STABILITY STUDY OF COCOA BUTTER BODY SCRUB FORMULATED WITH

GROUND COCOA POD HUSK

Azila, A.K.* and Nur Azilah A.

Cocoa Innovation & Technology Centre, Malaysian Cocoa Board,
PT12621, Nilai Industrial Area, 71800 Nilai, Negeri Sembilan, Malaysia
*email: aziela@koko.gov.my

Malaysian Cocoa J. 7: 40 - 45
ABSTRACT - Cocoa body scrub was formulated with cocoa butter without addition of emollient
agent, and ground cocoa pod husk as exfoliating agent. Initial studies showed the products tend to
rancid and bloom was finally overcome. The stability of the product was evaluated by freeze/thaw
stability cycle and accelerated stability method. The freeze/thaw stability cycle was carried out by
stressing the product under 4oC for 24 hours and the following 24 hours under 40oC, and repeated
several times. The accelerated stability method was conducted under 45 oC in an oven for twelve weeks
to determine the pH, viscosity and the appearance of the product. This product passed three cycles of
freeze/thaw and accelerated stability study for 8 weeks predicted the product can withstand 10 months of
shelf-life without any deteriorations.

Key words: Cocoa, Body Scrub, Cosmetics, Accelerated Stability Study.

INTRODUCTION burning of the skin, and irritation in the nose

Daily exposure to the environment and
natural body keratinisation accumulates the
dead skin layer on the stratum corneum which
leads to an older looking and thick layer of
skin. This dead skin, however, will naturally
slough-off within two weeks or more
depending on age. Nevertheless, the slough-
off of the old dead skin-layer can be
accelerated with the application of an
exfoliating cosmetic product, either in
chemically or physically which results in
more supple and smooth new skin layer, and
younger in appearance.
Skin exfoliation is a cosmetic
technique aimed at improving one’s skin
appearance by removing dead skin cells from
the surface of the skin. Basically, there are
two types of exfoliation, i.e. chemically or
physically. Chemical exfoliation involves the
use of chemical substances such as enzymes
and alpha-hydroxy acids (AHAs), glycolic
acid from sugar cane, malic acid (apple) and
citric acid (various citrus fruits). These
AHAs exfoliate dead skin cells by facilitating
the degradation of the binding structures
between cells leading an increased
desquamation of the horny cells, with
increased new cell regeneration. However,
improper use or application of AHA not at
safe levels (Bombeli, 2005) can bring about
several adverse effects, such as stinging and
and eye area.
Other than chemical agent, the dead
skin layer can also be removed physically by
the application of a cosmetic product with
particulate materials of 10/400 mesh. The
particle or exfoliating agent, either synthetic
or natural, is usually an inert material in the
product that has the capability to remove the
dead skin layer or loose flakes of stratum
corneum and polish the skin. However,
excessive usage of body scrub can also be
irritating (Williams, 1992). The application
of body scrub is said to be equal to two-to-
three times tape stripping. Synthetic
materials that are usually use as scrubbing
agents are polyethylene beads, while sugars,
ground seed husks and loofah are natural
ingredients use in body scrubs.
The treated cocoa pod husk serves as
inert materials to the cream of the body scrub.
However, the stability of this product has to
be determined prior to the application, where
consumers’ expectations are always for
product with a longer shelf life. Products that
have showed a separation layer due to the
creaming or floating would usually be judged
as expired or not stable and cannot be used by
the consumer.

MATERIALS & METHODS
Treatment of Cocoa Pod Husks
The cocoa pod husks (CPHs) were collected
from LKM Hilir Perak R&D Centre. It was
chopped into about 1 cm2 size-pieces and
weighed before sun-dried for seven days.
Dried CPHs were then ground into powder
using rotary mill and sieved for 425µm
particle size. Each fifteen grams of sieved
CPHs were soaked and boiled with different
volume of distilled water and duration
(minutes) for comparison; the treatments
were labelled as T1 to T3 in Table 1. The
series of formulated product obtained labelled
as T1 – T3, referring to the treatment applied
to the ground CPHs, prior to the formulation
stage.

