Nature-Identical Preservatives On The MoveTrend scouting with help from Mintel shows that phenoxyethanol remains as the main preservative system in skin care, soap and bath products. There is a major transition, however, toward nature-identical organic acids like benzoic acid/sodium benzoate and Dehydroacetic Acid (DHA). Globally, DHA is currently ranked as one of the top 14 with 20% increased use from 2013 to 2014.

This edition of the Ashland preservatives newsletter is dedicated to a “new to the world” preservative technology that answers the global trend toward nature-identical and cost-eff ective preservation.

Industrial Biocides Divested

Ashland recently announced that it has agreed to sell the industrial biocides business within Ashland Specialty Ingredients to Troy Corporation, a global leader in microbial control products and performance additives.

Industrial biocides are used to help control and prevent the growth of bacteria, mold and other microorganisms in a wide range of coatings, construction materials and energy products.

Ashland’s lineup of preservative products, used in a wide variety of personal care products in consumer markets, is excluded from the Troy agreement. Ashland remains committed to the further development and growth of its preservatives business.

Disclaimer : Ashland Inc. and its subsidiaries (“Ashland”) believe that all information provided with respect to its products is accurate at the time such information is provided. All statements, information, and data presented herein are believed to be accurate and reliable, but are not to be taken as a guarantee, an express warranty, or an implied warranty of merchantability or fi tness for a particular purpose, or rep-resentation, express or implied, for which Ashland assumes legal responsibility. They are off ered solely for your consider-ation, investigation, and verifi cation. All recommendations or suggestions contained herein must be evaluated by the user to determine their applicability or suitability for a particular application. Users are encouraged to read and understand the Material Safety Data Sheet (MSDS) and to abide by all use and safety recommendations detailed therein and on all product labeling. No freedom to use any patent owned by Ashland is to be inferred.

Skin Care, Soap and Bath Products - Mintel Data

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Preservatives NewsletterAshland Consumer Specialties

Customer EditionJune 2015

ContentsClick on the item toread the article

Nature-Identical Preservatives On The Move

Optiphen™ P Preservative Platform

Web-based Preservatives Selector Tool

Regulatory Update

Preservatives Highlightedin this Issue

We appreciate yourinput and opinion.Please rate thisnewsletter by clickingthe question mark.

With good chemistry great things happen.™

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Preservatives Newsletter (Customer Edition)

Optiphen™ P preservative Platform Companies are faced with market pressure to move away from certain preservative chemistries due to, new regulatory requirements and due to ever changing end-product formulation trends. Formulators are thus challenged to find a preservative system that fits all products and at the same time offers broad-spectrum protection. The formulators often look for preservatives that do not contain alcohol, parabens, isothiazolinone, halogens, or formaldehyde donors. Furthermore, formulators require progressive preservative systems that are cost-effective. The Optiphen P preservative technology platform was developed to address these needs and offer a solution for end-product preservation. This new to the world technology is based on an optimized delivery system that maximizes efficacy of the actives, which will have minimal impact on the rheological properties of end products.

Optiphen DP preservative is the first technology from this platform to be introduced to the market. This patent-pending delivery system boosts the performance of the active ingredients, with no or minimal interference or destabilization of the end product. The product provides comprehensive antimicrobial protection in both aqueous and emulsion-type formulations. Additionally, this preservative meets the growing consumer trend for natural products and conforms to the requirements for several eco-labels, including Bra Miljöval (Good Environmental Choice), Nordic Eco-labelling (Swan), and the EU Eco-label (Flower) 2014/893/EC.

Optiphen DP preservative is easy-to-use. The following examples indicate how Optiphen DP preservative performs well in wipes, shampoo, and lamellar gels.

Wipes: The addition of 1% Optiphen DP preservative showed excellent efficacy when combined with 0.3% of the booster, Optiphen OD preservative booster, in wipes systems. As shown in chart 1 baby wet wipes (pH 4.5 – 5.0) were inoculated with mixed microbial suspensions containing approximately 107 cfu/mL microorganisms. The wet wipes were stored at room temperature in the dark and the microbial load was evaluated after 7, 14, and 21 days after inoculation. No growth of bacteria, yeast or fungi was detected after 21 days of inoculation.

