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Stability Testing

What is stability testing?


Stability testing is the only true way to determine the correct shelf life or expiry date of your
product. Consumers expect their products to be aesthetically pleasing and perform
appropriately over the shelf life of the product. Stability testing is a way to ensure your
product will meet these expectations.
How is stability testing conducted?
In the ideal world, you would store your product at 25-30C for 2-3 years, and monitor any
changes to the product, before launching into the market place. Obviously, this is not
commercially viable. So instead, we conduct accelerated stability testing on your product to
provide you with a high degree of confidence that your product will be suitable in 2 or 3
years from now, after only 6 9 months.
Different products need different stability testing methods. We work with you, taking into
consideration the specific needs of your product, its ingredients and performance
characteristics, to ensure the stability program we develop best reflects your commercial
needs with a high degree of confidence in the results obtained.
Your stability program involves the following items you receive all documentation at
each test point and on completion:
-

Full stability protocols

Storage under appropriate test conditions

Full testing as per the protocol

Reports and recommendations

We can also prepare lab batches of your product for testing purposes if required.
We endeavour to provide you with the most cost effective stability testing program that is
going to provide you with valid results, whilst being conservative as possible with the budget.
Some standard stability testing includes:

25C or ambient temperature for 3 36 months

40C for 3 18 months

55C for 1 3 months

Freeze/thaw cycles

Light tests

Preservative efficacy testing (PET)

Assays of actives and preservatives

Stability programs are an important part of the product development process that are often
overlooked because they seem too hard or too expensive but there is nothing cheap about
a product recall. We are here to make it as cost effective, easy and timely as possible
contact us to find out how we can give you peace of mind and help you protect consumer
confidence in your product information: info@personalcarescience.com.au or call +61 8 8463
0990.

7 reasons to do a stability test on a cosmetic

by Perry Romanowski
One of the primary tests that you will run on your cosmetic formulations is a stability test.
You can read this other post for a complete procedure for stability testing.
In this post I wanted to go over the times when you should do a stability test.
1. New working prototype.

You dont need to do stability testing on every prototype but when you get to the point of
having one that gives good results, you should put up at least a minimal stability test. This
would include control samples (4C and RT) and samples at accelerated temperatures of at
least 45C. Early stability testing will speed up the launch process.
2. New raw material source.

Often your purchasing department will find a cheaper source of a material that you are
currently buying. Theyll then want to use the ingredient right away. However, dont use it
until you have conducted a proper stability test. Just because two raw materials have the same
INCI name, that doesnt mean they are the same. When you run the cosmetic stability test, be
sure to run a sample with the current formula along side the formula with the new ingredient.
3. Scaling up to production.

When your formula gets made on in production for the first time, youll need to do a stability
test. Things dont always work the same in production batches as in lab batches.
4. New production process.

Speaking of production, another important time to do a stability test is when you make any
changes to the production process. Often the compounders will discover faster ways to make
products but youll need to verify that the product will remain stable before implementing.
5. New packaging.

Even when you dont change the formula, you may have to run a new stability test. The most
common instance is when you change the packaging that the product is sold in. This could be
a whole new package type or simply a change in the package resin source.

6. Regulatory requirements.

Sometimes you have to run a stability test just to satisfy the regulatory paperwork of a new
market that your product is being sold in.
7. New production plant.

If your product is successful enough it might be produced in a different manufacturing


facility. In this case youll need to do a stability test just to ensure that the product remains to
be of the proper quality.
If you want to create consistently, high quality products, stability testing of cosmetic formulas
is one of the primary tests to run.

How To Stability Test a Cosmetic Formula

by Perry Romanowski

Heres the biggest difference between what you experienced in your college organic
chemistry lab versus a cosmetic formulation lab. In an organic lab, you mix chemicals
together and hope something happens. Ideally, you get a chemical reaction you expect. As a
formulating chemist, you mix chemicals together and hope nothing happens. Cosmetics are
mixtures of chemicals that mostly arent supposed to react with each other.
Unfortunately, they often do react (or otherwise change) so you need to test your formulas to
see how long they will last. This is called Stability Testing and is something a cosmetic
scientist spend much of her time doing. In this post, well give a brief description of the test
and suggest when, why and how it should be done.
What is stability testing?

Stability testing is simply an experiment in which you create a batch of your formula and put
samples of it at different environmental conditions for a set period of time. These conditions
vary in temperature and light levels and are meant to simulate what will happen to the
product during its life cycle.
At select intervals you evaluate your samples for various physical, chemical and performance
characteristics to see how they have changed. If the changes are minimal according to your
company standards, then your formula is said to have passed stability testing. This means
you can have confident that when the formula is shipped to stores and ultimately customers, it
will still be as good as when it was first manufactured.
The underlying assumption in stability testing is that increasing storage temperature speeds
up any aging reactions that will occur. A handy rule of thumb is that a sample stored at 45C
for 8 weeks is equivalent to one that is stored at room temperature for one year. This isnt an
exact predictor, but is good enough for the purposes of cosmetic products.
A sample stored at 45C for 8 weeks is equivalent to one stored at room temperature for a year

When do you perform stability testing?

