Stability of The Cosmetics

Accelerated stability, comparative
shelf life prediction for cosmetic

products
Dr. Arnold Uhl, Dr. Titus Sobisch, LUM GmbH, Berlin, GERMANY
in-cosmetics 2015
1.
2.
3.
4.
Introduction
Technology
Cosmetic o/w-emulsion
Conclusion
1
2015 LUM GmbH
ISO/TR 13097:2013 Guidelines for the

characterization of dispersion stability
Table of contents
http://www.iso.org/iso
Foreword
Introduction
/home/store/catalogu
1 Scope
e_tc/catalogue_detail.
2 Terms and definitions
htm?csnumber=52802
3 Basics of stability
3.1 Stability Summary
3.2 Characteristic features with regard to dispersion stability
3.3 Alteration of the state of a dispersion
4 Characterizing the change of the state of a dispersion
4.1 General comments
4.2 Direct methods
4.3 Correlative methods
4.4 Procedures to accelerate the evaluation of long-term stability
5 Prediction of the shelf life of a dispersion
5.1 General comments
5.2 Comparative analysis
5.3 Predictive analysis
Annex A A compilation of relevant international and national standards
Bibliography
Accelerated stability, comparative shelf life prediction for cosmetic products, in-cosmetics 2015
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ISO/TR 13097: 5. Prediction of shelf life

5.2. Comparative analysis
For QC purposes and for optimizing product properties or
product processing of an existing formulation, it is possible to
use a reference product for which the kinetics of stability
behaviour is well known and to compare the stability data of
the reference sample with the results of the new optimized
product using the same direct method and stability criteria.
If the alteration rate is slower than the reference sample, then
the new product can be considered as stable.
This approach is robust as no mathematical extrapolations are
used, but it does not quantify the product shelf life. This
approach can be used for virtually all types of dispersions and
acceleration methods according to 4.4. of TR
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Why measure cosmetic products accelerated?

Typical shelf life for example:
Shampoo / Conditioner 2-3 years
http://organizeyourlife.org/expiration.htm (22.6.2012)
Face Make up (Liquid: liquid

foundation, concealing liquids,
liquid/cream blush, eyeshadow,
etc.) 6-12 months
http://www.buzzle.com/articles/makeup-expiration-dates-shelflife-of-makeup.html (15.2.2012)
Sun cream 2-3 years
http://www.nhs.uk/chq/Pages/1970.aspx?CategoryID=70&SubCate
goryID=169 (22.2.2012)
For product development and improvement

fast and reliable information is required.
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Dispersions are beautiful and complex.

Sedimentation G
Flocculation
Creaming G
Coagulation D [G]
G = Gravity driven
D = Diffusion driven
Ostwald ripening D
Phase Inversion D
Coalescence D [G]
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products
in-cosmetics 2015
1. Introduction
2. Technology
6
2015 LUM GmbH
STEP-Technology:
Space and Time resolved Extinction Profiles
Concentration at all positions at all times

NIR light source for almost all samples
Blue light source for nanoparticles, liposomes, transparent formulations
X-ray source for high concentrated sediments and inorganic particles
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STEP-Technology in LUMiFuge / LUMiSizer

Physical acceleration
from 6 x to 2300 x
Light
Sample
Acceleration by
temperature 4C to 60C.
Sensor
Multi-wavelength.
Multisample analysis
(up to 12 simultaneously).
Transmission
kinetics
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STEP-Technology in LUMiFuge / LUMiSizer
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How can we use STEP-Technology?
Particle migration at gravity or in the

accelerated measurement
Stokes Law:
v=
2 . r2. f() . xg
9
v Particle velocity
Density
dyn. Viscosity of cont. phase
r2 Particle size
Particle concentration
xg real-time or accelerated -Physical acceleration
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How can we use STEP-Technology?
Particle migration at gravity

or in the accelerated measurement
Optical detection of
particle concentration
IO
d
Stokes Law:
v=
2
9
. r2
. f() .
I
xg
v Particle velocity
Density
dyn. Viscosity of cont. phase
r2 Particle size
Particle concentration
xg real-time or accelerated
Lambert-Beers Law:
- ln
I
=E=..d
IO
= f (, r, n, ...)
I0 Light factor | light intensity

Extinction coefficient
d optical path length (cell thickness)
NIR, blue & further wavelength)
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What can we determine?