Chart 1: Baby Wipes Challenge Tests

Shampoos: A mild clear conditioning shampoo of the formula shown in Table I was prepared by dissolving the cocamidopropyl betaine and SLES in water, then adding the Ceraphyl™ 41 ester, C12 - 15 alkyl lactate, citric acid, sodium chloride and Optiphen DP preservative at 0.5% by wt. The system was then inoculated with microorganisms (bacteria, yeast and fungi) following the 28 day double inoculation test protocol. The microbial suspension contained about 105-6 cfu/g microorganisms. The inoculated product was stored at 30°C and the microbial load was evaluated after 7, 14 and 21 days after inoculation. After 21 days, the formulation was reinoculated with the same microorganisms at a similar strength. As shown in Chart 2, the shampoo passed the 28 day double inoculation tests with excellent preservation delivered by the 0.5% Optiphen DP preservative. Also shown in Chart 2, excellent preservation of the shampoo was obtained with already 0.5% Optiphen DP preservative. No yellowing of the system was detected.

June 2015

1.0E+00 1.0E+01 1.0E+02 1.0E+03 1.0E+04 1.0E+05 1.0E+06 1.0E+07

cfu/

g

Wet Wipe Unpreserved

Bacteria

Yeast

Fungi

1.0E+00

1.0E+01

1.0E+02

1.0E+03

1.0E+04

1.0E+05

1.0E+06

1.0E+07

Inoculation 7 d 14 d 21 d

cfu/

g

Wet Wipe with 1% Optiphen DP preservative + 0.3% Optiphen OD preservative booster

Bacteria Yeast Fungi

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Preservatives Newsletter (Customer Edition)

Table I – Mild Clear Conditioning Shampoo

Ingredients INCI Name %W/W Supplier

Deionized Water Water 75.41

Tego™ Betain C 60* Cocamidopropyl Betaine (46.4%) 6.50 Evonik

Emal™ 270th* Sodium Laureth Sulfate (70%) 13.00 KAO Chemicals

Ceraphyl 41 ester C12-15 Alkyl Lactate 1.00 Ashland

Citric Acid (25% Aq. Solution) Citric Acid 0.09

Sodium Chloride (25% Aq. Solution) Sodium Chloride 4.00

* Tradename owned by a third party.

Chart 2: Shampoo Challenge Test

Lamellar Gels: A lamellar gel with excellent skin care properties was prepared following directions in Table II. The system was then inoculated with microorganisms (bacteria, yeast and fungi) following the 28 day double inoculation tests described above. The addition of 1.6% Optiphen DP preservative was able to offer good protection to this system passing the 28 day double inoculation test without any yellowing development. (Chart 3).

June 2015

1.00E+00

1.00E+01

1.00E+02

1.00E+03

1.00E+04

1.00E+05

1.00E+06

1.00E+07

cfu/

g

Unpreserved Control

Bacteria

Yeast

Fungi

1.00E+00

1.00E+01

1.00E+02

1.00E+03

1.00E+04

1.00E+05

1.00E+06

cfu/

g

0.5% Optiphen DP preservative @ pH 5.3

Bacteria

Yeast

Fungi

1.00E+00

1.00E+01

1.00E+02

1.00E+03

1.00E+04

1.00E+05

1.00E+06

1.00E+07

cfu/

g

Unpreserved Control

Bacteria

Yeast

Fungi

1.00E+00

1.00E+01

1.00E+02

1.00E+03

1.00E+04

1.00E+05

1.00E+06 cf

u/g

0.5% Optiphen DP preservative @ pH 5.3

Bacteria

Yeast

Fungi

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Preservatives Newsletter (Customer Edition) June 2015

Table II – Lamellar Gel

Ingredients INCI Name %W/W Supplier

Phase A

Deionized Water Water 77.23

Versene™ 220 Crystals* Tetrasodium EDTA 0.07 Dow

Glycerin Glycerin 5.00 RITA

TEA Triethanolamine 0.05 Ruger

UltraThix™ P-100 polymer Acrylic Acid/VP Crosspolymer 0.50 Ashland

Phase B

ProLipid™ 141 lamellar gel

Glyceryl Stearate (and) Behenyl Alcohol (and) Palmitic Acid (and) Stearic Acid (and) Lecithin (and) Lauryl Alcohol (and) Myristyl Alcohol (and) Cetyl Alcohol

