GUIDELINES FOR STABILITY TESTING OF SUNSCREENS # compiled by the Australian Society of Cosmetic Chemists (ASCC), the Cosmetic Toiletry, Fragrance Association of Australia (CTFAA), the Nutritional Foods Associations of Australia (NFAA) and the Proprietary Medicines Association of Australia (PMAA) accepted by the Therapeutic Goods Administration (TGA) APRIL 1994 products required to be included in the Australian Register of Therapeutic Goods (ARTG)General Comments In discussions with the Therapeutic Goods Administration (TGA) and industry, it has been acknowledged that sunscreen preparations, while being designated therapeutic goods fall across the therapeutic goods/cosmetic interface and therefore must compete in both markets, It has been agreed that a balance should be struck that achicves the appropriate Confidence in the. quality and stability of the product without disadvantaging quick Tesponses to market and regulatory trends. ‘The purpose of this guideline is to describe the types of stability testing programme that are suggested to achieve those goals. Generation of adequate stability data to support an assigned shelf life for a therapeutic Sunscreen product is the responsibility of the sponsor - this is an agreed self-regulatory Process between TGA and industry. These stability guidelines should be viewed as the minimum requirement and sponsors may need to generate additional data to adequately justify the shelf-life claim. Sponsors are reminded that a condition of listing on the Australian Register of ‘Therapeutic Goods (ARTG) for these products is that sponsors must conduct stability studies to currently recognised standards, retain the data and notify TGA should any results indicate that the assigned shelf-life cannot be supported. Appropriate action, commensurate with public safety, should then be agreed.Specific Requirements 1. Both the physical stability of the product and the chemical stability of the actives should be established on not less than two lots of the formulation, ‘These lots may be laboratory batches but they should appropriately retlect the scaled-up production process. However, two production batches of that product must be subjected w real-time Stability testing for confirmation. Tt should not be necessary to seyuire Stability data on production batches before launch. Ongoing stability Programmes may be necessary eg. where changes have taken place to manufacturing procedures, or quality of the raw material, etc. 2. Physical Stability testing should include : appearance (eg. emulsion stability, crystallisation at high and low temperatures, etc). odour PH Gf water continuous) for broad spectrum sunscreens, % transmission according 10 AS2604 (or subsequent revisions) or equivalent methods immediate container and product compatibility (on all contact surfaces) 3. Chemical Stability testing should include : 34 actvels), to be determined by a stability:indicating, validated assay (eg. HPLC)Chemical Stability testing should include: (continued) 32 actives to remain within the limits of 90% - 120% of label claim for the shelf-life of the product.- (Overages may be formulated into the product however these must be declared at time of listing.) In borderline cases, the shelf-life might be justified by SPF measurement. 33 preservative efficacy at the start, at the end of the period of accelerated Stability testing and at the end of real time shelf-life, It may be useful to monitor chemical stability of preservatives dusing stability testing using a stability-indicating validated assay, Frequency Testing 4.1 Accelerated studies - suggested testing intervals are: 0, 3, 6, 12°, 24°, and 30° months but other time points eg. 1,2, 4 or 5 may also be used and may be necessary for some tests for adequate accelerated studies, ~ see also 6. Prediction of Shelf Life 42 Real time studies Testing at initial and annual intervals should be sufficient However, it is not necessary to have completed these testing programmes before launching the product, * depending on shelf life required to be justified by the study 4.Packs Stability testing should be carried out in the packs in which the product will be marketed, If this is not possible, stability testing should be catsied out in packs constructed of the same material, Prediction of Shelf Life 6.1 Shelf life may be predicted from accelerated data ONLY IF THE ACCURACY AND REPRODUCEABILITY OF THE RESULTS IS ADEQUATE TO SUPPORT THE FXTRAPOLATION. ALL DATA MUST BE FULLY DEFENSIBLE. 6.2 For the first three years of predicted shelf life, extrapolation using a minimum of six month stability data may be possible for products exhibiting minimal instability eg. Elevated Temp.” Possible (Above Labelled Time Period Shelf Life Storage Conditions) Prediction r 10°C 6 months 2 years +10°C 9 months 3 years 415°C 6 months 3 years * it may be advisable to monitor and log incubator function6. Prediction of Shelf Life (continued) 63 At least four real time data points, including the initial and 6 months, should be evaluated using acceptable statistical methods to justify the exuapulation. 6.4 The predicted value of the final concentration of the Sunscreen active should not fall outside expiry limits (Le. 90% - 120% of the label claim) at the end of the extrapolated shelf life. - refer Section 3.2 6.5 For predicted shelf life greater than three years, 2-fold extrapolation should be allowed. For example, for a five-year shelf life (maximum permissible), two and a half years of accelerated stability data at not less than 10°C above the recommended storage temperature should be required. 6.6 Stability programme to collect real time data from at least two production batches stored at the recommended storage condition should be initiated to confirm the extrapolated shelf life, ~ TGA SHOULD BE ADVISED IF THE PRODUCT FALLS OUTSIDE SPECIFICATION WITH APPROPRIATE ACTION NEGOTIATED AND AGREED 7. A shelf life greater than five years is not permitted for sunscreen products.From July 1, 1994 sunscreens should be labelled with storage conditions in accordance, with the Therapeutic Goods Order (TGO) 48 "General Requirements for Labels of Drug Products". Sponsors should note clause 139 of the Code of GMP for Sunscreens states that finished products should be stored in an environment compatible with the labelling ‘There shall be no requirement for products intended for Export market only to carry an expiry date, if the country of destination does not require expiry dating. If the country of destination requires expiry dating, then extrapolation of stability data to support shelf life should conform with the local regulatory requirement of that country, and not necessarily to the Australian requirement. ‘Suabuity fnat