2006 ANNUAL SCIENTIFIC MEETING 77
Table J: Order of Addition and Efficiency Tips (continued)
Add polymerto(deionized) water of the Efficiency can be improved by including
Acrylates 1.0-3.0o/ofor formulation. Add primary surfactants. betaines in combination with typical
Copolymer clear products Neutralize to a pH of6.5. Add remaining sulfates and sulfonates. Best efficiency in
(specialty) surfactant'!. Add conditioning and systems using moderate to high level of
1.5 l.8%for ancill
ary
in
gr
edient'!, and if desired, surfactant actives (15-23 wt.%).
pearlized products appearance modifiers. Add fragrance, dyes "Back-acid thickening',.and/or sodium
and preservatives. Adjust final pH with chloride can be used to increase efficiency.
citric acid solution ("back-acid" process).
Add sodium chloride to adjust
viscosity (if necessary).
Order of addition is very important.
Add pol
ym
er to (deionized) water of the Efficiency can be improved by including
Polyacrylate-1 1.0 1.5% formulation. Add primary and secondary betaines in combination with typical
Crosspolymer surfactant'!. Add conditioning and ancillary sulfates and sulfonates. Best efficiency in
ingredients, fragrance,dyesand systems using moderate to high surfactant
preservatives. Neutralize to pH 6.0 actives (15-23 wt.%). "Back-alkaline
thickening''3 and/or sodium chloride can be
used to increase efficiencv.
Ta e :bl 4 S tora• e &B andhne: p roce d ures
Polymer Type Shelf Life (Under
(INCI Designation) Storage Recommended Comments
Storage Conditions)
Storeinclean, dry
Carbomer environment. Containers 2 years Polymerissuppliedat2%moisture�
should be kept tightly closed to above 2% may cause clumping or difficulty in dispersion.
avoid moisture pickup.
Avoid dusting.
Acrylates/C 10-30 Store in clean, dry
Alkyl Al-'rylate environment. Containers 2 years Polymerissuppliedat2%moisturec
Crosspolymer should be kepttightlyclosed to above 2% may cause clumping or difficulty in dispersion.
avoid moisture pickup.
Acrylates Store in unopened containers 9months. Best results if product is filtered before use.
Copol
ym
er at 5-30°C. Optimal storage Conditions exposing the
poymer
l (as supplied) to high
Do not FREEZE. temperature is 21 °C. shear should be avoided. Keep storage vessels and
Recommended to use in full transfer equipment clean. Prompt flushing of transfer
drum quantities. eauioment is recommended.
Polyacrylate-1 Store in unopened containers 6months. Mix (do not filter) prior to use. To avoid skinning and
Crosspol
ym
er at 20-30°C. product discoloration. do not open drums until ready to
Product is freeze-thaw stable use. Pol
ymer
contains amine groups which can discolor
as supplied Recommended when exposed to the atmosphere this does not impact
to use in full drum quantities. oolvmer nerformance.
T b 5 Cl a le�: eamn2 Procedures
Polymer Type
(INCI Designation) Recommended Procedure (Overview)
Oil-free formulas should be cleaned with hot saline solution. Emulsion formulas should be cleaned with hot
Carbomer detergent solution. Use wann to hot alkaline water (65°C). Raise pH using caustic.
Add ionic detergent such as sodium tri
po
lyphosphate. Agitate for 30 minutes.
Tum agitation off &drain. Scrao loose dcoosits. Reoeat 2-3 times.
Acrvlates/C 10-30 Oil-free formulas should be cleaned with hot saline solution. Emulsion formulas should be cleaned with hot
Alkyl Acrylate detergent solution. Use warm to hot alkaline water (65°C). Raise pH using caustic.
Crosspolymer Add ionic detergent such as sodium tripolyphosphate. Agitate for 30 minutes.
Tum agitation off &drain. Scrap loose deposits. Repeat 2-3 times.
