257 CRITICAL FACTORS TO OBTAIN STABLE HIP GEL-IN-OIL EMULSIONS
temperatures, but conversely to water-in-oil, water-in-silicone, and conventional HIP W/O
emulsions,13 the addition of salts was not required.
The interest of the HIP gel-in-oil concept for the development of cosmetic emulsions with
original aesthetics was highlighted some years ago.18 First of all, it provides an attractive
smooth and mirrored gloss appearance for the end user, with an unexpected contrasting
sensory profile starting with a first fresh sensation evolving to a cushion-comfortable finish.
As a result, the gel-in-oil emulsion is able to impart a similar emollience to conventional
cream gel, oil-in-water (O/W), and W/O formulations with a reduced oil concentration19
and provides an inherent water resistance character. The texture of gel-in-oil emulsion
alone (without any olfactory, packaging, or brand environment) was demonstrated to arouse
positive emotions in consumers.20
From the formulator’s point of view, the concept takes advantage of high compatibility
with active ingredients,21 including those rich in electrolytes. Gel-in-oils also withstand
the incorporation of a high quantity of solvents, sometimes required to solubilize these
active ingredients (e.g., glycols, ethanol, etc.). The manufacturing process, cold and using
low mixing energy, is industrially advantageous, saving time and increasing sustainability
by reducing carbon emissions.17
Despite these advantages, the factors affecting the emulsion structure and behavior have
not been thoroughly clarified, thus limiting the use of the concept. As is known for other
inverse emulsions, it is difficult to predict the long-term stability of gel-in-oil without
waiting for three months, even using accelerated tests (storage at 45°C and freeze–thaw
cycles in particular). Due to high concentration of the dispersed phase, gel-in-oils mainly
provide compact textures, which make them difficult to prepare and diminish the
relevance of accelerated tests based on centrifugal force (such as the LUMiFuge® device
from Germany) or based on multiple light-scattering analyses (such as the Turbiscan® LAB
device from France).
The objective was therefore to study rigorously the factors affecting the emulsion structure,
stability, and behavior under stress for a better understanding of the limitations of the
formulation. First, details of the manufacturing process needed to be investigated using a
simple formula to confirm the recommendations: preparation mode (i.e., direct or indirect)
Figure 1. Gel-in-oil macroscopic appearance and structure representation.
258 JOURNAL OF COSMETIC SCIENCE
and agitation type (i.e., mixing, homogenization). Key composition factors were also
scrutinized: impact of gel viscosity by increasing the doses of a suitable rheology modifier
emulsifier level ratio between the internal aqueous phase and the external oily phase and
nature of the oil. This work also aimed to find an appropriate test to check quickly that the
formulation is optimized without waiting for the conventional stability tests. With this in
mind, flow and oscillatory rheology experiments were explored to test the structure and
resistance of gel-in-oils.
MATERIALS AND METHODS
INGREDIENTS AND COMPOSITION OF THE FORMULATION BASE
Formulation experiments were carried out by changing one parameter at a time. A formula
base with a reduced number of ingredients was chosen to facilitate analysis of the impact
of changes (Table I).
Ingredients were weighed using an ML 1602 precision balance (Mettler Toledo GmbH,
Greifensee, Switzerland) to prepare 300 g of each formulation.
CHARACTERIZATION AND STABILITY OF FORMULATIONS
Viscosity measurement. The viscosity of the samples was measured using a Brookfield
LVDVI+™ viscometer using an appropriate spindle and speed 6 (Brookfield Engineering
Laboratories Inc., Middleboro, MA, USA). Measurements were taken one day after
manufacturing (D1), after 7 days (D7), after 1 month (M1), and after 3 months (M3).
Microscopic observations. The stable formulations were observed using an optical microscope
Meiji® MT-9300 (Meiji Techno Co., Ltd., Saitama, Japan) with a magnification of ×400,
one week after manufacturing (D7), and images were captured by an attached charge-
coupled device camera GR500W (Shanghai Goldroom Im/Export Trade Co., Ltd.,
Shanghai, China).
Table I
Formulation Base With Fixed Ingredients and Variables Studied
Phase Ingredient %(w/w)
Gel Demineralized water Up to 100
phase Hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymera 0.6/0.7/0.8/1/1.2
Xylitylglucoside and anhydroxylitol and xylitolb 3.00
Phenoxyethanol and ethylhexylglycerinc 0.80
Oily Octyldodecanol and octyldodecyl xyloside and PEG-30
dipolyhydroxystearated
0.50/1/1.5/2/2.5/3
phase Caprylic/capric triglyceridee 3/5/8/13/18/23/28
a Polyelectrolyte rheology modifier (Seppic, La Garenne Colombes, France).
b Moisturizing active ingredient playing here the role of antifreeze agent (Seppic, La Garenne Colombes,
France): fixed ingredient in all the trials.
c Preservative (Thor Specialty Chemical Co., Ltd., Zhenjiang, China): fixed ingredient in all the trials.
d Liquid emulsifying system (Seppic, La Garenne Colombes, France).
e Oil (Croda International Plc, Goole, United Kingdom).
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