CHAPTER 3

METHODOLOGY

This chapter includes the type of research design, the materials and equipment
used in the experimentation, protective and safety measures, the deliberation of the
data collection procedure, and the statistical treatment of the study. This chapter allows
the process of experimentation and evaluation to be assessed for purposes of validity.

3.1 Research Design

In line with the research study’s objectives, which are to formulate a natural
facial moisturizer and to distinguish the differences between the varied ratios of GLE
and CW at different parameters, true experimental design was administered. True
experimental design contains three important factors: independent and dependent
variables, pretesting and post-testing, and experimental and control groups (DeCarlo,
2018). It is said to be the most accurate type of experimental research, as it supports
or refutes a hypothesis with the use of statistical analysis.

Since pretesting was not necessary in the study, a specific type of true
experimental design was adhered, which was the posttest-only control group. This
research design has at least two groups, the experimental group and control group.
The latter did not receive any treatment or intervention. Data were collected on the
outcome measure only after the application of treatment. In the study, the experimental
group was the five formulations of facial moisturizers treated with varied ratios of GLE
and CW, 1:9, 3:7, 1:1, 7:3, and 9:1. The control group was the pure formulation without
GLE and CW. Random samples of the moisturizer from the groups were then post-
tested for the different parameters, which were physical appearance, pH value, scent
acceptability, and spread ability. In the experiment, there were three (3) trials for each
formulation in order to secure more reliable results.

3.2 Research Environment and Setting

The collection of guava leaves and coconut water and dried guava leaves
extraction were conducted in one of the researchers' residence located at Brgy. Dos,
Katipunan, Zamboanga Del Norte. The coconut water was collected one day earlier
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and was stored in the refrigerator, while the drying and extraction of guava leaves was
done one week before the formulation of skin moisturizer.

The formulation of facial moisturizer was conducted in the same location,

specifically in the kitchen, where the materials and other equipment needed for the
experiment were readily available.

The finished formulations of facial moisturizer were evaluated through their

physiochemical and organoleptic properties in a range of three days, including the day
of formulation. Moreover, for the scent acceptability property, five of the researchers
divided an adequate amount of the finished formulations. In their own convenience,
each researcher was allocated with a specific number of respondents within their
community to smell and rate the product. In total, there were 50 individuals who
willingly participated.

3.3 Ethical Considerations

This research study was conducted with the adherence of the important
principles of ethics. With this, respect and confidentiality of identity was the prime
priority of the researchers as they conversed with the respondents. A letter was given
beforehand to ask for the respondents’ permission. They were informed regarding on
the details and steps they will have to undergo before the evaluation of scent
acceptability. Their participation on the study was from their own will and can anytime
withdraw from it.

3.4 Instrumentation and Materials

The formulation of skin moisturizer from guava leaves extract and coconut
water made use of necessary materials and equipment.
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3.4.1 Materials Used for Guava Leaves Extraction

• Dried Guava Leaves

Dried guava leaves were vital for this process as the leaves were extracted for the
formulation of facial moisturizer. It was limited for about nine (9) grams only.

• Glycerin

The glycerin was used as a solvent to extract dried guava leaves and as a
natural preservative. This was directly mixed with the dried guava leaves. 90 mL of
glycerin were used in total.

3.4.2 Tools Used for Guava Leaves Extraction

• Metal Strainer
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A metal strainer was utilized to separate the liquid extract from the pieces of

guava leaves in the mixture.

• Measuring cups

It was used to accurately measure the liquid ingredients.

• 3 mL Syringe

It was used to measure smaller amounts of liquid ingredients.

• Scissors
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Researchers used scissors for cutting the guava leaves into smaller pieces for

easier blending.

• Blender

An electric blender was used to get a powder-like texture of dried guava leaves.

• Stove

It was utilized to heat the mixture of guava leaves and glycerin, specifically in

a low heat temperature for about 10 minutes.

