Performance Characterization of Natural...

F L O R A T E C H T I F F A N Y O L I P H A N T , M S

M A R C H 2 0 , 2 0 1 7

Performance Characterization of Natural Ingredients Compared to

Silicone and Quaternium Compounds in Hair Care

Applications

© Copyright 2017 International Flora Technologies, Ltd., All Rights Reserved Floratech Proprietary & Confidential

1

Outline

Introduction Functions of silicones and quats, how they work, and formulation

issues

Possible replacements for silicones and quats Comparative studies Floraesters K-100® Jojoba / Floraesters K-20W® Jojoba versus quats Floramac® 10 versus silicones

Conclusions


2

Functions of Conditioning Agents

Enhance mildness (of shampoo formulations) Provide ease of wet combing / provide lubricity Increase hair softness Increase hair shine Make hair more manageable Prevent buildup of static electricity Leave hair silky and smooth / lay down cuticles Protection against thermal and mechanical damage Hair dye color protection


3

How Conditioning Agents Work

Deposition Coating the porous, hydrophilic damaged hair Adsorb hydrophilic head down, hydrophobic tail up Confer hydrophobicity to hair Durability during several wash cycles


4

Commonly Used Quat Conditioning Agents

Cationic Surfactants and Polymers Cetrimonium Chloride Quaternium-80 Hydroxypropyltrimonium Hydrolyzed Wheat Protein Polyquaternium compounds Silicone quaternium compounds


5

Commonly Used Silicone Conditioning Agents

Cyclopentasiloxane Phenyl Trimethicone Dimethicone (various viscosities) Amodimethicone Fluids Silicone Polyethers


6

Issues with Cationic Conditioning Agents

Silicones De-foamers Silicones are incompatible with typical ingredients used in

shampoos Large amounts of silicones are necessary in rinse-out products

to ensure deposition Particularly reduced deposition profile in dyed hair

Silicone droplet size makes clear formulations difficult Silicones are undesirable by consumers


7

Issues with Cationic Conditioning Agents

Quats Allergens Phenolic quats are considered endocrine disrupters

Both Must be formulated in such a way to induce phase separation

during rinsing so it doesn’t wash off (particularly in shampoos) Build up on hair Negative connotation by consumers as not natural Toxicity to aquatic life


8

Products That Use Conditioning Agents

Shampoos 2-in-1 shampoos

Conditioners Leave-on and rinse-out

Hair Serums Hair Masks Hair Styling Products Shine Sprays

9

Emollients Emollient Derivatives

Jojoba Oil Macadamia Oil Sunflower Oil Olive Oil Isododecane Isononyl Isononanoate Coco Caprylate South Pacific Monoi Oil Pentaclethra Macroloba

Seed Oil

Floraesters K-100 Jojoba Floraesters K-20W Jojoba Floramac 10 Derivatives of Sunflower

Oil Derivatives of Olive Oil Hydrogenated Methyl

Abietate

Possible Replacements For Quats & Silicones

10

Derived from Jojoba Oil Naturally-derived

(Ecocert / COSMOS certified)

Film forming / water resistant

High oxidative stability Oil-free / preservative-

free

Non-greasy feel Low odor & color Renewable resource TGA approved EU & China REACh

compliant Low usage levels

Floraesters K-100 / K-20W Jojoba


11

Hydrolyzed Jojoba Esters: The Chemistry

O

O

O

O-K+ HO

KOH + H2O

Potassium Jojobate Jojoba Alcohols Hydrolyzed Jojoba Esters

[Floraesters K-20W Jojoba]: 20% Hydrolyzed Jojoba Esters + 80% Water (Aqua) [Floraesters K-100 Jojoba]: 80% Hydrolyzed Jojoba Esters + 10% Jojoba Esters + 10% Water (Aqua)

Jojoba Oil

*All of the above structures are trans-free.


