Integra 44 microbiocide -...

Integra™ 44 microbiocideCreate natural cleaning products withan Ecocert verified preservative derivedfrom glycine

Preservatives aligned to the greendetergent standards Ashland’s Integra™ 44 microbiocide for detergent products is Ecocert verified. Aligned to cleaning product standards promoting alternatives to classic chemistry that are less onerous to the environment, formulators may specify Integra 44 microbiocides when manufacturing green detergents. Derived from glycine, an amino acid, Integra 44 microbiocide is one of the safest handling preservation technologies available for use in liquid detergents.

Integra 44 microbiocide is a fast-acting liquid microbiocide offering broad-spectrum antimicrobial activity on par with classical microbiocide chemistry. Moreover, in high alkaline conditions, the microbiocide maintains its antimicrobial activity, providing manufacturers the flexibility they need to produce a range of formulations. Suitable for formulations that range in pH from 3.5 to 12, easy-to-use and safe-to-handle, manufacturers will find Integra 44 microbiocide is the natural choice for preserving liquid detergents in any marketplace.

Optimizing Integra 44 microbiocide in liquid detergentsEvery cleaning product will have its own optimal preservation level and every formulation requires challenge testing to determine preservation efficacy. Ashland’s microbiologists offer cleaning product manufacturers that utilize Integra 44 microbiocide free challenge testing services for concept formulations and commercial liquid cleaning products.

Sample formulations for cleaning product applications and challenge testing services may be arranged by contacting Ashland in your region (see back cover) or by contacting us at [email protected].

Integra 44 microbiocide for natural detergents• Aqueous solution of sodium hydroxymethylglycinate• Derived from glycine – a naturally occurring amino acid• Broad-spectrum antimicrobial activity• Effective against bacteria and fungi• For use in pH range of 3.5 to 12• Easy-to-use and safe-to-handle• Excellent for water-based applications such as liquid

detergents, dishwashing liquids and cleaning products

Integra 44 microbiocide in household and industrial cleaning applicationsIntegra 44 microbiocide is available for use in a range of liquid household and industrial cleaning formulations, including laundry detergents, fabric softeners, dishwashing products, general purpose detergents, industrial cleaners, liquid soaps and hard surface cleaners. When used as directed (between 0.2 and 1.0% as supplied), Integra 44 microbiocide provides adequate protection for surfactant-based formulations.

Performance parameters A well-established microbiocide with a long history of safe use, Integra 44 microbiocide offers a performance window beyond the scope of many traditional microbiocide technologies. The technology stands out for its:

Broad-spectrum activity• Integra 44 microbiocide is active against gram-negative and

gram-positive bacteria but is also effective against fungi. Integra 44 microbiocide is particularly effective against Pseudomonas aeruginosa, a common spoilage organism.

Antimicrobial activity in high-alkaline systems • Most microorganisms require an environment with a pH

between 5 and 9. Sometimes a species will survive up to pH 12. Integra 44 microbiocide remains effective from pH 3.5 - 12, giving the formulator flexibility.

Compatibility• Integra 44 microbiocide remains effective in surfactant

systems and most common formulations. Color changes have been observed, however, with fragrances containing citral, although antimicrobial properties are not affected.

Effective use at low concentrations• Typical formulations use Integra 44 microbiocide at low

concentrations, usually 0.2% - 1.0% as supplied, thereby providing cost-effective preservation.

Ease of handling • Integra 44 microbiocide is supplied as a 50% aqueous

solution, allowing for easier handling in manufacturing when compared to powdered preservatives. Integra 44 microbiocide also shows excellent water solubility and low oil solubility, so it will remain in the water phase where it acts against microorganisms.

Low order of toxicity • Information provided below are typical properties of Integra

44 microbiocide and are not necessarily specifications.

Solubility Integra 44 microbiocide shows ideal solubility characteristics for water-based systems. It is highly water soluble and has a very low solubility in non-aqueous solvents, as shown in the following table:

Integra 44 microbiocide Minimum InhibitoryConcentration (MIC) resultsMinimum Inhibitory Concentrations (MICs) are a useful screening procedure for antimicrobial activity; however, they do not necessarily represent antimicrobial activity in finished products. Adequate preservative efficacy can only be assured with appropriate challenge studies.

Active Ingredients

Sodium hydroxymethylglycinate 48.0-52.0%

Appearance Colorless to yellow

Color (APHA) 500 max.

