particle characterization in the cosmetics industry · 2010. 4. 15. · microsoft powerpoint -...

© 2010 HORIBA, Ltd. All rights reserved.

Particle Characterization in the Cosmetics Industry

Mark [email protected]


Particles in CosmeticsAny product containing a powderPigments, talc, micaEmulsions (creams, lotions)Liposomes; simple, complexTypes of cosmetics containing particles (emulsion droplets)


Original Foundation: Pan-Cake

Foundation and powder in oneBase was talc (particle), not oil or waxApplied with wet spongePatent in 1937By 1940 1 in 3 N American women owned & wore Pan-Cake


Create our Own Product

BaseTalc, rice powder

PigmentIron oxide

FillerClay

GlitterMica

SPFTiO2

They’re allparticles!

Can measuresize of allusing one system:LA-950


Measuring Powders as Powders

•Direct flow ofpowder to cell

•0 to 4 bar•Report P used•Feedback to control powder flow

Add powder to vibrating tray, flows through cell where measurement made. Quick, easy, no glassware to clean.

LA-950


Base: Rice Powder


Iron Oxide – 170 Shade

LA-950 wet accessoriesDisperse powder into a liquidCan measure down to 30 nm

Use ultrasound?


Gold Glitter Powder

Wet Dry

Measure wet + dry, choose preferredVerify correct P for dry powder feeder


Gold Glitter Image Analysis

Optics

Powder Disperser


Shape ParametersISO 9276-6:2008 :Representation of results of particle size analysis –Part 6: Descriptive and quantitative representation of particle shape and morphology

Meso-shape descriptors

How round?Circularity: C = 4 π A

P2Aspect ratio?AR = xFmin/xFmaxnot for very elongated

Convexity = Pc/PPc = convex hull perimeter


Mica


Kaolin Clay

Note: small % below 100 nm, making thisa “nanoparticle.Safety concerns?


Sunscreen: TiO2

Powder dispersed inwater using surfactantand ultrasound.Note: 14.5% < 100nmSafety concerns?


Sunscreen w/ZnO

Note: %< 100nm depends on sample treatment (ultrasound)


Sunscreen: ZnO


Nanoparticle Safety: Cosmetics

“Preliminary scientific research has shown that many types of nanoparticles can be toxic to human tissue and cell cultures…”Suggests banning all cosmetics with particles <100nmMany sunscreens contain ZnO or TiO2 particles <100 nm


Nanoparticle Safety

NGO Friends of the Earth issue report requesting ban on all skin care products w/particles <100nmClaim: some nano-articles are dangerous, so ban allIndustry claims some nano-particles are safe, so don’t worryFDA says we only believe data in peer reviewed journals, but form task force to investigateIn 2012 Cosmetics manufactures must notify European Commission of any “nanoscale materials” in products


Nanoparticle or Not?

SSA = 6/ρD

50 nm

D from SEM ~50 nmD from SSA ~60-70 nmD from DLS ~250 nm(light scattering due toBrownian motion)So: is this a nanoparticle?

ultrasound

Used ultrasound to disperseto primary particles or useweak acid to break bondsD from DLS ~50 nm


Acoustics: ZnO Study

POWDER Name, Manufacturer

Median size, microns

Cum % of nano-particles <100 nm

Zinc oxide, 99.5+% by AcrosOrganics

0.273±0.01 11.0±1.4

Zinc oxide, reagent ACS byAcros Organics

0.430±0.02 7.0±0.5

Z50-500 USP powderpackaged by Fisher Scientific

0.561±0.017 2.7±0.39

Z52-500 USP powderpackaged by Fisher Scientific

0.660±0.037 1.9±0.4

S80249 by Fisher Scientific 0.398 ± 0.001 6.1±0.2Zinc oxide ACS reagent gradeby MO Biomedicals, LLC

0.349±0.017 8.2±2.1

Zinc oxide Polystormor byMallinckrodt Chemicals

0.223±0.009 19.6±1.8

Zinc oxide Nanopowder byAmerican Elements

0.631±0.1 4.7±2.5

Base

Dopant



0.0

0.2

0.4

0.6

0.8

1.0

1.2

PSD

, we i

ght b

asis

10-2 10-1 100 101

Diameter [um]

Zinc oxide, reagent ACS by Acros OrganicsZinc oxide, 99.5+% Acros OrganicsZ50-500 USPZ52-500 USPS80249 by Fisher ScientificZinc oxide 99.99% by Alfa AesarZinc oxide ACS MO Biomedicals, LLCPolystormorTM by Mallinckrodt ChemicalsNanopowder America Elements



