the content of F~ is increased to 1500ppm (Hodge et aL, 1980; Fogels et aL, 1988). (Note: The maximum level permitted by the EEC Cosmetics Directive is 1500ppm F~.) These studies have resulted in various professional bodies, such as the Council of Dental Therapeutics of the American Dental Association, and the British Dental Association, giving a formal qualification and acceptance of toothpastes once the data showing their clinical effectiveness have been reviewed and accepted. Such accreditation was first given in the US to a stannous fluoride-calcium pyrophosphate toothpaste in 1960 (American Dental Association, Council on Dental Therapeutics, 1960). Ultimately in the early 1990s the World Health Organization recognized that use of an appropriately fluoridated dental cream was one of the major reasons for a dramatic decline in caries in the developed world (WHO, 1994). They concluded that the additive results of long-term usage far surpassed the initial reductions measured in the 3-year clinical trials. Today, anti-cavity toothpastes containing fluoride salts at either 1000 or 1500 ppm have almost become generic and are the 'cost of entry' into the category. Significantly less than 5% of the dentifrice volume sold in developed world countries is non-fluoridated. Various fluoride sources have been used throughout the past thirty years, depending upon the formulator's objectives: 8(a) Sodium Monofluorophosphate (Na2PO3F) 8(b) Sodium Fluoride (NaF) 8(c) Organo (amine) Fluorides 8(d) Stannous Fluoride (SnF2)