Odor Characteristic amine

pH 9.5-12.0

Specific gravity (@ 25°C) 1.27-1.30

CAS registry formula 70161-44-3

EPA reg. no. 57978-4

Molecular formula C3H6NO3Na

Molecular weight 127.10

Solvents Solubility (in grams/100g of solvent)

Water Miscible

Propylene glycol 112g

Glycerin 119g

Butylene glycol <0.10g

Mineral oil <0.10g

Ethanol 3-A anhydrous <0.10g

Bacteria ATCC No.Active Ingredient

(ppm)

Gram-positive

Bacillus subtilis 6633 300

Staphylococcus aureus 6538 600

Gram-negative

Enterobacter aerogenes 13048 600

Enterobacter cloacae 33457 300

Escherichia coli 8739 600

Proteus vulgaris 9920 300

Pseudomonas aeruginosa 9027 600

Burkholderia cepacia 25416 450

Pseudomonas fluorescens 13525 300

Fungi ATCC No.Active Ingredient

(ppm)

Aspergillus niger 16404 1200

Candida albicans 10231 2500

Integra 44 microbiocide challenge studies Liquid dishwashing detergent 28-day challenge test A 28-day challenge study was run to determine the antimicrobial activity of Integra 44 microbiocide at levels of 0.2% and 0.4% in a liquid dishwashing detergent. Separate samples of the dishwashing detergent were tested using selected industrial challenge organisms. Integra 44 microbiocide at levels of 0.2% and 0.4% showed complete kill of all microorganisms tested in 48 hours and 28 days. The control, which did not contain preservatives, failed the challenge test with bacteria and mold.

Liquid dishwashing formulation

Manufacturing procedure: To water at room temperature, add alkylbenzene sulfonic acid and NaOH with agitation. Mix thoroughly. Add alkamide DC 212/S. Add NaCI. Adjust pH to 9.2 using 10% NaOH. Add Integra 44 microbiocide.

Challenge test organismsThe following organisms were cultured, prepared and standardized according to methods MLM 100-3, 4 & 5. The inoculum concentrations are listed as the original inoculum and reinoculum counts.

All formulations preserved with Integra 44 microbiocide passed the challenge test as adequately preserved at a low level of 0.2% as supplied.

Liquid fabric softener 28-day challenge testA 28-day challenge study was run to determine the antimicrobial activity of Integra 44 microbiocide at the level of 0.2% and 0.4% in a liquid fabric softener. Separate samples of the fabric softener were tested using selected industrial challenge organisms. Integra 44 microbiocide at a level of 0.4% showed complete kill of all microorganisms tested in 7 and 28 days. The control, which did not contain preservatives, failed the challenge test with bacterial and mold.

Liquid fabric softener formulation

*Trademark owned by a third party

Challenge test resultsAll formulations preserved with Integra 44 microbiocide passed the challenge test as adequately preserved at a low level of 0.40% as supplied.

Challenge test organismsThe following organisms were cultured, prepared and standardized according to methods MLM 100-3, 4 & 5. The inoculum concentrations are listed as the original inoculum and reinoculum counts.

Product handling Material may darken with prolonged exposure to elevated temperatures. Do not store above 30°C. Increased color does not diminish the antimicrobial activity.

Toxicology and safetyAn extensive safety database is available for Integra 44 microbiocide based on a large number of studies that demonstrated a low level of product toxicity to humans and the environment.

Integra 44 microbiocide is neither teratogenic nor mutagenic and did not produce evidence of cumulative skin irritation or allergic contact dermatitis when tested in a human repeated insult patch test panel. Moreover, ecological testing demonstrated Integra 44 microbiocide is practically non-toxic in standard avian and fresh-water fish and invertebrate species.

Integra 44 microbiocide toxicology summaryData below represents 50% active product, unless otherwise specified.

Overall, the data shows Integra 44 microbiocide may be safely used as a broad-spectrum preservative and microbiocide for household applications.

Subjects Results

Acute oral LD50 in rats(both sexes)

2100 mg/kg

Acute dermal LD50 in rabbits >2000 mg/kg

Primary eye irritation in rabbitsMildly irritating without washout, non-irritating with washout (5% aqueous solution)

Primary skin irritation in rabbits Non-irritating

Dermal sensitization in humansNot a sensitizer (0.5% aqueous solution)

Mutagenicity

Non-mutagenic in Salmonella reverse mutation assay (Ames), chromosomal aberration assay, rat hepatocyte, primary culture/DNA repair test

Developmental toxicity in rats Not teratogenic

Ingredients Weight %

Water, distilled 88.40

Alkylbenzene sulfonic acid 7.30

Alkamide DC 212/S 2.30

NaOH 1.00

NaCl 0.80

Integra 44 microbiocide 0.20

Ingredient Weight %

Water, deionized 93.35

Miranol DM* (Solvay) 3.00

Arquad 2HT 75* (AKZO) 2.00

Surfadone™ LP-300 wetting agent (Ashland)