0

1

2

3

4

5

6

7

8

Att

enu a

tion

[ dB

/cm

/MH

z]

100 101 102

Frequency [MHz]

zinc oxide A in solvent

zinc oxide B in water

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

P SD

, wei

ght b

asis

0

20

40

60

80

100

n ano

-pa r

ticle

s ran

g e10-2 10-1 100 101

Diameter [um]

zinc oxide Bzinc oxide A



1

2

3

4

5

6

7

% n

ano-

par t

icle

s, m

easu

red

1 2 3 4 5 6% nano-particles, estimated

Percentage of nano particles in Z52-500 sample after incremental additions of the Mallinckrodt Chemicals sample. The X-axis is a percentage calculated from the known amount of the added Mallinckrodt sample, assuming that it contains 20% on nano-particles, according to the Table 1. The Y-axis is a percentage calculated from the attenuation spectra, which is measured for the mixture.


DT-1201 Hardwaresample


Piezo crystal Electrodes

A

ColloidVibrationCurrent

CVI C Pp m

md=

−∇

ρ ρρ

ϕμ

msmp

smspomd K

Kρρρρρρ

ηςεε

μ)()(

Mobility..Dynamic

−

−=

Zeta Potential Probe

Electroacoustics – Zeta Potential


Zeta Potential

If surface has + charge, then - ions attracted to surface+ ions attracted to – ions, builds electric double layerSlipping plane: distance from particle surface where ions move with particleZP = potential (mV) at slipping plane


Stability

Want stable dispersionEither suspensions or emulsionsSuspensions sediment & flocculateEmulsions phase separate, creaming or coalescence

good

bad

good

bad


StabilizationSteric stabilization: coat surface with polymersParticles can’t touch so they don’t interactElectrostatic stabilization: alter surface chemistry to put charge on particle surfaceRepel like magnets


pH Titration of Rutile 7%vl & Alumina 4%vl

85 nm

300 nm

PSD unstable @ IEPaggregates form


Skin CreamEmulsion w/SPF 15


Emulsion Stability

Greater zeta potential Add surfactant toStabilize emulsionTest zeta potentialVs. surfactant conc.


Emulsions

Creams: semi-solid emulsions, mixtures of oil & waterOintment : viscous semisolid preparation used topically

Vehicle of an ointment is known as ointment base Hydrocarbon bases e.g. hard paraffin, soft paraffinAbsorption bases e.g. wool fat, beeswaxWater soluble bases e.g. macrogols 200, 300, 400Emulsifying bases e.g. emulsifying wax, cetrimideVegetable oils e.g. olive oil, arachis oil, coconut oil


Emulsions

Liniment, (or embrocation) is a medicated topical preparation for application to the skin. Preparations of this type are also called balm.

Liniments are of a similar viscosity to lotions (being significantly less viscous than an ointment or cream) but unlike a lotion a liniment is applied with friction; always rubbed in. Liniments are typically sold to relieve pain and stiffness

Paste: substance that behaves as a solid until a sufficiently large load or stress is applied, at which point it flows like a fluid.


Cosmetic Emulsion Patent

Collected with HORIBA LB-500LB-550

Microemulsions areTransparent & thermodynamicallystable, <150 nm


Liposomes


Liposome DeliveryActiveingredient

Liposome approachesskin barrier layer

Liposome fuses withskin barrier layer

Liposome dissolves &releases actives(retinol?)

Penetrates into skin


Liposomes by DLS

Liposome size after 5 passes through

100 mm membrane, mean size ~ 250 nm

Liposome size after 20 passes through

100 mm membrane, mean size ~ 150 nm

www.horiba.com/us/en/scientific/products/particle-characterization/


Retinol Formulation - Delivery

“Retinal contained in the core spaceof the vesicle which has a meandiameter of 10~50nm”…


SummaryMany cosmetic products either powder (particle) based, or contain powdersWide range measured by laser diffraction (LA-950)Image analysis provides additional shape informationAcoustics measures size & zeta potential with no dilutionDLS for sub-micron size + dilute zeta potential


For More DetailsVisit horiba.comApplication Notes:

AN152 Measuring Emulsions using AcousticsAN161 Particle Size Analysis of CosmeticsAN171 Measuring Nanoparticles using AcousticsAN174 Measuring Liposomes using DLS

Webinars:State of the Art Laser Diffraction PerformanceThe DT Series Acoustic SpectrometersSize and Stability for Biotech and Nanotech

particle characterization in the cosmetics industry · 2010. 4. 15. · microsoft powerpoint -...

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