Table 1: Treatment to CPH

Treatment
Sampl
Duration
e Total Volume of water used (ml)
(min)
T1 60 3 x 800
T2 180 1 x 800
T3 30 100 (Ethanol) & 2x100 (Methanol)

Sample labelled T1 was formulated Preparation of Cocoa Body Scrub

with CPH soaked three times with 800ml of
distilled water and boiled for 60 minutes each
times. For sample labelled T2, the CPH was
treated with 800ml distilled water and boiled
for two hours. T3 was formulated with CPH
soaked with 100mL of 70% ethanol (boiled)
for depigmentation, followed by 2x100mL of
70% methanol for gum removal. Finally, the
treated CPHs were weighed after removal of
excess water/solvent by drying in the oven.
The formulation is based on Williams (1992)
but the mineral oil was replaced with cocoa
butter and polyethylene beads with ground
CPHs. Cocoa body scrub formula is
summarised in Table 2. Part A is water phase
and part B is the oil phase, while part C
represents the miscellaneous ingredient as in
this case ground CPH and fragrance.

Table 2: Formulation of Cocoa Body Scrub

Ingredients Function Weight percentage, wt%
Part A Cocoa body scrub Williams (1992)
Water, Deionised To dilute 50.0 - 60.0 48.35
Thickener To thicken the formulation 0.50 – 1.00 4.0
Preservative To preserve 0.50 – 1.00 0.1
Surfactant Ease of washing after application 5.0 – 10.0 3.0
Part B
Cocoa butter Emollient 15.0 – 25.0 20.0
Emulsifier To emulsify the water and oil phase 4.0 – 5.0 10.0
Sorbitol Humectants 3.0 – 3.5 10.0
Glycerin Humectants 3.0 – 3.5 1.0
Part C
Ground cocoa pod husk Exfoliating particulate 425 µm 1.0 – 2.0 5.0
Fragrance Odour properties of the product q.s 8.5
Total 100.00 100.00

To make the cream, melt cocoa
butter prior to the addition of sorbitol,
glycerin and emulsifier, and heated to 75 oC.
Separately, in another beaker, thickener was
soaked in deionised water until hydrated prior
to the addition of preservative and heated to
75oC. Then, part B was poured into part A
and homogenized for 15 minutes. The
mixture was then cooled down to 40oC with
continuous agitation before the addition of
part C, then promoted into container and left
for 24 hours or overnight to set. After this,
the physical properties of the cosmetic
product were measured, initially, to make sure
the formula is well set and the ingredients
were mixed and structured very well.
Freeze/thaw and Accelerated Stability Study
During freeze-thaw cycle, the products were
placed in the freezer for 24 hours, followed
by cooling down to room temperature prior to
oven heating at 45oC and then cooling down
again to room temperature to complete one
cycle. The cycle was then repeated severally,
where the minimum amount of cycles for a
stable product is three and five cycles
maximally (Klein, 2007). Then, the physical
properties, i.e. viscosity and pH of the
product is measured and recorded. In
addition, the odour and colour change of the
product was observed.
Consequently, the product was also
placed in an oven at 45oC as accelerated
stability study. The container or jar was put
in several positions for three months of
storage. The measurements was recorded at
initial, 1-4 week of storage and finally after
two and three months of storage. The
physical properties of the product, i.e. pH and
viscosity (cP) were recorded.
Sample labelled from T1-T3 were
placed in the oven at 45oC in several
positions for three months. Measurement of
pH and viscosity were carried out at initial,
every week for the first month and followed
by the end of the second month and third
month. pH measurement was carried out
using a pH meter, where one gram of each
samples were diluted with nine grams of
deionised water prior to the measurement.
The viscosity was determined using
Brookfield DVII at 45oC, with spindle
number 27. Other additional physicals
changes e.g. colour and odour was also
observed.
Statistical analysis - Analysis of means was
used to observe any difference in pH and
viscosity value of samples over the time with
significant level at p<0.10 using Minitab.
RESULTS & DISCUSSION
Incorporation of cocoa butter into cosmetic
product require proper handling and
processing, especially correct formulation
temperature and right amount in the
formulation. Although the defect of the
product can be masked in several ways, such
as addition of thickener and fragrances, a
better product can be achieved by the right
ingredient amount and temperature to obtain
the beneficial of natural products.
This cocoa butter body scrub as an
emulsion product would needed an emulsifier
to prevent separation or instability of the
product. Stability of the emulsion product is
also enhanced by the addition of adequate
amounts of thickener. The thickener slows
down the thermodynamically breakdown of
the emulsion and also exhibit emulsifier
behaviour due to their interaction with the
water portion in the formulation.
Nevertheless, separation of water
from oil phase, or vice versa, is also
prevented by heating hot oil and water phase
75oC prior to combination of oil and water
phase, during mixing in the homogenization
process. These actions are important in
achieving the stable emulsion. During
homogenization, the oil phase is turned into
small droplets where it can stay longer in
water phase.
Consequently, the heating process
before mixing is purposely to obtain the same
liquid temperature between the phases so that
the stable structure can be developed. In
addition, improper mixing and heating
process for the cocoa butter product can lead
to the blooming of the product as it happens
in chocolate making. Blooming effect
occurred when the crystalline structure of the
cocoa butter is not well-formed during the
formulation. Figure 1 shows the blooming of
cocoa body scrub due to improper processing
during formulation.
 Figure 1: Blooming of Cocoa Body Scrub

