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Sunscreen Cream Formulation with Natural Ingredients, including Arabic gum

and Beeswax Foundation

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 Sunscreen Cream Formulation with …..

Sirte University Scientific Journal(Applied Sciences) Vol.9(1) ,June 2019

Sunscreen Cream Formulation with Natural

Ingredients, including Arabic gum and Beeswax
Foundation
Fathia A. Mosa and Randah O. Makhlouf
e-mail: fathia@su.edu.ly

Department of Chemistry, Faculty of Sciences, Sirte University, Sirte, Libya

Abstract

The aim of this research was to develop sunscreen cream formulation with natural ingredients and
calculated sun protection factor (SPF) for it. The sunscreen is prepared using water phase that includes
distilled water as a main solvent, glycerine as a moisturizer, Arabic gum as a thickener, and citric acid as a
preservative. The oil phase is composed of one of the following oils: paraffin oil, olive oil, sesame oil or pond
oil, and beeswax foundation as emulsifier. Zinc oxide and titanium dioxide are both employed in sunscreen
as inorganic physical sun blockers. The best cream texture was obtained in the case of using beeswax
foundation as emulsifier by 8%. The best solubility of sunscreen cream is obtained using equal proportions
of hexane and ethanol. An in vitro SPF (sun protection factor) of used samples is calculated according to
Mansur’s method. Moreover, Mansur’s method calculates only SPF values of organic substances
(triglyceride oils) but physical sun blockers (zinc oxide and titanium dioxide) cannot be calculated by
Mansur’s method. By comparing SPF values for triglyceride oils, the best protection value is obtained using
olive oil. For other oils were found to be around 6. Therefore it can be founded that triglyceride oils have
absorbency in UV region so that these oils can be used in the formulation of sunscreens as emollients and
sun blockers. This formulation of sunscreen cream is focused on using natural ingredients, creamy texture,
and efficacy..

Keywords: SPF, Sun protection factor, Titanium dioxide, Zinc oxide, Olive oil, Triglyceride oils.

1. Introduction

There is agreement between the scientific and medical societies that exposure to sunlight is a main
reason to damage the skin.1 An electromagnetic radiation in sunlight called ultraviolet (UV).
Ultraviolet light is artificially divided into three ranges: UVA (320-400 nm), UVB (290–320 nm),
and UVC (200–290 nm)[1,2]. Sunscreens are the most common products that used for skin
protection against solar UVB radiation which causes sunburn, photoaging, skin cancer, formation

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 F. A. Mosa and R. O. Makhlouf

of telangiectasia, and pigmentation irregularities[2,3] Both UVA and UVB can cause sunburn,
photo ageing, erythema and inflammation.4 Generally, UVC does not have harmful effects on the
skin[2]

Sun blocking chemicals can be classified according to the type of protection they afford to the
following categories:

a. Inorganic (physical blockers)

The two primary inorganic UV filters are Zinc oxide (ZnO) and titanium dioxide (TiO2) white
particles which used in the cosmetic and pharmaceutical industries. 5 Moreover, Titanium dioxide
is somewhat more effective in UVB protection while zinc oxide absorbs more broadly in the UVA
range.6 Both these filters can block UV light through reflection and scattering properties (Figure
1)[6]. Their maximum concentration authorized is concentration of 25% in a UV filter.[5]

b. Organic (chemical absorbers)

Organic UV filters such as benzophenones, absorb UV radiation with excitation to a higher energy
state [7]. Excess energy is dispersed by emission of higher wavelengths or relaxation by
photochemical processes, for example isomerisation and heat release (Figure 1) [7]. Their
absorption range and their strength are affected by the chemical structure and type of substituents.5

c. Natural (chemical absorbers)

―Natural chemicals like polyphenols (flavonoids, tannins), carotenoids, anthocyanidins, few
vitamins, triglyceride oils, volatile oils from vegetables, fruits, medicinal plant parts (leaves,
flowers, fruits, berries), algae and lichens are more effective over synthetic chemicals which is due
to their long term beneficial effects especially against free radical generated skin damages along
with UV-rays blocking‖ [9]. Moreover, Oils have been a part of human lifestyles for ages, and
their safety has been evaluated by millions of users down through the centuries [8].

