CLAY FACIAL MASKS 47
PRELIMINARY STABILITY TEST (PST)
The formulations were left at rest for 24 h before testing to ensure full water adsorption
(11,14). After this period, 5 g of each visually stable formulation (homogeneous visual
aspect) were submitted (three replicas) to centrifuge (model 208N, Fanem Ldta, Sao
Paulo, Brazil) testing. The formulations were evaluated 1000, 2000, and 3500 rev/min- 1
rotor speed, during 15 min at each velocity (15).
The formulations were classified, after centrifuge testing, according to liquid phase
separation volume: 7-10 ml (IM), intensely modified 4-6 ml (M), modified 1-3 ml
(SM), slightly modified and those without phase separation (N). Formulations classified
as normal were submitted to the accelerated stability test.
ACCELERATED ST ABILITY TEST (AST)
Yhe formulations were submitted to the stress conditions of temperature in a short
storage period. The amount of the formulations submitted to AST was 30 g, considering
that on each day of analysis there was a sample that did not return to storage conditions.
Samples were stored in polyethylene packing material. Temperatures, storage periods,
and days of analysis were (13,15):
(a) 45.0° ± 0.5°C 14 days analysis at the 1sr, 3rd ,7t\ and 14th days.
(b) -10.0° ± 0.5°C/24 h and 45.0° ± 0.5°C/24 h (temperature cycles)
12 days analysis at the 6t h and 12th days.
(c) 5.0° ± 0.5°C 14 days analysis at the 15\ 3rd ,7t\ and 14t h days.
Yhe formulations were first acclimatized for at least 1 h at room temperature
(24° ± 2.0°C) prior to testing, considering the first day of analysis (t1) as 24 h after the
preparation of the formulations.
Yhe physicochemical characteristics evaluated, on each day of analysis, were: organo-
leptic characteristics (visual aspect, color, and odor), pH value, and apparent viscosity
(13,15). The formulations were dispersed (1:10) in distilled water in order to measure
pH values. The apparent viscosity of the formulations was determined using a rotational
viscometer (model Visco Star R, Fungilab S.A.). The apparent viscosity measurements
were obtained under the following experimental conditions: 24° ± 2.0°C, 18 g samples,
TRll spindle, and rotation speed of 100 rpm. Analyses were accomplished in parallel
with a reference sample, stored at a controlled room temperature (22° ± 2°C).
RESULTS AND DISCUSSION
PRELIMINARY STABILITY TEST (PST)
The formulations presented a red color, an earthy characteristic odor, and pH values
ranging from 6.8 to 7 .1.
After centrifuge testing, the F2 formulation was intensely modified with a considerable
phase separation. Yhis instability was attributed to an insufficient viscosity of the
formulation to keep a high content of soiids dispersed. The clay types differed from each
other mainly by their mineral composition, which has an influence on the viscosity and
48 JOURNAL OF COSMETIC SCIENCE
stability of formulations (7). Magnesium aluminum silicate, which was added to the F2
formulation, is widely used as a thickening agent in many cosmetic preparations, due to
its thixotropic and pseudoplastic properties. The colloidal structure of this clay provides
excellent suspension of fine particles in aqueous systems (16) however, it did not offer
the suspension efficiency of other clay particles (kaolin and montmorillonite) in the
formulations studied.
Clays and organic thickeners, such as gums, are often used synergistically in cosmetic
products to provide a balance of suspension stability. The gums' protective colloidal
action improves clay stability in the presence of electrolytes, surfactants, water-solubles,
and even against phase separation (11,17). This fact was also observed in this study, once
hydroxypropyl starch phosphate (Fl) and xantham (F3) gums promoted stability in both
formulations after centrifuge testing, preventing phase separation. Therefore, only the
Fl and F3 formulations were classified as normal after PST, and they were submitted to
AST.
ACCELERATED ST ABILITY TEST (AST)
Formulations Fl and F3 maintained normal color and odor in all storage conditions.
These formulations did not present variation in the initial pH value (7 .3), superior to
± 1.0%, probably due to the buffer effect of clay that occurs when a suspension is at a pH
very near its natural pH (range of pH close to 6.0 or 7.5-8.0) (18). However, they
presented variations in visual aspect (Table I) and apparent viscosity (Figure 1) in the
same evaluated conditions. These alterations could be associated with temperature and
time influences on the clay hydration process.
The structural framework of clay is composed of thousands of submicroscopic platelets
Table I
Visual Aspects Observed in Fl and F3 Formulations at Different Temperatures in Storage Conditions in
the Accelerated Stability Test
Temperatures of
storage conditions
5.0° ± 0.5°C
22° ± 2.0°C
45.0° ± 0.5°C
-10.0° ± 0.5°C/24 h
45.0° ± 0.5°C/24 h
Days of
analysis
t
l 3
7
14
3
7
14
3
7
14
7
14
t
1 =24 h after preparation of clay masks.
SM =slightly modified.
N =normal.
Visual aspect
Fl F3
Homogeneous Homogeneous
SM SM
SM SM
SM SM
N SM
N SM
N SM
SM SM
SM SM
SM N
SM N
SM N
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