12

Hair Care Study Details

Blind Vehicle-controlled Controlled environmental conditions


13

Deposition of Hydrolyzed Jojoba Esters

Objective: Evaluate Hydrolyzed Jojoba Esters at 1% in water for its

potential to remain deposited on hair after rinse-out Methodology: Extraction and HPLC analysis for Hydrolyzed Jojoba

Esters after application and rinse of 1% solution N = 3 tresses

Results: 4.7% ± 2.7% (~30% of Floraesters K-20W Jojoba)

of the Hydrolyzed Jojoba Esters applied to hair tresses remained on the hair after rinse-out


14

Hair Care Study: Comb Force

Objective: Evaluate shampoos and conditioners with and without

Floraesters K-20W Jojoba and Floraesters K-100 Jojoba, respectively, for their potential to reduce wet comb force alone, compared to, and in conjunction with quats

Methodology: Comb force evaluations [via Test Resources Q Series

(100Q) Universal Testing Machine] were conducted before and after treatment with a shampoo or rinse-out conditioner

N = 8 tresses per product


15

Formula 1: Natural Shampoo & Conditioner

Vehicle Shampoo (%wt/wt): Water (q.s.), Disodium Laureth Sulfosuccinate (12.0%), Decyl Glucoside (8.0%), Sodium Lauroyl Sarcosinate (8.0%), Cocamidopropyl Betaine (8.0%), Acrylates Copolymer (3.0%), Methyl Glucose Caprate / Caprylate / Oleate (and) Propanediol (2.0%), Sodium Cocoyl Isethionate (2.0%), Glycol Distearate (1.5%), Phenoxyethanol (and) Caprylyl Glycol (and) Ethylhexylglycerin (and) Hexylene Glycol (0.8%), Guar Hydroxypropyltrimonium Chloride (0.7%), Fragrance (0.7%), Aminomethyl Propanol (0.4%), and Disodium EDTA (0.1%).

Vehicle Conditioner (%wt/wt): Water (q.s.), Glyceryl Stearate (and) Cetearyl Alcohol

(and) Sodium Stearoyl Lactylate (6.0%), Cetyl Alcohol (2.0%), Propanediol (1.0%), Polyglyceryl-2 Stearate (1.0%), Ethylhexyl Methoxycinnamate (and) BHT (1.0%), Theobroma Grandiflorum Seed Butter (and) Tocopherol (1.0%), Prunus Amygdalus Dulcis (Sweet Almond) Oil (1.0%), Ethyl Macadamiate (1.0%), Phenoxyethanol (and) Caprylyl Glycol (and) Ethylhexylglycerin (and) Hexylene Glycol (0.8%), Fragrance (0.5%), Tocopheryl Acetate (0.5%), Hydroxyethylcellulose (0.1%), and Disodium EDTA (0.1%).


16

Reduced Comb Force: Shampoo

Conclusion: 2.5% Floraesters K-20W Jojoba produced statistically significant decreases in comb force (p<0.05) from baseline, and directionally significant decreases in comb force (p<0.10) over the vehicle shampoo.

Wet Comb Force

0%

10%

20%

30%

40%

50%

60%

Perc

entR

educ

tion

inPe

akW

etCo

mb

Forc

e

A

B

B - vehicle shampooA - vehicle shampoo + 2.5% FloraestersK-20W Jojoba


17

Reduced Comb Force: Rinse-Out Conditioner

Conclusion: 1% Floraesters K-100 Jojoba produced statistically significant decreases in comb force (p<0.05) compared to the vehicle conditioner and baseline.