1. v -velocity at x=1 for gravity, x=6-2300 for accelerated tests
for the formulation in its original concentration
| Stability & shelf life | Particle Interactions |
2.
Hydrodynamic density of particles (solid or liquid)

in liquid continuous phase
3. r Droplet size / Particle size distribution

4.
Dynamic viscosity of continuous phase
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Analysis results for QC/QA and R&D
Fingerprinting of transmission profiles
Instability index
Separation kinetics
Droplet / Particle size,

separation velocity &
density distributions
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products
in-cosmetics 2015
1. Introduction
2. Technology
3. Cosmetic o/w-emulsion
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2015 LUM GmbH
Cosmetic emulsion (o/w type)
Applied SOP for discussed and further unknown samples. Controlled stop
after 1 hour. Effective analysis time 5 min (future measurement time
at 50C).
Acceleration by temperature 50C identical to one of customers realtime storage temperatures.
4000 rpm equivalent to 2300 times higher gravity at position of 130 mm
(reference = cell bottom).
Detection by NIR at 865 nm ideal for turbid or coloured samples.
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Cosmetic emulsion (o/w type) after separation
By naked eye after 64 min at higher gravity

(2300 times physically accelerated) and 50C.
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Cosmetic emulsion (o/w type) 3 min
Evolution of transmission profiles during 3 min at higher gravity

(2300 times physically accelerated) and 50C
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64 min at higher gravity (2300 times physically accelerated), 50C;

NIR-results confirmed by visual inspection.
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Instability index* after 250 s
*Dispersion Letters Technical, T4 (2013) 1-4 ISBN: 978-3-944261-29-4

ww.dispersion-letters.com, Region-of-Interest 4 mm from cell bottom
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Creaming velocity* @higher gravity, 50C
*Tracing the movement of the interface clear water phase/ emulsion at a transmission of 11 %
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Comparative Shelf Life Prediction A vs. B

Customers shelf life information:
Emulsion A breaks after 2 months, B does not break.
Chemical composition & application are the same.
Qualitative result:
Transmission profiles of A change before those of B, A shows a
faster separation. Separation type identical.
Quantitative result (relative):
Instability index of A is much higher than B.
Quantitative result (absolute):
Creaming velocity of A is much higher than B.
B is the more stable formulation than A.
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23
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products
in-cosmetics 2015
1.
2.
3.
4.
Introduction
Technology
Cosmetic o/w-emulsion
Conclusion
24
2015 LUM GmbH
CONCLUSION
Acceleration by higher gravity and by temperature allow for a fast
and easy comparative shelf life prediction of cosmetic
products according to ISO/TR 13097: 2013, chapter 5.2.
Multisampling approach in LUMiSizer / LUMiFuge instruments
make it an efficient method for up to 12 samples at the same time.
The large variety of cosmetic formulations (chemical
composition, optical properties, concentration, separation types) is
respected by different sample cells, different detection
wavelengths, but the same STEP-technology.
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From Particle Characterization

1.Particle properties of micro- and
nanoparticles
MICROPARTICLES
NANOPARTICLES
Multi-wavelength
Separation Analyser LUMiReaderPSA
Multi-wavelength
Dispersion Analyser LUMiSizer
ISO 13317-1
ISO 13318
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via Dispersion Stability of
1. Particles
2. After Shave Balms, Creams, Leather

Gels, Liposomes, Make up, Nail
Varnish, Shampoo, Softener, Sun Care,
Tooth Paste
ISO/TR 13097
Real-Time
Direct and Accelerated
Multi-wavelength Stability Analyser

LUMiReaderPSA
LUMiFuge
Multi-wavelength
LUMiSizer
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to Properties of Separated Phases