Acrylates Storage tanks should be cleaned by thorough flushing or using the caustic fill and soak method. If buildup
Copolymer occurs on smaller pieces of equipment, it can be removed by soaking in 1.5% caustic solution. The causitc
solution can be heated to 75°C. Cleaning of transfer piping and pumps can be minimized by leaving lines
full (with no air tOCkets ).If not kept full, transfer lines should be flushed well after each use.
Polyacrylate-1 Storage tanks should be cleaned by thorough flushing or using an acidic solution to soak and then flush.
Crosspol)'mer If buildup occurs on smaller pieces of equipment, it can be removed by soaking.
Transfer lines and equipment should be flushed well after each use.

78 JOURNAL OF COSMETIC SCIENCE
CLEANING AFTER MANUFACTURING: THE fORGOTTON STEP OF SCALE UP
Christopher C. Heisig, Ph.D. and Gurusamy Manivannan, Ph.D.
STERIS Corporation, St. Louis, MO 63166
ABSTRACT
Many cosmetic and personal care companies are expanding their businesses to include the manufacturing of
products with drug claims (e.g., antibacterial soaps, sunscreens). There is growing scrutiny by the FDA on
drug-manufacturers to prove that their cleaning validation programs are compliant (i.e., that they prevent cross-
contamination and inadvertent microbial load in subsequent products). However, even before addressing
cleaning validation, an evaluation of a company's entire cleaning system is needed. This includes evaluating
cleaning equipment capabilities, types of soils, test methods, cleaning chemistry and the impact of cross-
contamination on subsequent products. The selection of proper cleaning agents is vital, since some soils can be
cleaned with water alone or with a commodity cleaner (e.g., NaOH, KOH), while other "difficult-to-clean"
soils warrant additional cleaning mechanisms through the use of materials such as surfactants and chelants.
This presentation will focus on some of the chemistries used for cleaning mixing tanks and vessels and will
provide examples.
INTRODUCTION
In 1993, the FDA issued a guidance document to reinforce cGMP compliance requirements directed towards
cleaning validation. 1 These requirements are aimed primarily at the pharmaceutical industry however, as the
cosmetic and personal care industries continue to expand into new markets, many are becoming manufacturers
of both drug and non-drug products. This ongoing product expansion has required some to review and update
their cleaning strategies and procedures.
The scale-up process, during which the entire manufacturing environment should be taken into account, is a
strategic point where cleaning procedures can be addressed. The cleaning equipment used varies throughout
the industry, including "clean-in-place" systems, agitated immersion, and manual methods. Some companies
have equipment dedicated for the manufacturing of products that are classified as drugs, while others have
equipment that are used for manufacturing both drug and non-drug products. Some employ grouping
strategies, where similar products are made in one manufacturing vessel, and cleaned using one procedure
when possible. When evaluating an entire facility, some even extend the same quality approach to all of their
cleaning procedures, whether a drug product is manufactured in that tank or not. The underlying purpose is to
eliminate residue that can carry over to and contaminate the next (drug) product.
Fundamental to cleaning performance are the actual cleaning chemistries employed. Some companies use
commodity cleaners (e.g., hydroxides, acids, alcohols) to address their needs. Others may need more
''complex" chemistries due to the types of soils they are trying to clean. For example, "formulated cleaning
products" often contain surfactants, chelating agents, dispersants, suspending agents, hydrolyzing agents or
other materials to assist in cleaning the targeted difficult-to-remove soils from product contact surfaces.
The most common materials used in formulated cleaning products are surfactants. These "surface-active"
components provide wetting and assist in solubilizing and/or emulsifying soils. The choice of surfactants used
in a cleaning system is dependent on the intended cleaning use. Such requirements as cleaning time, use-
temperature, concentration, foaming properties and rinsability will help in deciding which surfactant systems
are best for a specific application.
1 FDA. "Guide to Inspection of Cleaning Processes." Division of Field Investigations, Office of Regional
Operations, Office of Regulatory Affairs, July 1993.