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Photo stability Testing on Pharmaceuticals

Presentation · August 2017

DOI: 10.13140/RG.2.2.17727.61609

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Photo stability
Testing on Pharmaceuticals
-Bujji Reddy Kanchi
Introduction

 Temperature, Humidity and Light are very important, essential to us.

 But this important factors may have an influence on our products to
degrade.

 Drug substance(API) or Drug Products(FPP)

#API : Active pharmaceutical ingredient.

#FPP : Finished pharmaceutical product.

Introduction-Light

 Light is the one of the environmental factor that can influence the product
quality.

 Study of product quality under the influence of light is called photo stability
testing..
Photo stability-Light source

 Natural day light(Sun light )has of both UV and Visible light wave lengths.
UV light :
Part of UV light is absorbed by ozone layer in the atmosphere. Part of the UV
light comes to the earth(320 nm to 400 nm)

Visible light:
Visible light is in the range of 400-800 nm of wave length.
Photo stability conducted for two
reasons
1. Confirmatory testing 2. stress testing

1. To know the product is light sensitive or not

-Confirmatory testing
Confirmatory studies are those undertaken to establish photostability
characteristics under standardized conditions.
Stress testing

To know the degradation pathways due to light and develop stability

indicative analytical method for determination of impurities and assay.
- Forced degradation study testing

Forced degradation testing studies are those undertaken to degrade the sample
deliberately. These studies, which may be undertaken in the development phase
normally on the drug substances, are used to evaluate the overall photosensitivity of
the material for method development purposes and/or degradation pathway
elucidation.
Photo stability-Illumination

 To achieve the condition of these light energy . these conditions are

artificially arranged to expose on the drug substance or products directly/
Immediate container.

 Light Exposure criteria (Not less than each visible and UV):
1.2 million lux hours for visible + 200 watt hours /sq.m. of UV energy.

There are two options to provide these conditions in photo stability

chamber.
Option-1 (quick exposure)

 Source that provides both Visible and UV elements at the same time –
Xenon discharge lamp – Metal halide lamp

 Simultaneously both UV and Visible exposures

Option 2

 Separate irradiation of the same sample with visible radiation followed by

near UV

 Visible lamp : Cool White Fluorescent Lamps that provide an output as per
ISO 10977
 UV lamp : Black lamp
For Near UV irradiation we use Black Light Fluorescent Lamps with – Spectral
distribution between 320 to 400nm – Max energy emission between 350 and
370nm
Batches to be selected

 Select one batch and 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

 At the end of the exposure period, the samples should be examined for
any changes in physical properties (e.g., appearance, clarity, or color of
solution) and for assay and degradants by a method suitably validated for
products likely to arise from photochemical degradation processes.
Judgment of Results

 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,
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.
Calibration of exposure
1.2 m luxhours and 200watt/sq.m
 Lux meters can be used.
 Or Actinometry
 Quinine Chemical Actinometry :
 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 colourless 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 400 nm using a 1 centimeter (cm)
path length. Calculate the change in absorbance, Δ A = AT - Ao. The
length of exposure should be sufficient to ensure a change in absorbance
of at least 0.9.
Estimation of time for the standard
exposure.
1.2 million lux hours
Read the intensity using lux meter externally :
Eg : the lux meter shows 20000 lux units when externally read by lux meter.

Time taken to achieve 1.2 million Lux is

= 1.2 x 1000000
20000
= 60 hours
Estimation of time for the standard exposure
200 watt/sq.meter

Read the uv meter externally :

Eg : the radiometer shows 10 watts/sq.meter.

Time taken to achieve 200 watts/sq.meter

= 200
10
= 20 hours.
 Option-1 takes less time than Option -2 exposure.
Time taken for confirmatory study

 Time taken for confirmatory study depends of capacity of illumination in the

stability chamber.
For example,
If the chamber emits radiation 50000 lux per hr, then it takes 24
hours to achive 1.2 million lux hours

 For forced degradation study 2 to 3 times to the confirmatory testing

exposure .
Decision tree for drug products
Decision

 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).
Questions and answers

 Which guideline is recommended for photo stability

A : ICH Q1B
 Purpose of Photo stabilty testing
A : to label the product is light sensitive or not and Forced degradation study
for developing methods and degradation pathways.
 How many batches required for testing
A: 1
Questions and answers

 What are the photostabilty conditions

light providing an overall illumination of not less than 1.2 million lux hours and
an integrated near ultraviolet energy of not less than 200 watt hours/square
meter
 What is option-1 testing
Any light source that is designed to produce an output similar to the D65/ID65
emission standard such as an artificial daylight fluorescent lamp combining
visible and ultraviolet (UV) outputs, xenon, or metal halide lamp. D65 is the
internationally recognized standard for outdoor daylight as defined in ISO
10977 (1993). ID65 is the equivalent indoor indirect daylight standard.
Questions and answers

 What is option 2 testing

For option 2 the same sample should be exposed to both the cool white
fluorescent and near ultraviolet lamp. 1. A cool white fluorescent lamp
designed to produce an output similar to that specified in ISO 10977(1993) ;
and 2. A near UV fluorescent lamp having a spectral distribution from 320 nm
to 400 nm with a maximum energy emission between 350 nm and 370 nm; a
significant proportion of UV should be in both bands of 320 to 360 nm and 360
to 400 nm.
Questions and answers

 What is criteria of sample Thickness during exposure

Not more than 3 mm
 Does all types of photo chambers takes same time to complete the
exposure
No. it depends on light illumination capacity available in the chamber
 Is there a need for photo safety testing of peptides/proteins?
In general, there is no need for photosafety testing of peptides/proteins.
(reference :emea, 17 March 2011 EMA/CHMP/SWP/336670/2010 )
Calibration of photo stability chamber

 How to do Calibration of stability chambers.

Using actinometry as specificed by ICH Q1B(2%quinine monohydrochloride
dihydrate ) or Light meters.

 What are calibration parameters

 Temperature accuracy and uniformity.
 Exposure-specified illumination
(1.2 million lux and 200 watt hours of UVA /sq meter)
  Thank you
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