4.50 Ashland

Ceraphyl™ 847 ester Octyldodecyl Stearoyl Stearate 4.00 Ashland

Ceraphyl 424 ester Myristyl Myristate and Myristyl Laurate 2.00 Ashland

Ceraphyl 494 ester Isocetyl Stearate 3.00 Ashland

Belsil™ DM 100* Dimethicone 1.00 Wacker

Emulsynt™ GDL emulsifi er Glyceryl Dilaurate 1.00 Ashland

Phase C

Vital™ ET biofunctional Disodium Lauriminodipropionate Tocopheryl Phosphates 1.50 Ashland

TEA Triethanolamine 0.15 Ruger

Total 100.00

* Trademark owned by a third party.

Procedure 1. Add Phase A ingredients in the water.2. Disperse UltraThix P-100 polymer in Phase A, heat to 75°C. Helix blade, 500 RPM.3. Combine Phase B ingredients in a separate beaker, heat to 75°C.4. At 75°C homogenize Phase A with Turrax. After a couple of minutes add Phase B with Turrax.5. Cool to 50°C, add Phase C, homogenize with Turrax then switch to blade mixer.

pH 5.4 – 6.0; White shiny cream; Viscosity: 21,000

Chart 3: Lamellar Gel Challenge Tests

1.00E+00

1.00E+01

1.00E+02

1.00E+03

1.00E+04

1.00E+05

1.00E+06

1.00E+07

cfu/

g

Unpreserved Control

Bacteria

Yeast

Fungi

1.00E+00

1.00E+01

1.00E+02

1.00E+03

1.00E+04

1.00E+05

1.00E+06

cfu/

g

1.6% Optiphen DP preservative @ pH 6.0

Bacteria

Yeast

Fungi

1.00E+00

1.00E+01

1.00E+02

1.00E+03

1.00E+04

1.00E+05

1.00E+06

1.00E+07

cfu/

g

Unpreserved Control

Bacteria

Yeast

Fungi

1.00E+00

1.00E+01

1.00E+02

1.00E+03

1.00E+04

1.00E+05

1.00E+06

cfu/

g

1.6% Optiphen DP preservative @ pH 6.0

Bacteria

Yeast

Fungi

5

ConclusionIn multiple challenge tests conducted in our global laboratories, Optiphen DP preservative has been shown to protect products in the range of 0.3% to 2.0%. The technology is based on organic acids, so it is recommended for products at pH of 6.0 or lower. Optiphen DP preservative can be used to preserve wet wipes systems, rinse-off cosmetics (shampoos, shower gels, foam bath, body washes, conditioners, etc.) and care products (moisturizers, cream, sunscreens, lotions, gels, foundations, etc.).

Optiphen DP preservative is the first product launched from the Optiphen P preservative platform. This patent-pending delivery system boosts the performance of the active ingredients, with no or minimal interference or destabilization of the end product. This new technology contains nature-identical and naturally derived actives and conforms to Eco-label requirements from several organizations.

Web-based Preservatives Selector Tool

Use the Ashland preservative selector tool in your day-to-day work. It is easy to navigate, and helps you determine the preservative technology that best fits your needs. The tool is accessible from any desktop computer or mobile device. If you have yet to use the tool, check it out under preservativeselector.com.

Regulatory UpdateEuropean Commission publishes two regulations restricting the use of parabens and CMIT/MIT

On 18 September 2014 EU Commission regulation No 1004/2014 was published amending Annex V of the EU Cosmetics Regulation and confirming that propyl and butyl parabens are safe for use in cosmetic products where the sum of individual concentrations of propyl and butyl parabens does not exceed 0.14% (as acid). The same regulation also prohibits the use of propyl and butyl parabens in leave-on cosmetic products designed for application to the nappy area of children below 3 years. Leave-on products not intended to be applied to the nappy area of children less than 3 years should be labelled with “Do not use on the nappy area”. Under the amending regulation, companies had 6 months to place compliant products onto the EU market (from 16 April 2015) and 12 months to remove non-compliant products (until 16 October 2015).