2. After Shave Balms, Creams, Leather Gels, Make up, Nail Varnish,
Shampoo, Softener, Sun Care, Tooth Paste
3. Sediment concentration profiles,

cream layer properties after
accelerated separation
1. Particles
Separation Analyser
LUMiReader X-ray
ISO/TR 13097
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2015 LUM GmbH
More information:
The formulation of a distinctive skin care product
Prediction of Emulsion Stability: Facts and Myths
Accelerated Stability Testing of W/O Creams
Predicting the shelf life of Liquid Fabric Softeners
See also the bibliography in ISO/TR 13097 and search by keyword

for links to literature on http://www.lum-gmbh.com/Literature_Database.html
R. Moyon, K. Golz, L. Zastrow, SFW Journal 4-2007.
V. Andr, N. Willenbacher, H. Debus, L. Bger, P. Fernandez, T. Frechen, J. Rieger,

Cosmetics and Toiletries Manufacture Worldwide, 2003, 102-109.
A. Brmer, R. Daniels, 4th World Meeting on Pharmaceutics, 2002, Florence, IT
P. Vinson, M. Weaver, D. Bohlen, M. Thompson, W. Broeckx

Procter & Gamble, International Workshop Dispersion Analysis 2012, Berlin, Germany,
www.dispersion-letters.com/wpcontent/uploads/2012/02/Predicting_the_shelf_life_of_Liquid_Fabric_Softeners.pdf
(17.2.2012).
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29
2015 LUM GmbH
Thank you for your

attention.
Your kindly invited to

meet us at Stand 6C60
and ...
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30
2015 LUM GmbH

Stability of The Cosmetics

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Stability of The Cosmetics

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Accelerated stability, comparative

shelf life prediction for cosmetic

ISO/TR 13097:2013 Guidelines for the

ISO/TR 13097: 5. Prediction of shelf life

Why measure cosmetic products accelerated?

Face Make up (Liquid: liquid

Sun cream 2-3 years

For product development and improvement

Dispersions are beautiful and complex.

Accelerated stability, comparative

Concentration at all positions at all times

STEP-Technology in LUMiFuge / LUMiSizer

STEP-Technology in LUMiFuge / LUMiSizer

How can we use STEP-Technology?

Particle migration at gravity or in the

How can we use STEP-Technology?

Particle migration at gravity

I0 Light factor | light intensity

What can we determine?

Hydrodynamic density of particles (solid or liquid)

3. r Droplet size / Particle size distribution

Dynamic viscosity of continuous phase

Analysis results for QC/QA and R&D

Fingerprinting of transmission profiles

Droplet / Particle size,

Accelerated stability, comparative

Cosmetic emulsion (o/w type)

Cosmetic emulsion (o/w type) after separation

By naked eye after 64 min at higher gravity

Cosmetic emulsion (o/w type) 3 min

Evolution of transmission profiles during 3 min at higher gravity

Cosmetic emulsion (o/w type) 5 min

Evolution of transmission profiles during 5 min at higher gravity

Cosmetic emulsion (o/w type) 10 min

Evolution of transmission profiles during 10 min at higher gravity

Cosmetic emulsion (o/w type) 64 min

64 min at higher gravity (2300 times physically accelerated), 50C;

Instability index* after 250 s

*Dispersion Letters Technical, T4 (2013) 1-4 ISBN: 978-3-944261-29-4

Creaming velocity* @higher gravity, 50C

Comparative Shelf Life Prediction A vs. B

Accelerated stability, comparative

From Particle Characterization

via Dispersion Stability of

2. After Shave Balms, Creams, Leather

Direct and Accelerated

Multi-wavelength Stability Analyser

to Properties of Separated Phases

3. Sediment concentration profiles,

The formulation of a distinctive skin care product

Prediction of Emulsion Stability: Facts and Myths

Accelerated Stability Testing of W/O Creams

Predicting the shelf life of Liquid Fabric Softeners

See also the bibliography in ISO/TR 13097 and search by keyword

R. Moyon, K. Golz, L. Zastrow, SFW Journal 4-2007.

V. Andr, N. Willenbacher, H. Debus, L. Bger, P. Fernandez, T. Frechen, J. Rieger,

A. Brmer, R. Daniels, 4th World Meeting on Pharmaceutics, 2002, Florence, IT

P. Vinson, M. Weaver, D. Bohlen, M. Thompson, W. Broeckx

Thank you for your

Your kindly invited to

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