1.00

Fragrance 0.25


Organisms

S. aureus 6538 3.0 x 106 CFU/g of product 2.2 x 106 CFU/g

E. aerogenes 13048 6.1 x 106 CFU/g of product 5.0 x 106 CFU/g

P. vulgaris 9920 2.5 x 106 CFU/g of product 5.6 x 105 CFU/g

P. putida 31800 1.8 x 106 CFU/g of product 1.1 x 105 CFU/g

P. fluorescens 13625 1.1 x 106 CFU/g of product 7.8 x 106 CFU/g

C. albicans 10231 2.5 x 106 CFU/g of product 1.3 x 106 CFU/g

A. niger 16404 1.2 x 105 CFU/g of product 1.0 x 105 CFU/g

Preservative Assay (CFU/g) 48 hours 7 days 14 days 21 days 28 days

Integra 44 microbiocide at 0.20%

A. niger 16404 4.0 x 101 3.0 x 101 <10 <10 <10

C. albicans 10231 <10 <10 <10 <10 <10

E. aerogenes 13048 <10 <10 <10 <10 <10

P. putida 31800 <10 <10 <10 <10 <10

P. vulgaris 9920 <10 <10 <10 <10 <10

S. aureus 6538 <10 <10 <10 <10 <10

P. fluorescens 13625 <10 <10 <10 <10 <10


A. niger 16404 1.5 x 101 <10 <10 <10 <10

C. albicans 10231 <10 <10 <10 <10 <10

E. aerogenes 13048 <10 <10 <10 <10 <10

P. putida 31800 <10 <10 <10 <10 <10

P. vulgaris 9920 <10 <10 <10 <10 <10

S. aureus 6538 <10 <10 <10 <10 <10

P. fluorescens 13625 <10 <10 <10 <10 <10

Organism








Waterless hand cleaner 28-day challenge A 28-day challenge study was run to determine the antimicrobial activity of Integra 44 microbiocide at the level of 0.4% in a waterless hand cleaner. Separate samples of the waterless hand cleaner were tested using selected industrial challenge organisms. Integra 44 microbiocide at the level of 0.4% showed complete kill of all microorganisms tested in seven days. The control, which did not contain preservatives, failed the challenge test with bacteria, yeast and mold.

Waterless hand cleaner formulation


Manufacturing procedure: Phase A: combine water, sodium hydroxide and propylene glycol and mix until homogeneous. Phase B: in a separate vessel gently heat Isopar M, Emersol 233LL, mineral oil, Surfadone LP-300 wetting agent, Antaron V-216 polymer and lanolin to 35-40°C. Use continuous mixing until homogeneous. Add to Phase A and continue mixing. Add lgepal CO-730, cool to 25-30°C, cover and let stand overnight.

Challenge test resultsThe formulation preserved with Integra 44 microbiocide at the level of 0.40% as supplied passed the double challenge test as adequately preserved.

Liquid hand soap 28-day challenge test studiesA 28-day challenge study was run to determine the antimicrobial activity of Integra 44 microbiocide at levels of 0.2% and 0.4% in liquid hand soap. Separate samples of the liquid hand soap were tested using selected industrial challenge organisms. Integra 44 microbiocide at levels of 0.2% and 0.4% showed complete kill of all microorganisms tested in 48 hours and 28 days. The control, which did not contain preservatives, failed the challenge test with bacteria, yeast and mold.

Liquid hand soap formulation


Manufacturing procedure: Mix all ingredients into water until a clear gel forms. Warm as necessary to dissolve ingredients.

Challenge test resultsAll formulations preserved with Integra 44 microbiocide passed the challenge test as adequately preserved at a low level of 0.20% as supplied.

Challenge test organismsMethod MLM 100-9 was followed for this study. The organisms were cultured and the inoculums have been prepared and standardized according to procedures MLM 100-3, 4 & 5. The inoculum and reinoculum (second value) concentrations were:

Challenge test organisms

Ingredient Weight %

Water, deionized 48.80

Sodium lauryl ether sulfate (28%)

40.00

Alkateric® CAB-O* (Solvay) 10.00

Surfadone LP-300 wetting agent (Ashland)

1.00


Ingredient Weight %

Water, distilled 49.00

Isopar® M* (Exxon) 25.00

Sodium hydroxide(10% aqueous)

7.5

Emersol® 233LL* (Emery) 7.5

Surfadone LP-300 wetting agent (Ashland)

3.00

Igepal CO-730* (Stepan) 3.00

Carnation mineral oil (Carnation) 2.50

Propylene glycol 1.50

Antaron™ V-216 polymer (Ashland)

0.50

Lanolin, USP 0.10


Organism







Organism




B. cepacia 25416 3.2 x 106 CFU/g of product 4.3 x 104 CFU/g





A. niger 16404 <10 <10 <10 <10 <10

C. albicans 10231 <10 <10 <10 <10 <10

P. fluorescens 13625 <10 <10 <10 <10 <10

P. putida 31800 <10 <10 <10 <10 <10

P. vulgaris 9920 <10 <10 <10 <10 <10



A. niger 16404 <10 <10 <10 <10 <10

C. albicans 10231 <10 <10 <10 <10 <10

E. aerogenes 13048 <10 <10 <10 <10 <10

B. cepacia 25416 <10 <10 <10 <10 <10

P. fluorescens 13625 <10 <10 <10 <10 <10

S. aureus 6538 <10 <10 <10 <10 <10

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

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

[email protected]

ashland.com

® Registered trademark, Ashland or its subsidiaries, registered in various countries™ Trademark, Ashland or its subsidiaries, registered in various countries© 2013, AshlandPC-12552

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.

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