Docslide - Us - Stability of The Cosmetics PDF

Accelerated stability, comparative
shelf life prediction for cosmetic

products
Dr. Arnold Uhl, Dr. Titus Sobisch, LUM GmbH, Berlin, GERMANY
in-cosmetics 2015
1. Introduction
2. Technology
3. Cosmetic o/w-emulsion
4. Conclusion
1
2015 LUM GmbH
ISO/TR 13097:2013 Guidelines for the
characterization of dispersion stability
Table of contents
Foreword http://www.iso.org/iso
Introduction /home/store/catalogu
1 Scope e_tc/catalogue_detail.
2 Terms and definitions
3 Basics of stability
htm?csnumber=52802
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 www.lum-gmbh.com 2
2015 LUM GmbH
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
2015 LUM GmbH
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-shelf-
life-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.
2015 LUM GmbH
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]
2015 LUM GmbH
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
2015 LUM GmbH
STEP-Technology in LUMiFuge / LUMiSizer
Physical acceleration
from 6 x to 2300 x Light
Sample
Acceleration by Sensor
temperature 4C to 60C.
Multi-wavelength.
Transmission
Multisample analysis
(up to 12 simultaneously). kinetics
2015 LUM GmbH
STEP-Technology in LUMiFuge / LUMiSizer
2015 LUM GmbH
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
2015 LUM GmbH
How can we use STEP-Technology?
Particle migration at gravity Optical detection of

or in the accelerated measurement particle concentration
IO
d
Stokes Law:
I
v= 2 . r2
. f() . xg
9 Lambert-Beers Law:
I
v Particle velocity - ln =E=..d
IO
Density = f (, r, n, ...)
dyn. Viscosity of cont. phase I0 Light factor | light intensity
r2 Particle size Extinction coefficient
Particle concentration d optical path length (cell thickness)
xg real-time or accelerated NIR, blue & further wavelength)
2015 LUM GmbH
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
2015 LUM GmbH
Analysis results for QC/QA and R&D
Fingerprinting of transmission profiles
Droplet / Particle size,

Instability index Separation kinetics
separation velocity &
density distributions
2015 LUM GmbH
products
in-cosmetics 2015
1. Introduction
2. Technology
14
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 real-
time 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.
2015 LUM GmbH
Cosmetic emulsion (o/w type) after separation
A B
By naked eye after 64 min at higher gravity

(2300 times physically accelerated) and 50C.
2015 LUM GmbH
Cosmetic emulsion (o/w type) 3 min
Evolution of transmission profiles during 3 min at higher gravity

(2300 times physically accelerated) and 50C
2015 LUM GmbH

2015 LUM GmbH

2015 LUM GmbH
64 min at higher gravity (2300 times physically accelerated), 50C;

NIR-results confirmed by visual inspection.
2015 LUM GmbH
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
2015 LUM GmbH
Creaming velocity* @higher gravity, 50C
*Tracing the movement of the interface clear water phase/ emulsion at a transmission of 11 %
2015 LUM GmbH
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.
2015 LUM GmbH
products
in-cosmetics 2015
1. Introduction
2. Technology
4. 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.
2015 LUM GmbH
From Particle Characterization
1.Particle properties of micro- and

nanoparticles
MICROPARTICLES NANOPARTICLES
Multi-wavelength Multi-wavelength
Separation Analyser LUMiReaderPSA Dispersion Analyser LUMiSizer
ISO 13317-1 ISO 13318

2015 LUM GmbH
via Dispersion Stability of
2. After Shave Balms, Creams, Leather

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

LUMiReaderPSA LUMiFuge LUMiSizer
2015 LUM GmbH
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
2015 LUM GmbH
More information:
The formulation of a distinctive skin care product
R. Moyon, K. Golz, L. Zastrow, SFW Journal 4-2007.
Prediction of Emulsion Stability: Facts and Myths

V. Andr, N. Willenbacher, H. Debus, L. Bger, P. Fernandez, T. Frechen, J. Rieger,
Cosmetics and Toiletries Manufacture Worldwide, 2003, 102-109.
Accelerated Stability Testing of W/O Creams

A. Brmer, R. Daniels, 4th World Meeting on Pharmaceutics, 2002, Florence, IT
Predicting the shelf life of Liquid Fabric Softeners

P. Vinson, M. Weaver, D. Bohlen, M. Thompson, W. Broeckx
Procter & Gamble, International Workshop Dispersion Analysis 2012, Berlin, Germany,
www.dispersion-letters.com/wp-
content/uploads/2012/02/Predicting_the_shelf_life_of_Liquid_Fabric_Softeners.pdf
(17.2.2012).
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
2015 LUM GmbH
Thank you for your
attention.
Your kindly invited to

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

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Accelerated stability, comparative

shelf life prediction for cosmetic

5.2. Comparative analysis

If the alteration rate is slower than the reference sample, then

This approach is robust as no mathematical extrapolations are

Face Make up (Liquid: liquid

Sun cream 2-3 years

For product development and improvement

Concentration at all positions at all times

NIR light source for almost all samples

Particle migration at gravity or in the

Particle migration at gravity Optical detection of

1. v -velocity at x=1 for gravity, x=6-2300 for accelerated tests

| Stability & shelf life | Particle Interactions |

2. Hydrodynamic density of particles (solid or liquid)

3. r Droplet size / Particle size distribution

4. Dynamic viscosity of continuous phase

Fingerprinting of transmission profiles

Droplet / Particle size,

By naked eye after 64 min at higher gravity

Evolution of transmission profiles during 3 min at higher gravity

Evolution of transmission profiles during 5 min at higher gravity

Evolution of transmission profiles during 10 min at higher gravity

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

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

Customers shelf life information:

Quantitative result (relative):

Quantitative result (absolute):

B is the more stable formulation than A.

Acceleration by higher gravity and by temperature allow for a fast

Multisampling approach in LUMiSizer / LUMiFuge instruments

The large variety of cosmetic formulations (chemical

1.Particle properties of micro- and

ISO 13317-1 ISO 13318

2. After Shave Balms, Creams, Leather

Multi-wavelength Stability Analyser Multi-wavelength

3. Sediment concentration profiles,

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

Your kindly invited to

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