3.4.3 Materials used for Skin Moisturizer Formulation

• 60 mL Guava Leaves Extract

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• 60 mL Young Coconut water

Photo by Any Lane from Pexels

• 144 mL Pure Glycerine

In water phase, these liquid components were mixed together in a ceramic

mixing bowl.

• 132 mL Shea Butter

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• 30 mL Emulsifying wax

• 144 mL Coconut oil

• 30 mL Vitamin E Oil
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• Essential Oil (Vanilla Essence)

In oil phase, these five components were mixed together. The shea butter was
melted with a hot water bath beforehand. Emulsifying wax is a cosmetic emulsifying
ingredient that was used to give the cream a smooth consistency.

• 12 mL Phenoxyethanol Cosmetic Preservative

For any cream products that contain water in the ingredients, a preservative
was necessary to prevent nasty mold and bacteria growing in the mixture.

3.4.4 Tools used for Skin Moisturizer Formulation

• Measuring cups
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It was used to accurately measure the liquid ingredients.

• 3 mL Syringe

It was used to measure smaller amount of liquid ingredients.

• Spatula

A plastic spatula was used to stir the mixture thoroughly.

• Aluminum foil

Aluminum foil was used to seal the bowl with the mixture inside before it was
placed into a freezer for about three (3) minutes.

• Glass jars

Photo by OpenClipart-Vectors from Pixabay

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Labeled glass jars were essential for the safe storage of the varied ratios of
facial moisturizer formulations.

• Blender

An electric blender was used to fully emulsify water and oil phases together.

3.5 Personal Protective Equipment

For the researchers' health and safety, the following were the amenities used
and worn that have protected them from risks in the entire course of the
experimentation:

• Laboratory Gown

In the processes of guava leaves extraction and facial moisturizer formulation

and evaluation, the researchers wore a laboratory gown to protect their skin from
accidental contact and minor splashes.

Photo from Pngall

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• Face Mask

This was worn to cover the nose and to prevent the inhalation of the unpleasant
scent that can possibly cause serious problems if directly inhaled.

Photo by Engin Akyurt from Pexels

• Laboratory Gloves

A pair of laboratory gloves was essential for the protection of the hand during
the experimentation.

Photo by Sora Shimazaki from Pexels

• Safety glasses/ Goggles

Safety glasses or goggles acted as a protective to protect the eyes from a

sudden strike of particulates, water, or chemicals.

Photo by Mier Chen from Pixabay

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3.6 Data Collection

Pre-designed procedures from related literature and studies were conducted to

attain the study’s goal in evaluating all the formulations’ physiochemical and
organoleptic properties. Some procedures were manipulated and adjusted depending
on the researchers’ preferences and the availability of materials and equipment.

For the determination of pH value, the standard procedure with pH paper and
scale was followed. For spread ability, samples were placed in between two glasses
and the final diameter reached by each sample after application of weight was
measured by a caliper. The physical appearance was based on the researchers’ visual
evaluation. Lastly, the scent acceptability was determined through 50 individuals’
sensory analysis and 5-point hedonic scale rating.

The data gathered were tabulated and interpreted through a statistical tool.
Since there were more than two means of samples within each group that were
compared, One-way Analysis of Variance (ANOVA) was used to determine whether to
accept or reject the null hypothesis. When the null hypothesis for each parameter was
rejected and over-all significant difference existed between groups, researchers run a
follow-up or post-hoc test, which was the Tukey’s Honestly Significant Difference test.
This test revealed where exactly the significant difference exists between groups.

