ICH Q1B GUIDELINE PDF

References 1. This document is an annex to the parent guideline and addresses the recommendations for photostability testing. Preamble The intrinsic photostability characteristics of new drug substances and products should be evaluated to demonstrate that, as appropriate, light exposure does not result in unacceptable change. Normally, photostability testing is carried out on a single batch of material selected as described under "Selection of Batches" in the parent guideline. Under some circumstances these studies should be repeated if certain variations and changes are made to the product e. The guideline primarily addresses the generation of photostability information for submission in registration applications for new molecular entities and associated drug products.

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References 1. This document is an annex to the parent guideline and addresses the recommendations for photostability testing. Preamble The intrinsic photostability characteristics of new drug substances and products should be evaluated to demonstrate that, as appropriate, light exposure does not result in unacceptable change. Normally, photostability testing is carried out on a single batch of material selected as described under "Selection of Batches" in the parent guideline.

Under some circumstances these studies should be repeated if certain variations and changes are made to the product e. The guideline primarily addresses the generation of photostability information for submission in registration applications for new molecular entities and associated drug products.

The guideline does not cover the photostability of drugs after administration i. Alternative approaches may be used if they are scientifically sound and justification is provided. A systematic approach to photostability testing is recommended covering, as appropriate, studies such as: Tests on the drug substance; Tests on the exposed drug product outside of the immediate pack; and if necessary; Tests on the drug product in the immediate pack; and if necessary; Tests on the drug product in the marketing pack.

The extent of drug product testing should be established by assessing whether or not acceptable change has occurred at the end of the light exposure testing as described in the Decision Flow Chart for Photostability Testing of Drug Products. Acceptable change is change within limits justified by the applicant.

Light Sources The light sources described below may be used for photostability testing. The applicant should either maintain an appropriate control of temperature to minimize the effect of localized temperature changes or include a dark control in the same environment unless otherwise justified.

D65 is the internationally recognized standard for outdoor daylight as defined in ISO ID65 is the equivalent indoor indirect daylight standard. For a light source emitting significant radiation below nanometers nm , an appropriate filter s may be fitted to eliminate such radiation.

Option 2 For option 2 the same sample should be exposed to both the cool white fluorescent and near ultraviolet lamp. A cool white fluorescent lamp designed to produce an output similar to that specified in ISO ; and A near UV fluorescent lamp having a spectral distribution from nm to nm with a maximum energy emission between nm and nm; a significant proportion of UV should be in both bands of to nm and to nm.

Procedure For confirmatory studies, samples should be exposed to light providing an overall illumination of not less than 1. An example of an actinometric procedure is provided in the Annex. If protected samples e. Drug Substance For drug substances, photostability testing should consist of two parts: Forced degradation testing and confirmatory testing.

In these studies, the samples should be in chemically inert and transparent containers. In these forced degradation studies, a variety of exposure conditions may be used, depending on the photosensitivity of the drug substance involved and the intensity of the light sources used. For development and validation purposes, it is appropriate to limit exposure and end the studies if extensive decomposition occurs.

For photostable materials, studies may be terminated after an appropriate exposure level has been used. Under forcing conditions, decomposition products may be observed that are unlikely to be formed under the conditions used for confirmatory studies. This information may be useful in developing and validating suitable analytical methods. If in practice it has been demonstrated they are not formed in the confirmatory studies, these degradation products need not be further examined.

Confirmatory studies should then be undertaken to provide the information necessary for handling, packaging, and labeling see section I. Normally, only one batch of drug substance is tested during the development phase, and then the photostability characteristics should be confirmed on a single batch selected as described in the parent guideline if the drug is clearly photostable or photolabile.

If the results of the confirmatory study are equivocal, testing of up to two additional batches should be conducted. Samples should be selected as described in the parent guideline. All such precautions should be chosen to provide minimal interference with the exposure of samples under test. Possible interactions between the samples and any material used for containers or for general protection of the sample should also be considered and eliminated wherever not relevant to the test being carried out.

As a direct challenge for samples of solid drug substances, an appropriate amount of sample should be taken and placed in a suitable glass or plastic dish and protected with a suitable transparent cover if considered necessary. Solid drug substances should be spread across the container to give a thickness of typically not more than 3 millimeters. Drug substances that are liquids should be exposed in chemically inert and transparent containers. Analysis of Samples At the end of the exposure period, the samples should be examined for any changes in physical properties e.

Where solid drug substance samples are involved, sampling should ensure that a representative portion is used in individual tests. Similar sampling considerations, such as homogenization of the entire sample, apply to other materials that may not be homogeneous after exposure. The analysis of the exposed sample should be performed concomitantly with that of any protected samples used as dark control if these are used in the test.

