stability of the cosmetics

© 2015 LUM GmbH

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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

Accelerated stability, comparative shelf life prediction for cosmetic products, in-cosmetics 2015 www.lum-gmbh.com

© 2015 LUM GmbH

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ISO/TR 13097:2013 Guidelines for the characterization of dispersion stability

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Table of contents Foreword Introduction 1 Scope 2 Terms and definitions 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

http://www.iso.org/iso/home/store/catalogue_tc/catalogue_detail.htm?csnumber=52802


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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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ISO/TR 13097: 5. Prediction of shelf life


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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)

For product development and improvement fast and reliable information is required.

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&SubCategoryID=169 (22.2.2012)

Presenter

Presentation Notes

Shelf life information for hair care products is given by web sources with 6 months to 3 years, �a period too long for real-time analysis in research and development.�Direct and accelerated analysis is a must.


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Dispersions are beautiful and complex.

Creaming G

Ostwald ripening D

Phase Inversion D

Coalescence D [G]

Flocculation

Coagulation D [G]

Sedimentation G

G = Gravity driven

D = Diffusion driven

Presenter

Presentation Notes

Inks, paints, pigment dispersions may undergo different separation processes, sometimes in parallel, sometimes one after the�other. �Sedimentation and creaming can directly be physically accelerated. �Some diffusion driven processes can be accelerated by increasing the temperature. Different LUM instruments support your specific application.

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products


1. Introduction 2. Technology

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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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Presentation Notes

With STEP technology you always know what happens in all parts of your sample from to to bottom at any time. Complex multi-component formulations, as common in paints and inks, �often show more than one separation process, so you do not lose any information applying STEP.


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STEP-Technology® in LUMiFuge® / LUMiSizer®

Light

Sample

Sensor

Transmission

kinetics Multisample analysis (up to 12 simultaneously).

Acceleration by temperature 4°C to 60°C.

Multi-wavelength.

Physical acceleration from 6 x to 2300 x

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Presentation Notes

STEP technology as applied in LUMiFuge and LUMiSizer is important for the measurement of inks, paints, pigment dispersion products. The combination of STEP technology with multisample analytical centrifugation allows the characterization of �high and low concentrated products, of high and low viscosity, in their original concentration.�It is done in the temperature range from +4°C to +60°C, relevant for formulation, transport, storage and application of products. The acceleration from 6 up to 2300 times gravity provides results much faster than any real-time measurement.


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STEP-Technology® in LUMiFuge® / LUMiSizer®

Presenter

Presentation Notes

STEP technology as applied in LUMiFuge and LUMiSizer is important for the measurement of inks, paints, pigment dispersion products. The combination of STEP technology with multisample analytical centrifugation allows the characterization of �high and low concentrated products, of high and low viscosity, in their original concentration.�It is done in the temperature range from +4°C to +60°C, relevant for formulation, transport, storage and application of products. The acceleration from 6 up to 2300 times gravity provides results much faster than any real-time measurement.


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How can we use STEP-Technology®?

Particle migration at gravity or in the accelerated measurement

Stokes‘ Law: v = . f(α) . xg 2 ∆ρ . r2

9 η v – Particle velocity ρ – Density η – dyn. Viscosity of cont. phase r2 – Particle size α – Particle concentration xg – „real-time or accelerated“ -Physical acceleration


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Optical detection of particle concentration

I IO

- ln = E = ε . α . d ε = f (λ, r, n, ...)

d

IO

I

Lambert-Beer‘s Law:

How can we use STEP-Technology®?

I0 – Light factor | light intensity ε – Extinction coefficient d – optical path length (cell thickness) NIR, blue & further wavelength)

Particle migration at gravity or in the accelerated measurement

Stokes‘ Law: v = . f(α) . xg 2 ∆ρ . r2

9 η

v – Particle velocity ρ – Density η – dyn. Viscosity of cont. phase r2 – Particle size α – Particle concentration xg – „real-time or accelerated“


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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. ρ – Hydrodynamic density of particles (solid or liquid) in liquid continuous phase

3. r – Droplet size / Particle size distribution

4. η – Dynamic viscosity of continuous phase

Presenter

Presentation Notes

Applying Stokes Law different material parameters can be obtained.


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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

Presenter

Presentation Notes

A simple qualitative sample comparison is done by evaluation of the transmission fingerprints, either step-by-step or all at once.�The quantitative instability index provides you with a quality control parameter for your formulation. �The detailed separation kinetics with separation velocities and separated phase volume provides more detailed information for R&D. �Particle size, separation velocity and density distributions characterize components of formulations.

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products


1. Introduction 2. Technology 3. Cosmetic o/w-emulsion

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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 50°C).

• Acceleration by temperature 50°C – identical to one of customer‘s 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.

Presenter

Presentation Notes

The instability index is the control value for make up at a time (here 2 h) for a given relative centrifugal acceleration (here RCA 1910 g).�It is used for comparison of samples of the same type under identical conditions and allows to say which is the most instable sample�with the highest index value (here make up 2 from producer P1) and the most stable sampe (here products from producer P2).


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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 50°C.

A B

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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 50°C

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

*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

Customer‘s 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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CONCLUSION

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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…

Multi-wavelength Separation Analyser LUMiReader®PSA

ISO 13317-1

1.Particle properties of micro- and nanoparticles

Multi-wavelength Dispersion Analyser LUMiSizer®

ISO 13318

MICROPARTICLES NANOPARTICLES

Presenter

Presentation Notes

Product portfolio of LUM GmbH related to particle characterization for HPC and pharmaceutical industries (March 2013).


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…via Dispersion Stability of…

Multi-wavelength LUMiReader®PSA

2. After Shave Balms, Creams, Leather Gels, Liposomes, Make up, Nail Varnish, Shampoo, Softener, Sun Care, Tooth Paste…

Multi-wavelength LUMiSizer®

Real-Time Direct and Accelerated

Stability Analyser LUMiFuge®

1. Particles ISO/TR 13097


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…to Properties of Separated Phases

Separation Analyser LUMiReader® X-ray

ISO/TR 13097

1. Particles

3. Sediment concentration profiles, cream layer properties after accelerated separation

2. After Shave Balms, Creams, Leather Gels, Make up, Nail Varnish, Shampoo, Softener, Sun Care, Tooth Paste…

Presenter

Presentation Notes

Product portfolio of LUM GmbH for characterization of Coatings (March 2013).


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More information: The formulation of a distinctive skin care product

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

Prediction of Emulsion Stability: Facts and Myths V. André, N. Willenbacher, H. Debus, L. Böger, P. Fernandez, T. Frechen, J. Rieger, Cosmetics and Toiletries Manufacture Worldwide, 2003, 102-109.

Accelerated Stability Testing of W/O Creams A. Brämer, 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

Presenter

Presentation Notes

Now see the detailed application presentation.

http://www.lum-gmbh.com/Literature_Database.html


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Thank you for your attention.

Your kindly invited to meet us at Stand 6C60 and ...

Presenter

Presentation Notes

Now see the detailed application presentation.

stability of the cosmetics

Documents

product shelf life

basics of stability

stability summary

stability criteria

stability data

typical shelf life

comparative analysis

accelerated analysis