Wet Comb Force

0%

10%

20%

30%

40%

50%

60%

Perc

entR

educ

tion

inPe

akW

etCo

mb

Forc

e

A

B

B - vehicle conditionerA - vehicle conditioner+ 1% FloraestersK-100 Jojoba


18

Formula 2: Traditional

Vehicle Conditioner (%wt/wt): Water (q.s.), Glyceryl Stearate (and) Cetearyl Alcohol (and) Sodium Stearoyl Lactylate (4.0%), Cetyl Alcohol (3.0%), Propanediol (1.0%), Polyglyceryl-2 Stearate (1.0%), Ethylhexyl Methoxycinnamate (and) BHT (1.0%), Moringa Oil/Hydrogenated Moringa Oil Esters (1.0%), Macadamia Integrifolia Seed Oil (1.0%), Ethyl Macadamiate (1.0%), Phenoxyethanol (and) Decylene Glycol (and) Propylene Glycol (0.8%), Fragrance (0.5%), Tocopheryl Acetate (0.5%), Niacinamide (0.3%) Hydroxyethylcellulose (0.1%), Disodium EDTA (0.1%), Pyridoxine Hydrochloride (0.1%), and Citric Acid (0.1%).


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Conclusion: 1% Floraesters K-100 Jojoba and 1% Cetrimonium Chloride both produced statistically significant decreases in comb force (p<0.05) compared to the vehicle conditioner, the conditioner containing Hydrolyzed Wheat Protein, and baseline. 0%

10%

20%

30%

40%

50%

Perc

ent

Redu

ctio

n in

Peak

Wet

Com

bFo

rce

B

D

C

A

E

Wet Comb Force

D - vehicle + 1% Cetrimonium ChlorideC - vehicle + 1% Quaternium-80B - vehicle + 1% Hydrolyzed Wheat ProteinA - vehicle

E - vehicle + 1% FloraestersK-100 Jojoba


20


Conclusion: The addition of 1% Floraesters K-100 Jojoba produced statistically significant decreases in comb force (p<0.05) compared to each respective vehicle conditioner with quats and baseline.

0%

10%

20%

30%

40%

50%

60%

Perc

ent

Redu

ctio

n in

Peak

Wet

Com

bFo

rce

B

E

D

C

A

G

F

Wet Comb Force

E - vehicle + 1% Quaternium-80 + 1% FloraestersK-100 JojobaD - vehicle + 1% Quaternium-80C - vehicle + 1% Hydrolyzed Wheat Protein + 1% FloraestersK-100 JojobaB - vehicle + 1% Hydrolyzed Wheat ProteinA - vehicle

G - vehicle + 1% Cetrimonium Chloride + 1% FloraestersK-100 JojobaF - vehicle + 1% Cetrimonium Chloride


21

Hair Care Study: Frizz

Objective: Evaluate conditioners with and without Floraesters K-100

Jojoba for their potential to reduce frizz

Methodology: Frizz was analyzed before and after exposure to high

humidity (>70%) 1 product application / rinse N = 3 tresses per product


22

Conclusion: 1% Floraesters K-100 Jojoba produced 30% less frizz when compared to the vehicle conditioner.

vehicle conditioner

vehicle conditioner + 1% Floraesters K-100 Jojoba

Reduced Hair Frizz: Rinse-Out Conditioner


23

Hair Care Study: Heat Protection

Objective: Evaluate conditioners with and without Floraesters K-100

Jojoba for their potential to provide heat protection and reduce hair breakage

Methodology: Hair breakage was analyzed before and after exposure to high

heat + reversion (100 passes with a flat iron at 450°F + 4 hours at >75% humidity)

1 product application / rinse N = 9 tresses per product


24

Increased Heat Protection: Rinse-Out Conditioner

Breakage

Mean ± SE

Mean ± SD

Conclusion: 1% Floraesters K-100 Jojoba produced 38% fewer broken hair fibers after heat exposure when compared to the vehicle conditioner.

**Indicates statistical significance (p<0.05) between test articles. *Indicates statistical significance (p<0.05) between test article and control.