Since youll be making hundreds or thousands of prototypes during your career, it wont be
practical to run a stability test on all of them. Youll also find that changes happen so rapidly
at your company, you wont have time to properly test many of your formulas. But there are
times when you need to do stability testing. Here is a short list of some of the most important
times to conduct a stability test.
1. New prototypes Whenever you make a new formula and are satisfied with the way it
performs, youll want to do a stability test to ensure that it will stay together. Dont bother
testing all your prototypes, just the ones that work the way you want.
2. New raw materials Whenever you have to change the fragrance, color, or other raw
material in a formula, youll have to do a stability test to make sure there arent unacceptable
changes. Also, when you have a new raw material source (or supplier) youll want to run a
test.
3. New manufacturing procedure Manufacturing is always trying to find faster ways to
make formulas. This often means they change some order of addition or shorten mixing time.
Whenever changes like these happen, it could affect your formula. Run a stability test to see
if the change is acceptable.
4. New packaging Cosmetic products change their look almost yearly so packaging is
constantly being modified. Whenever you get a new package, youll have to determine if the
formula continues to be compatible. Stability testing helps ensure that it is.
How do you stability test a cosmetic?

There are no set rules on how you must conduct a stability test for cosmetic products. Of
course, for cosmetic OTC products like sunscreens, AP/DO, or dandruff shampoos the FDA
has specific stability test requirements that you have to follow. See the FDA website for more
information.
Here is a basic format you can follow for conducting a cosmetic formula stability test.
Step 1 Make your batch. Calculate how much to make based on the number of samples
youll be using for the test. Its a good idea to make 30-40% more than you think youll need.
Step 2 Fill your samples. Ideally, youll have the correct packaging but dont count on it.
When appropriate, fill glass jars with the product along with the finished package. In stability
testing, you want to do both glass and packaging if possible. The number of samples depends
on how much testing your doing but at minimum you should have 2 samples for each storage
condition.
Step 3 Take initial readings. Once you have a sample filled test it for all the characteristics
youre going to evaluate later. The exact tests depend on the product but minimally youll

want to record notes about the appearance, color and fragrance. Youll also want to take pH
and viscosity readings. For aerosol products you will test spray patterns.
Step 4 Put samples at different conditions. Stability testing requires different temperature
and light conditions. Some standard temperatures include 50C, 45C, 37C, 25C (RT), and 4C.
Youll also want to conduct a freeze/thaw stability test which involves cycling your product
through 24 hours of freezing then 24 hours of thawing. Different lighting conditions involve a
fluorescent light box and a natural light box (to simulate sunlight).
Step 5 Evaluate the product. Samples should be evaluated at the following intervals. 2
weeks, 4 weeks, 8 weeks, 12 weeks, and 52 weeks. Only the RT, 37C and 4C samples will be
evaluated after one year. The highest temperature samples and the light exposed samples only
need to be evaluated for the first three test intervals. The evaluation tests should be the same
ones you conducted when taking your initial readings.
Step 6 Determine stability. After 8 weeks you can confidently decide whether your
formula is stable or not. Nearly all products will exhibit some change so it will be up to you
(and your boss) to decide whether the product passed or not.
Early in your career, stability testing will be one of the most common activities youll do. If
you can create a system that you consistently follow, youll avoid burn-out and be able to
confidently communicate when a product is appropriate to launch.
How does this compare to your companys stability procedure? Leave a comment and let
the rest of the cosmetic chemists here know.
Tagged as: cosmetic science, cosmetic testing, stability testing
http://chemistscorner.com/cosmetic-stability-testing-is-soft-science/

