SUNTEST

Accelerated Tabletop Exposure Systems

A Comment on Photostability Testing According to ICH

 ICH Guideline for the Photostability Testing of

New Drug Substances and Drug Products

Dated November 1996

- Summary of the important details –

......

0 General

B. Light Sources

. . . . . . The applicant should either maintain an appropriate control of temperature

to minimize the effect of localized temperature change or include a dark control in
the same environment unless otherwise justified.

Option 1
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 UV outputs,
- xenon-lamps or
- metal-halide lamps
D65 is the internationally recognised standard for outdoor daylight as defined in
ISO 10977 (1993). ID65 is the equivalent indoor indirect daylight standard. For a
light source emitting significant radiation below 320 nm, an appropriate filter(s)
may be fitted to eliminate such radiation.

Option 2
For option 2 the 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 nm to 360 nm and
360 nm to 400 nm.

C. Procedure (*)

For confirmatory studies samples should be exposed to 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 . . . . . . .
Samples may be exposed side-by-side with a validated chemical actinometric
system to ensure the specified light exposure is obtained, or for the appropriate
period of time when conditions have been monitored using calibrated
radiometers/luxmeters.
. . . . . . If protected samples (e.g. wrapped in aluminium foil) are used as dark
controls to evaluate the contribution of thermally induced change to the total
observed change, these should be placed alongside the authentic sample.
......
(*) Interpretation see page 3 and 4
 How to calculate the test duration

in the SUNTEST

according to ICH Guideline

♦ The described cut-off in the UV at approx. 320 nm is requiring in the SUNTEST a

filter system consisting out of a coated quartz glass dish (Id.no.: 56052388) and two
window glass filters (Id.no.: 56052372 & 56077769): The specified spectral ditribution
of ID65 ”as defined in ISO 10977” is given.

♦ The first mentioned required radiant exposure - ≥ 1.2 million lux hours - only refers
to the visible wavelength range from approx. 400 nm to 800 nm due to the
photometric unit used (the spectral distribution of the radiation is folded with the
spectral sensitivity of the human eye). The second radiant exposure value - ≥ 200 watt
hours/meter square - is refering to a wavelength range from 300 nm to 400 nm (UV-
range).

♦ The irradiance level in the SUNTEST can be adjusted from a minimum value of 250
watts/m² to a maximum value of 765 watts/m² - between 300 nm and 800 nm.
With the above mentioned filter combination installed these limits correspond to a
range from approx. 22.5 watts/m² to 68.9 watts/m² in the UV-range between 300 nm
and 400 nm – and to a range from approx. 55 klux to 170 klux in the visible range
between 400 nm and 800 nm.
Note: All irradiance resp. illuminance values refer to the calibration/adjustement level in a SUNTEST !!

♦ How to calculate now the test duration in the SUNTEST to meet the radiant exposure
value between 300 nm and 400 nm and the one between 400 nm and 800 nm ?

♦ 200 watt hours/m² (between 300 nm and 400 nm)

At minimum irradiance level:
200 watt hours/m² ÷ 22.5 watts/m² = 8.9 hours SUNTEST exposure
At maximum irradiance level:
200 watt hours/m² ÷ 68.9watts/m² = 2.9 hours SUNTEST exposure

♦ 1.2 million lux hours (between 400 nm and 800 nm)

At minimum irradiance level:
1.2 million lux hours ÷ 55 klux = 21.8 hours SUNTEST exposure
At maximum irradiance level:
1.2 million lux hours ÷ 170 klux = 7.1 hours SUNTEST exposure
♦ Programming the higher irradiance level shortens the test duration approx. by the factor
”3”, when compared to a test run at the minimum irradiance level ! As the ICH
Guideline does not specify an irradiance level, the user may adjust it according to his
individual requirements.

But: Be aware that the temperature, for example the BST (Black Standard
Temperature), will increase when the irradiance is raised !
Knowing the thermosensitivity of the material to be tested, you have to find out the
optimum irradiance level:
High enough to accelerate the test and low enough to avoid unwelcome
temperature effects !
Optionally you can fit the SunCool to the SUNTEST, a cooling aggregate, to
keep the temperature low either when running a test at a higher irradiance level, or
even when running a test at the minimum irradiance level, in case you are testing
really thermosensitive drugs or drug products.
Please take into accout what is required by the ICH Guideline under ”I. C. Procedure”:
” . . . . . . protected samples (e.g. wrapped in aluminium foil) are used as dark
controls to evaluate the contribution of thermally induced change to the total
observed change, . . . . . . ”.

♦ Running a test (for example at the minimum irradiance level) means that you have to
run an 8.9 hour-test (test end criterion: 200 watt hours/m² in the UV wavelength range)
and a 21.8 hour-test (test end criterion: 1.2 million lux hours in the visible wavelength
range) !
Due to the specific filter-/lamp-configuration the spectrum which is emitted by the
SUNTEST contains UV- and visible radiation, as defined by the requirement to
simulate ”Sunlight Behind Window Glass”.
A test run with the test end criterion ”1.2 million lux hours” therefore covers at the
same time the required radiant exposure in the UV-range (200 watts/m²) – respectively
exceeds this requirement by a factor of approx. 2.5 !

Thus the user wanting to reach in his test these minimum radiant exposure values has
two possibilities:
The user runs two tests - one for each test end criterion – with identical samples !
Or:
The user runs only one test covering both test end criteria, removing 50 % of his
samples after having reached the radiant exposure for the UV-range and the other
50 % after having reached the one for the visible range !

ATLAS
Material Testing Technology LLC
4114 North Ravenswood Avenue
Chicago, Illinois 60613
U.S.A.
Phone: +1(773)327-4520
Fax: +1(773)327-5787
ATLAS
Material Testing Technology GmbH
Vogelsbergstrasse 22
63589 Linsengericht/Altenhasslau
Germany
Phone: +49/6051/707-140
Fax: +49/6051/707-149
ICH_Nov96_E.doc