3.7 Process of Experimentation

3.7.1 Extraction of Guava Leaves

1. Guava leaves were collected and cleaned with clean, running water.

Figure 2. Cleaning of Fresh Guava Leaves

2. The leaves were then sun dried for 24 hours.

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(a) (b)

Figure 3. Sun Drying of Guava Leaves (a) 1st hour (b) 24th hour

3. After 24 hours, the dried guava leaves were cut into pieces and blended to
have that almost powder-like texture.

Figure 4. Blending of Dried Guava Leaves

4. Nine (9) grams of the powdered guava leaves were mixed with 90 mL of pure
glycerin in a glass jar.
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Figure 5. Mixing of Powdered Guava Leaves and Glycerin

5. The mixture was placed on a stove and was heated in a low heat temperature
for 10 minutes.

Figure 6. Heating of Mixture

6. After heating up the mixture, it was strained with a metal strainer to separate
the excess leaves and the extract.

Figure 7. Straining the Guava Leaves Extract

7. The final extract was stored in a glass jar for one week before usage.
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Figure 8. Storage of Guava Leaves Extract

3.7.2 Formulation of Facial Moisturizer

Water Phase

The process in the water phase for all formulations were the same, however
the amount of ingredients was varied according to the assigned ratio of GLE and CW.

1. Control Group (Pure formulation)

A mixture of 68 mL of distilled water and 24mL of vegetable glycerin was

stirred together in a ceramic mixing bowl.

2. Experimental Groups (With GLE:CW)

Forty-four (44) mL of distilled water, 24 mL of GLE:CW mixture, and 24mL

of vegetable glycerin were thoroughly stirred together in a ceramic mixing bowl.

GLE-CW Mixture:

1:1 : 12mL GLE and 12 mL CW

1:9 : 2.4 mL GLE and 21.6 mL CW

3:7 : 7.2 mL GLE and 16.8 mL CW

7:3 : 16.8 mL GLE and 7.2 mL CW

9:1 : 21.6 mL GLE and 2.4 mL CW

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Figure 9. Water Phase

Oil Phase

The process and ingredients in oil phase were identical in all formulations.

1. 150 g of shea butter will be melted on a hot water bath.

Figure 10. Melting of Shea Butter

2. Twenty-two (22) mL of melted shea butter, 24mL coconut oil, and 5mL Vitamin
E oil were mixed in a separate ceramic mixing bowl.
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Figure 11. Oil Phase

3. The water phase was then slowly added to the oil phase using an electric
blender and emulsifying wax to basically unite the water and the oil together.
The researchers let the mixture sit for one (1) minute to cool down and thicken.

Figure 12. Emulsification of Water and Oil Phases

Cool Down Phase

1. In this phase, 5-10 drops of fragrance oil and 2mL Phenoxyethanol cosmetic
preservative were added.
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Figure 13. Addition of Fragrance and Preservative

2. The formulation was then transferred to a metal bowl and mixed thoroughly.

Figure 14. Thorough Stirring of Mixture

3. After mixing, the bowl was sealed with an aluminum foil and placed in a freezer
for three (3) minutes to thicken.

Figure 15. Three-minute Refrigeration of Mixture

4. The mixture was then stirred again continuously using a plastic spatula to get
the thick and cream-like consistency. Steps three and four were repeated twice.
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Figure 16. Final Stirring of Thickened Mixture

5. Lastly, the final mixture of moisturizer was stored in a labeled glass jar.

Figure 17. Storing of GLE and CW Moisturizer

3.7.3 Evaluation of Facial Moisturizer

All the formulated moisturizers were characterized for the parameters, such as
physical appearance, pH value, spread ability, and scent acceptability.

Physical Appearance

1. The physical appearance was evaluated into three categories, which were
opacity or transparency, color, and phase change.
2. Opacity or transparency and phase change were evaluated through visual
inspection.
3. The color was described through a digital color picker, in order for the
researchers to provide more specific terms for the color.
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Figure 18. Color Picker App

4. In this procedure, the formulations that were stored in a glass jar were placed
in a naturally-illuminated room.
5. A phone camera was focused on the sample until the application identified its
exact color.

(a) (b) (c)

(d) (e) (f)

Figure 19. Color Identification (a) Control group (b) 1:1 (c) 1:9 (d) 3:7 (e) 7:3 (f) 9:1

pH Value

1. The pH of the moisturizer was determined by directly soaking the pH paper in

the six different formulations without dilution.
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Figure 20. Soaking of pH Paper in the GLE and CW Moisturizer

2. After that, the researchers placed the pH paper on a clear plastic film with label
and waited for an hour to observe any changes in its color depending on
formulation’s level of acidity.