Cosmetic Stability Testing is Soft Science

by Perry Romanowski

One of the most surprising things to me when I started a career as a cosmetic science was
how subjective things were. There are no definitive answers about which surfactants to use,
how much, or even what testing procedures make sense. Stability testing, which is an
ubiquitous test that all cosmetic chemists will do, is not an exact science and decisions about
whether something passes or fails are highly subjective.
This non-scientific tendency troubles my scientifically leaning mind.
However, while there is a lot of subjectivity in cosmetic science, there are some scientific
principles behind the tests. Take cosmetic stability testing for example. One of the
procedures for testing the stability of emulsions is to put a sample at an accelerated
temperature and measure whether characteristics such as pH, viscosity or appearance
significantly changes. There is a rough rule that says .
3 months of storage at 37 45C equals 1 year of storage at RT
This rule is derived not only from experience but it is based on the Arrhenius equation. This
equation gives a useful generalization that reaction rates of a chemical reaction double for
every 10 degrees of increased temperature. So, if a formula is stable for 12 months at RT
(25C), it would be stable at 35C for 6 months and 45C for 3 months.
Simple right?
Of course, technically speaking the Arrehenius equation is not really valid for emulsions. It
predicts what happens when a specific chemical reaction happens at elevated temperatures.
But when an emulsion is exposed to higher temperatures, there are reactions that occur
which would not happen at room temperature. For example, at conditions above the melting
point of some of the emulsified materials.
Not a waste of time

Just because it isnt technically correct that doesnt mean storing samples at accelerated
temperatures isnt useful or predictive. In fact, you should use elevated temperatures to
predict stability. However, dont be surprised when a formula seems perfectly stable after 3
months of high temperature storage but fails at room temperature after a year.
Instability happens.

Governmental Guidelines for Cosmetic Stability Testing

by Perry Romanowski

I stumble upon some of the most interesting things while going through the Internet. Back in
2004 the CTFA (now the PCPC) and its EU sister organization COLIPA issued some
Guidelines on Stability Testing. We have previously written about cosmetic stability testing
which was strictly based on experience. Lets see how our stability advice stacks up.
Stability testing Objective

According to the report, the objective of stability testing is to ensure that products meet
chemical, microbiological and performance standards.
Yep, thats pretty much why you do stability testing. The other important part is that it
provides a paper trail for you to help prove that you are only selling safe products.
Stability testing design

A cosmetic stability test should be designed to assure

Stability and physical integrity of cosmetic products under appropriate


conditions of storage, transport and use,

Chemical stability,

Microbiological stability,

The compatibility between the contents and the container

Indeed, this makes sense. This means you have to test the products under different
conditions, in the right packaging, and do microbiological testing. The system we have
described in our stability testing post meets these requirements.
Interestingly, they hedge their bets by saying that Because of the wide variety of cosmetic
products and their inherent complexity, standard stability tests cannot be prescribed. That

is a good point but if you are creating a standard product, there are standard methods you can
follow.
Predicting shelf life

One of the most common questions we get asked is how much time at accelerated
temperature will predict 1 or 2 years of stability testing. The rule of thumb that I have
always followed is that a sample stored at 45C for 8 weeks will predict how the sample will
behave when stored at room temperature for 1 year.
The COLIPA guidelines do not give any such recommendations. This is typical of political
organizations. They never want to say anything too specific. In truth, the 45C for 8 weeks is
just a guideline and it may not work for every formula.
What to test in stability tests

The guidelines give a good description of the things you should test including

Color, odor and appearance,

Changes in the container,

pH,Viscosity,

Weight changes

Microbial tests demonstrating the ability of the products to prohibit


microbial growth during normal use and other specific tests if necessary,

Analytical data in relation to other parameters for specific product types

Finally, the COLIPA guidelines suggest that stability samples should be put under additional
stress such as Freeze/thaw testing and light exposure. This is a good practice. Ive seen
numerous samples change color and fragrance character when exposed to UV light. This will
happen to any product that is sold in stores under fluorescent lighting.
The guideline ends with some tips on creating your own cosmetic stability test protocol. You
are free to create one based on these testing guidelines or you can just follow the system that
weve already written about.
Just remember, stability testing is crucial to ensure your product is safe, of high quality, and
remains functional. You can not launch a product without it.

Cosmetic Stability Test Freeze Thaw Cycles

by Perry Romanowski
Previously, we covered the basics of cosmetic stability testing. But one member of the
Chemists Corner community wanted some more details on Freeze Thaw testing. Well look at
that aspect of stability testing in a little more detail.
What is Freeze Thaw testing

Freeze thaw testing is a type of stability test in which you freeze your formula, then thaw it
out, and test to see what effect the process has on your product. To do a thorough freeze-thaw
test you will repeat the cycle a few times.
Why do Freeze thaw testing?

Freeze thaw testing gives you information that regular stability testing cant. Namely, it will
show you whether your formula will remain stable under varied conditions that it might
experience during the shipping and storage phases of the product life cycle.
Its likely that your product will be shipped via trucks or rail cars. These vehicles are rarely
equipped with temperature controls so it is likely that your product may freeze one day and
be in hot temperatures another. It is crucial that your formula is able to withstand extreme,
rapid temperature changes.
How to conduct a freeze-thaw test

While there is no right way to do a freeze-thaw test, the following method is standard in the
industry and will give you the information you need if you follow it.
Step 1 Prepare samples. (3 test, 1 control)
Step 2 Take initial readings.
Step 3 Put test samples in the freezer for 24 hours
Step 4 Remove samples and allow to thaw at room temperature
Step 5 - Put samples in 50C oven for 24 hours
Step 6 Remove samples & allow to equilibrate at room temperature.
Step 7 Take end of the cycle readings
You should repeat this test through 3 cycles. If done correctly it can be completed in 3 weeks.