Also published on 18 September 2014 was Commission Regulation (EU) No 1003/2014 amending Annex V of the EU Cosmetics Regulation and banning the use of CMIT: Chloromethylisothiazolone & MIT: Methylisothiazolone in leave-on products. Companies have 9 months to place compliant products onto the EU market (until 16 July 2015) and 18 months to withdraw non-compliant products from the market (until 16 April 2016).

European Commission proposal for formaldehyde

Following the reclassification of formaldehyde as a Category 1b Carcinogen from the 1st January 2016, the European Commission plans to remove the entry for formaldehyde from Annex V (Preservatives List) of the EU Cosmetics Regulation (1223/2009/EC). Its entry in Annex III which permits use in nail hardeners will also be updated in accordance with the recent SCCS: Scientific Committee of Consumer Safety conclusions on this use. By the 1st of January 2016, all products containing formaldehyde should be removed from sale and should be reformulated to remove formaldehyde apart from the permitted use in nail hardeners. There is no proposal from the European Commission to remove the entries for any of the formaldehyde donor preservatives from Annex V. We understand that the Commission instead plans to assess the formaldehyde coming from the donor preservatives through SCCS evaluations of the individual preservatives themselves.

Preservatives Newsletter (Customer Edition) June 2015

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Preservatives Highlightedin this Issue

Preservatives Newsletter (Customer Edition) June 2015

Trade Name INCI Name Features and BenefitsOptiphen DP preservative

Propylene Carbonate (and) Benzoic Acid (and) Dehydroacetic Acid (and) Propanediol (and) PVP

• Microbiostatic spectrum of activity, in some formulations additional booster is needed• Effective up to pH 6.0 • Global use†

• Cost-efficient preservative based on uncontroversial ingredients• Optimized delivery system without alchoholic antimicrobials

Optiphen ODpreservative booster

Caprylyl Glycol • Moisturizing agent• Solvent for active ingredients• Humectant• Preservative booster

† For country - specific details, please contact your technical service representative.

Global Headquarters

Ashland Inc.50 East RiverCenter Blvd.Covington, KY 41012 USATel: +1 859 815 3333

Ashland Specialty Ingredients8145 Blazer DriveWilmington, DE 19808 USATel: +1 877 546 2782

Regional Sales OfficesNorth AmericaBridgewater, NJ USATel: +1 800 505 8984

Latin AmericaSão Paulo, BrazilTel: +55 11 3649 0454 +55 11 3649 0450

Europe Barcelona, SpainTel: +34 93 298 0700Fax: +34 93 298 0705

Asia Pacific SingaporeTel: +65 6775 5366Fax: +65 6775 5433Shanghai, P.R. ChinaTel: +86 21 6090 6606Fax: +86 21 6090 6699

Middle East/Africa/IndiaTurkeyTel: +90 216 538 08 00Fax: +90 216 538 08 80

personalcare@ashland.com

ashland.com

® Registered trademark, Ashland or its subsidiaries, registered in various countries™ Trademark, Ashland or its subsidiaries, registered in various countries© 2015, AshlandPC-13231

The information contained in this brochure and the various products described are intended for use only by persons having technical skill and at their own discretion and risk after they have performed necessary technical investigations, tests and evaluations of the products and their uses. This material is for informational purposes only and describes products for use as ingredients in cosmetic products intended to enhance appearance and provide other cosmetic benefits. Certain end uses of some products may be regulated pursuant to rules governing medical devices or other regulations governing drug uses. It is the end user’s responsibility to determine the applicability of such regulations to its products. While the information herein is believed to be reliable, Ashland Inc. does not guarantee its accuracy and a purchaser must make its own determination of a product’s suitability for purchaser’s use, for the protection of the environment, and for the health and safety of its employees and the purchasers of its products.

Neither Ashland nor its affiliates shall be responsible for the use of this information, or of any product, method, formulation, or apparatus described in this brochure. Nothing herein waives any of Ashland’s or its affiliates’ conditions of sale, and no statement, information and data is to be taken as a guarantee, an express warranty, or an implied warranty of merchantability or fitness for a particular purpose, or representation, express or implied, for which Ashland and its affiliates assume legal responsibility. We also make no warranty against infringement of any patents by reason of purchaser’s use of any information, product, method or apparatus described in this brochure.