Initially, the cocoa body scrub was the untreated ground CPH has various
formulated with the untreated ground CPHs, particle sizes. This is also caused the
where the ground husks were incorporated grittiness as well as off-odour during
directly. The product became slimy and application. However, after the application of
brownish due to the resin compound in the CPH treatment, the final product appear to
CPHs that was expelled over time in the have white base with ground CPHs can be
presence of water in the formulation. At the evenly spread in the product, which was more
same time the product had uneven texture as appealing (Figure 2) and acceptable.

Before CPHs pre-treatment After CPHs pre-treatment

Figure 2: Cocoa Body Scrub

Sample T1 can be categorised as of sample T2 and T3 was summarised in

stable product by freeze/thaw cycles, where Table 3. By analysis of means, pH and
the pH and viscosity where showed no viscosity of sample T2 and T3 were varied
significant different during the first three significantly. Therefore, the samples were
cycles in Figure 3a and Figure 3b, not stable.
respectively. Mean value of pH and viscosity

One-Way ANOM for C40 by C39 One-Way ANOM for C29 by C28
Alpha = 0.1 Alpha = 0.1

4.5 12000

11770
4.4170
4.4
11500

4.3192
Mean

Mean

4.3
11088
11000

4.2213
4.2

10500
10405
4.1

0 1 2 3 4 5 0 1 2 3
C39 C28

(a) Analysis of means pH for T1 (b) Analysis of means viscosity for T1

Figure 3: Analysis of Mean for Sample T1

Table 3: Freeze/Thaw cycles for cocoa body scrub

 Mean pH Mean viscosity
Sample Sample
Cycl T1 T2 T3 T1 T2 T3
e
0 4.35* 4.18 4.22 10650* 17550 21250
1 4.35* 4.09 4.14 10500* 17050 16650
2 4.25* 4.26 4.38 11750* 19050 20250
3 4.41* 4.17 4.14 11450* 14750 8650
4 4.43 4.17 4.19 12750 20210 15260
5 4.13 4.04 4.17 11500 10250 5050
* Not significantly different

Results of accelerated stability test months at room temperature. Meanwhile, for

for sample T1, T2 and T3 were tabulated in
Table 4. The pH of all the product remains at
6 throughout the study which indicated no
chemical reaction occur between the cream
based and the ground CPH although different
treatment were applied. However, by
analysis of mean, the formulation showed
instability of viscosity obtained along the
study.
According to Arrhenius equation on
shelf-life of a product by accelerated stability
method, product that stabled at 50oC for one
month is predicted to have a shelf-life of eight
a product with stable condition at 40oC in
three month has the shelf-life of one year. In
this study, the product is put in an oven at
45oC for three months, to predict the shelf-life
of fifteen months.
Nonetheless, T1 exhibited stable
viscosity until the second month. The
stability shown insignificant different (p =
0.10) between the viscosity value of week 2,
3 and 8. However, the product became more
viscous after the third month, which means
the product was predicted to be stable for ten
months.

Table 4: Accelerated Stability of Cocoa Body Scrub with Treated Ground Cocoa Pod Husk

Mean value of Mean viscosity (cP), Storage in Oven at 45oC

Sampl Initial After oven Week Week Week Week Week Week
Initial
e weight (g) dry(g) 1 2 3 4 8 12
T1 15.05 8.45 5,000 4,888 4,538 4,363 4,163 4,438 7,013
T2 15.05 9.48 7,275 7,125 6,813 6,850 5,563 5,513 8,638
T3 15.05 8.06 12,210 12,410 11,210 8,688 10,075 9,938 8,688
CONCLUSIONS
The body scrub cream with cocoa butter and
treated ground cocoa pod husk as main
ingredients should be process and made at
75oC would be able to have a shelf life of 10
months. The removed portion of cocoa pod
husk should be investigated to obtain other
potential cosmetic benefits. The shelf life of
product must be investigated in order to
guarantee the product can arrived to the
consumer hand without defects.
ACKNOWLEGDEMENT
I gratefully thank Ministry of Science,
Technology and Innovation for e-Science
Fund 05-03-13-SF0015.
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