What to look for

While the specific tests will depend on the type of formula you are testing, generally youll
want to take readings for Appearance, Odor, Viscosity and pH. Make particular note of
whether there is any separating at the top or the bottom of samples. This is the most common
form of instability.
You may also test the products for performance characteristics just to ensure that the formulas
still work as expected.
Do you have any questions about stability testing or other cosmetic science topics? Send us
an email or leave a comment below
http://chemistscorner.com/
Cosmetic formula testing Triangle Test

by Perry Romanowski
As a cosmetic chemist, one of the most basic things you need to be able to do is to evaluate
formulas and new raw materials. This is one reason we highly recommend that formulators
try EVERY product they make. But just haphazardly trying a product will only give you so
much information. If you really want to know if a cosmetic formulation is different, youll
have to conduct a triangle test.
What is a triangle test

Simple put, a triangle test is a study in which you compare 3 samples and pick out the one
that is different. Of the three samples, one is actually different while two are the same. If you
can consistently pick out the different one, there is a pretty good chance that there is actually
some difference that youre picking up on. You might not always know what the difference is
but sometimes that doesnt matter. The key is that if you can notice a difference then there is
probably something different about it.
When to conduct a triangle test

Triangle tests are useful whenever you need to determine whether a change in the formula is
noticeable or not. So, they work well for

Fragrance evaluations When you have an odor change and you want to
see if there is a noticeable difference.

New raw materials To see if there is some performance effect by using a


raw material

Cost savings Remove a raw material and see if anyone can tell a
difference

Formula development See if changes youve made actually improve your


results

Triangle test basics

A triangle test can be done by one person or by an entire panel of people. The former is best
when you are making new prototypes and evaluating raw materials. The later is better for
making final decisions as it will give you some statistics and numbers to show your boss.
Step 1 Design your test
The first thing you have to do is figure out what test youll run to compare the samples. For
odor evaluations this can be a simple sniff test. Just put your formulas in a small jars, label
them and smell. I like to keep my eyes closed for odor evaluations or do it in a dark room so
you cant be influenced by color. For other products you can use any number of tests such as
foam tests, moisturizing tests, combing tests, etc. It really depends on what you are testing
and what characteristic you want to notice.
If you are doing a test in which you want to get some useful statistics, you need a panel of
about 30 people before you get meaningful data. However, if the differences are significant
youll be able to make decisions on many fewer test subjects (say 15).
Step 2 Make your samples
To do a triangle test you need to make two batches of a product. Be sure to create enough to
pour off multiple samples. One batch will be your control while the other will be your test.
When you are making your samples, flip a coin to decide which batch will be the one you
take two samples from and which will be the odd one out. Flipping a coin (or other random
process) is important because you dont want to always conduct the test in which the odd
sample is always the test sample.
Ideally, if you are going to test the samples, you should have someone else make and fill the
samples. At the very least you should have someone else fill and label them. That way you
can be singly blinded and wont be able to trick yourself.
Step 3 Test your samples
After the samples are made & labeled, run the test. Evaluate the products in the order they are
presented and give an initial guess as to which is the odd sample. It is useful to write down
your answer at this point.
Once youve tested the samples, it is helpful to re-run the test. This time you should randomly
mix the samples and evaluate them without knowing which sample is which. Try to hide the
labels. If you are unable to pick out the same sample then the first time was probably a fluke
and youll want to rerun it a few more times until you can consistently (or not) pick out the
same sample.

Step 4 Reveal the codes


Once you are certain youve got the odd sample, look at the codes to see if you picked out the
odd sample. If you did, then you can have some confidence that there really is a difference. If
you didnt, there probably isnt any real difference and the new raw material or the
formulation change you made was likely inconsequential, at least for the characteristic you
tested.
Step 5 Determine significance
If you were conducting the test with a panel of people you need to determine if there were
statistically significant differences. For people who like statistics you can figure out the Chi
squared distribution. X2=? (|O-E|)2/E, where O=observed and E=expected. Or you can use
this handy chart. Just find the number of people who have done the test on the left side and
see if the number of people who got it correct is on the right.

Click to enlarge
For example, if you did a test with 15 panelists, 9 of them would have to have picked the
correct odd sample for you to decide that there was a significant difference.
The triangle test is one of the key tools that a cosmetic chemist has at her disposal. You
should practice it often because the more you use it, the better youll get and the more useful
it will become.