Figure 21. One Hour Observation of the pH Paper

3. The resulting color was compared to the pH color chart to know its equivalent

pH value.

(a) (b) (c)

 (d) (e) (f)
Figure 22. Comparison of pH Paper and Color Chart (a) Control group (b) 1:1 (c) 1:9
(d) 3:7 (e)7:3 (f) 9:1

Spread Ability

1. The spread ability of the formulation was determined by placing a glass plate
over a paper with a printed circle shape, which is 3.81 cm in diameter.

Figure 23. Set-up for Spread Ability Test

2. Three (3) ml sample of the moisturizer was carefully syringed on the glass
plate, following the outline of the circle.

Figure 24. Placing of Samples Inside the Circle

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3. The sample was squeezed by placing another glass plate above the ground
plate.

Figure 25. Adding of Weight on the Sample

4. The resulting increase of diameter after 30 seconds was measured by a

calliper.

Figure 26. Measurement of the Resulting Diameter

Scent Acceptability

1. Untrained individuals from three barangays of Dapitan City, one in Katipunan,

and in Manukan were assigned to assess the scent acceptability of the
formulations. Convenience sampling technique was used in choosing these
individuals for the researchers’ own convenience, since they were only allowed
to go outside in a specific range of time and areas, due to the pandemic. The
school could also not be a source of respondents, since students were not
allowed in the premises. This type of sampling method relies on the availability
and accessibility of respondents. However, not all qualified individuals in the
supposed target population were given equal opportunity to be chosen and the
results were not enough to generalize the population. So, the researchers
increased the sample size to a total of 50 individuals to increase the statistical
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power of the convenience sample. The researchers have set a specific

standard for the involved respondents. All respondents were aged 13 years old
and above and were current consumers of moisturizing cream products during
that time of evaluation.

(a) (b) (c)

Figure 27. Assessment of Scent Acceptability by Chosen Respondents (a) Taguilon,

Dapitan (b) Manukan (c) Ma. Uray, Dapitan

2. All of them were given a consent form beforehand, which includes the
objectives of the study and a detailed overview of what they will do as
respondents for the scent acceptability test.
3. 5-point hedonic scale was the basis of the scent acceptability evaluation.

3.8 Waste Management

Guava processing generates large amounts of waste with great potential for
recycling as a slow-release nitrogen fertilizer. In an agro-ecosystem approach, guava
waste should be recycled to sustain plant nutrition over several guava production
cycles. Hence, after the extraction of guava leaves, the remains were all buried on the
ground for soil nutrition.

For the collection of coconut water, most parts of the fruit will be put into waste
if not utilized based on its benefits. Coconut shell has a lot of benefits. It can be used
for making charcoal and coconut shell powder. If further manufactured, it can be a
source of activated carbon used for purification of fruit juices, oils, and water. The husk-
coir, on the other hand, can be converted into a potting for plants. It is a great addition
to soil for its capacity to absorb nutrition that goes directly to plants. Lastly, the coconut
meat is edible and can be eaten fresh or processed. The researchers only utilized the
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coconut shell with husk-coir for soil nutrition and consumed the fresh coconut meat,
since other processes could not be adhered due to limited skills and equipment.

3.9 Health and Safety

Considering possibilities of danger and for the safety of everyone, the

researchers primed safety protocols and guidance before going through the
formulation and evaluation of facial moisturizer. Personal protective equipment (PPE),
particularly the laboratory gown, face mask, gloves, and safety glasses, were required
for the researchers to wear to ascertain safety during the said experimentation.

3.10 Research Flow Chart

Start

Collecion of Raw
Materials

Drying and
Extraction of Guava
Leaves

7-day Storage of
Extract

Formulation of
Facial Moisturizer

Continuous stirring
until it forms a
cream-like
consistency

Evaluation of Facial
Moisturizer

Collection and
Analysis of Data

Figure 28. Research Flow Chart