Judgment of Results The forced degradation studies should be designed to provide suitable information to develop and validate test methods for the confirmatory studies. These test methods should be capable of resolving and detecting photolytic degradants that appear during the confirmatory studies. When evaluating the results of these studies, it is important to recognize that they form part of the stress testing and are not therefore designed to establish qualitative or quantitative limits for change.

The confirmatory studies should identify precautionary measures needed in manufacturing or in formulation of the drug product, and if light resistant packaging is needed. When evaluating the results of confirmatory studies to determine whether change due to exposure to light is acceptable, it is important to consider the results from other formal stability studies in order to assure that the drug will be within justified limits at time of use see the relevant ICH Stability and Impurity Guidelines.

Drug Product Normally, the studies on drug products should be carried out in a sequential manner starting with testing the fully exposed product then progressing as necessary to the product in the immediate pack and then in the marketing pack. Testing should progress until the results demonstrate that the drug product is adequately protected from exposure to light.

The drug product should be exposed to the light conditions described under the procedure in section I. Normally, only one batch of drug product is tested during the development phase, and then the photostability characteristics should be confirmed on a single batch selected as described in the parent guideline if the product is clearly photostable or photolabile. For some products where it has been demonstrated that the immediate pack is completely impenetrable to light, such as aluminum tubes or cans, testing should normally only be conducted on directly exposed drug product.

It may be appropriate to test certain products, such as infusion liquids or dermal creams, to support their photostability in-use. The analytical procedures used should be suitably validated. All such precautions should be chosen to provide minimal interference with the irradiation of samples under test.

Where practicable when testing samples of the drug product outside of the primary pack, these should be presented in a way similar to the conditions mentioned for the drug substance. The samples should be positioned to provide maximum area of exposure to the light source.

For example, tablets, capsules, should be spread in a single layer. If direct exposure is not practical e. If testing of the drug product in the immediate container or as marketed is needed, the samples should be placed horizontally or transversely with respect to the light source, whichever provides for the most uniform exposure of the samples.

Some adjustment of testing conditions may have to be made when testing large volume containers e. When powder samples are involved, sampling should ensure that a representative portion is used in individual tests. For solid oral dosage form products, testing should be conducted on an appropriately sized composite of, for example, 20 tablets or capsules. Similar sampling considerations, such as homogenization or solubilization of the entire sample, apply to other materials that may not be homogeneous after exposure e.

The analysis of the exposed sample should be performed concomitantly with that of any protected samples used as dark controls if these are used in the test. Judgment of Results Depending on the extent of change, special labeling or packaging may be needed to mitigate exposure to light. When evaluating the results of photostability studies to determine whether change due to exposure to light is acceptable, it is important to consider the results obtained from other formal stability studies in order to assure that the product will be within proposed specifications during the shelf life see the relevant ICH Stability and Impurity Guidelines.

Annex A. Option 1 Put 10 milliliters mL of the solution into a 20 mL colorless ampoule, seal it hermetically, and use this as the sample. Separately, put 10 mL of the solution into a 20 mL colorless ampoule see note 1 , seal it hermetically, wrap in aluminum foil to protect completely from light, and use this as the control. Expose the sample and control to the light source for an appropriate number of hours. After exposure determine the absorbances of the sample AT and the control AO at nm using a 1 centimeter cm pathlength.

The length of exposure should be sufficient to ensure a change in absorbance of at least 0. Option 2 Fill a 1 cm quartz cell and use this as the sample. Separately fill a 1 cm quartz cell, wrap in aluminum foil to protect completely from light, and use this as the control. After exposure determine the absorbances of the sample AT and the control AO at nm. Alternative packaging configurations may be used if appropriately validated.

Alternative validated chemical actinometers may be used. Glossary Immediate primary pack is that constituent of the packaging that is in direct contact with the drug substance or drug product, and includes any appropriate label. Marketing pack is the combination of immediate pack and other secondary packaging such as a carton. Forced degradation testing studies are those undertaken to degrade the sample deliberately. Confirmatory studies are those undertaken to establish photostability characteristics under standardized conditions.

For the confirmatory studies, the batch es should be selected according to batch selection for long-term and accelerated testing which is described in the parent guideline. References Yoshioka, S. Report a problem or mistake on this page Please select all that apply: A link, button or video is not working It has a spelling mistake Information is missing Information is outdated or wrong Login error when trying to access an account e.

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All companies developing or manufacturing pharmaceutical drugs, require a robust photostability testing process to ensure product quality and regulatory compliance. Inadequate testing can result in costly delays and lost revenue. Photostability Guidelines Testing is carried out on a single batch of material selected. Under some circumstances these studies should be repeated if certain variations and changes are made to the product e. The guideline primarily addresses the generation of photostability information for submission in Registration Applications for new molecular entities and associated drug products.

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