0

20

40

60

80

100

120

140

160

180

vehicleconditioner

vehicleconditioner+ 1%K-100

heat+ reversion

# of

bro

ken

fiber

s

*

**


25

Hair Care Study: Color Protection

Objective: Evaluate shampoos and conditioners with and without

Floraesters K-20W Jojoba and Floraesters K-100 Jojoba, respectively, for their potential to provide color protection

Methodology: Wool swatches were dyed with commercial red or brown

permanent hair dyes N = 3 wool swatches per product Color (ΔE, Colorimeter) was analyzed initially and every 2

treatments + rinses with the products


26

Color Protection: Shampoo

Conclusion: 2.5% Floraesters K-20W Jojoba retained up to 35% more color when compared to the vehicle shampoo.

Color Retention

*Indicates statistical significance (p<0.05) between test articles.

0

5

10

15

20

ΔE

incr

easi

ngco

lor l

oss

8642# of wash / rinse treatment cycles

+10%

C

D

+35%

A

B*

*

**

D - vehicle shampoo + 2.5% K-20W (brown)C - vehicle shampoo (brown)

B - vehicle shampoo + 2.5% K-20W (red)

A - vehicle shampoo (red)


27

Color Protection: Rinse-Out Conditioner

Conclusion: 1% Floraesters K-100 Jojoba retained up to 22% more color when compared to the vehicle conditioner.

Color Retention

*Indicates statistical significance (p<0.05) between test articles.

0

5

10

15

20

ΔE

incr

easi

ngco

lor l

oss

8642# of wash / rinse treatment cycles

+13%

C

D

+22%

A

B*

*

*

*

D - vehicle conditioner + 1% K-100 (brown)C - vehicle conditioner (brown)

B - vehicle conditioner + 1% K-100 (red)

A - vehicle conditioner (red)


28

Hair Care Study: Consumer Preference

Objective: Determine the consumer perception of Floraesters K-100 Jojoba

in a conditioner

Methodology: N = 29 healthy female participants 1 application of each product to (N=3) hair tresses used for

consumer evaluation Consumer Preference Survey


29

Improved Consumer Preference: Rinse-Out Conditioner

Consumer Preference

Statistical (**) and directional (*) significance was apparent where indicated (p<0.05 and p<0.1, respectively).

Conclusion: Consumers preferred hair tresses treated with a conditioner containing 1% Floraesters K-100 Jojoba compared to hair tresses treated with the vehicle conditioner.

20%

40%

60%

80%

100%Hair Moisturization*

Hair Smoothness / Sleekness *

Hair Volume*

Hair Softness(Visual)*

Hair Softness (Feel)* Hair Shine*

Healthy Appearance of Hair*

FrizzManagement*

Non-Greasy to Touch

Pleasant to Touch*

Overall Product Performance*

vehicle conditionervehicle conditioner + 1%K-100

30

High oxidative stability Oil-free / preservative-

free Non-volatile silicone

alternative Non-greasy feel Derived from

macadamia oil

Low odor & color Renewable resource TGA approved EU & China REACh

compliant

Floramac 10 (INCI: Ethyl Macadamiate)


31

Formula 3: Leave-In Hair Serum

Vehicle Hair Serum (%wt/wt): Test Emollient (q.s.), Glyceryl Tribehenate/Isostearate/Eicosadioate (10.0%), Polyglyceryl-3 Beeswax (2.7%), and Phenoxyethanol (0.6%).


32

Hair Care Study: Comb Force

Objective: Evaluate leave-in hair serums with and without

Floramac 10 for their potential to reduce wet and dry comb force compared to silicones

Methodology: Comb force evaluations [via Test Resources Q Series

(100Q) Universal Testing Machine] were conducted before and after treatment with a leave-in hair serum



33

Reduced Comb Force: Leave-In Hair Serum

Conclusion: The inclusion of Floramac 10 resulted in statistically significant (p<0.05) decreases in wet comb force compared to Phenyl Trimethicone; and statistically significant (p<0.05) decreases in dry comb force compared to Phenyl Trimethicone and Cyclopentasiloxane.

*All products resulted in statistically significant (p<0.05) changes in wet and dry comb force from baseline.

-60%

-40%

-20%

0%

20%

40%

60%

80%

100%

DryComb Force

WetComb Force

Perc

entR

educ

tion

inCo

mb

Forc

e

A

A

B

B

C

C

Comb Force

C - Phenyl TrimethiconeB - CyclopentasiloxaneA - Floramac 10


34

Hair Care Study: Shine

Objective: Evaluate leave-in hair serums with and without

Floramac 10 for their potential to increase shine compared to silicones

Methodology: Shine measurements (via Glossymeter) were conducted

on dry hair before and after treatment with a leave-in hair serum with and without heat



35

Increased Shine: Leave-In Hair Serum

Conclusion: The inclusion of Floramac 10 and Phenyl Trimethicone resulted in statistically significant (p<0.05) increases in hair shine compared to Cyclopentasiloxane without heat. Floramac 10 resulted in statistically significant (p<0.05) increases in hair shine compared to Phenyl Trimethicone and Cyclopentasiloxane.

-40%

-20%

0%

20%

40%

60%

80%

With Heat

No Heat

Perc

ent C

hang

e in

Hai

r Shi

ne(re

lativ

eto

unt

reat

ed h

air) A

A

B

BC

C

{

{

Hair Shine



36

Hair Care Study: Breakage

Objective: Evaluate leave-in hair serums with and without Floramac

10 for their potential to reduce hair breakage compared to silicones

Methodology: Broken fibers counted after controlled, repeat combing

(1000 comb strokes) N = 6 tresses per product


37

Reduced Hair Breakage: Leave-In Hair Serum

Conclusion: The inclusion of Floramac 10 resulted in statistically significant (p<0.05) fewer broken hair fibers compared to Phenyl Trimethicone.

0

10

20

30

40

50

60

# of

bro

ken

hair

fiber

s

A

C

B

Hair Breakage



38

Hair Care Study: Consumer Preference

Objective: Determine the consumer perception of Floramac 10 in a leave-

in hair serum compared to Phenyl Trimethicone

Methodology: N = 24 healthy female participants Split head study Every other day use for 1 week Consumer Preference Survey


39

Improved Consumer Preference: Leave-In Hair Serum

Consumer Preference

Statistical (**) and directional (*) significance was apparent where indicated (p<0.05 and p<0.1, respectively).

Conclusion: Consumers preferred a leave-in hair serum containing Floramac 10 compared to a leave-in hair serum containing Phenyl Trimethicone.

20%

40%

60%

80%

100%

Ease of Combing*

Hair Strength*

Softness*

Silky

Shine**

Healthy Looking**

Smoothness**

Overall Product Performance

Phenyl TrimethiconeFloramac 10


40

Conclusions

Floraesters K-20W/K-100 Jojoba and Floramac 10 have beneficial effects within multiple hair care applications, including: Comb force reductions Frizz reductions Heat protection Breakage reductions Increases in hair shine Increase in consumer preference

Floraesters K-20W/K-100 Jojoba and Floramac 10 offer an effective alternative to quats and silicones in hair care


41

References

Colorimeter CL 400 and Glossymeter GL 200 are products of Courage+Khazaka (Köln, Germany).

Test Resources Q Series (100Q) Universal Testing Machine is a product of TestResources, Inc. (Shakopee, MN).

ΔE = √ [(L*2-L*1)2 +(a*2-a*1) 2 +(b*2-b*1) 2] Evans T and Wickett RR, eds. Practical Modern Hair Science.

Carol Stream, IL: Allured Business Media. 2012. Print. Johnson B, Murphy K, and Lin F, Silicones continue to shape

the hair care industry. Personal Care. November 2015; 29-31. http://chemicaloftheday.squarespace.com/most-

controversial/2011/8/31/quaternary-ammonium-compounds.html

http://chemicaloftheday.squarespace.com/most-controversial/2011/8/31/quaternary-ammonium-compounds.html



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