For designers and manufacturers of sunscreen requirements can be summarized in the following
four basic requirements[11, 12].

i. Effectiveness, choose the correct UV filters Mix and other key ingredients to accomplish
desired performance.
ii. Safety, whether objective or simply conceived by the media and the consumer,
iii. Registration, which is most important if the sunscreen, will be distributed to the world.
iv. Patent Freedom, i.e. "freedom of action" with respect to the third intellectual property rights
(IP)
The effectiveness of a sunscreen is usually expressed by sun protection factor (SPF) which is the
ratio of UV energy required to produce a minimal erythemal dose (MED) in protected skin to
unprotected skin [2]. High SPF numbers give the false impression they can provide enhanced

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protection when that is not the case.2 A well-formulated sunscreen with an SPF 30 still only
protects your skin from about 97% to 98% of the sun’s rays [2].

A simple, rapid and reliable in vitro method of calculating the SPF is to screen the absorbance of
the product between 290-320 nm at every 5 nm intervals. SPF can be calculated by applying
Mansur equation (1) [13-15].

Figure 1. Action mode of organic (left) and inorganic (right) UV filters.

2. Materials And Methods

.1.2 Chemicals and equipment:

Paraffin oil was purchased from Carlo Erba Reagents, Spain. Beeswax foundation was purchased
from Madybees, Egypt. Ethanol and hexane were purchased from BDH. Glycerine was bought
from Fluka chemika. Titanium oxide and Zinc oxide were purchased from Merk. All used natural
oils; citric acid and Arabic gum were purchased from local distributors in Libya and used without
further modification. Spectrophotometric determination of UV absorbance was carried out in 1 cm
path length cuvette (quartz), using JENWAY6305 UV/Visible spectrophotometer (single beam).
Samples mixing were carried out using Vortex mixer (Bio Cote). pH measurements were
performed using a pH Benchtop meter (Orion 2 star, Thermo Scientific)
1.1 Preparation of sunscreen product formulation
The sun protection cream was prepared on the basis of following percentages for the total weight

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 F. A. Mosa and R. O. Makhlouf

of the sample (5 gr) as shown in Table 1:

Table 1. The weights of each ingredient of sunscreen preparation are given as well as the
percentages of them to the total weight of sunscreen cream’s sample (5 gr)
Total Percentage Ingredient Name Percentage Weight

Water phase, total percentage = 68% Distilled water 58% 2.90 gr

Arabic gum 5% 0.25 gr

Glycerine 5% 0.25 gr

Oil, total percentage = 20% paraffin oil 20% 1.00 gr

Emulsifier, total percentage = 8% Beeswax foundation 8% 0.40 gr

Sunscreen, total percentage = 3.5% ZnO or TiO2 3.5% 0.18 gr

Preservative, total percentage = 0.5% citric acid 0.5% 0.03 gr

After the weighting of ingredients (Table 1), the following steps are taken:
i. Both of the water phase and the oil phase are heated separately to 70 °C for 15 minutes.
This will destroy any bacteria that may be present in both phases.
ii. The water phase is gradually added to the oil phase with the stirring. Then the solar blocker
and the preservative are added with good mixing using vortex.
iii. After cooling the cream pour into a box and close well and covered with a white tissue
until the measurement of SPF.
The pH of any cream or lotion can be tested and then pH level will be adjusted with adding citric
acid to be pH 6 to 6.5, which is the appropriate pH level for adult skin .

.1.2 Preparation of sunscreen sample for SPF measurements

122mg of each sample was weighed, transferred to a 100 mL volumetric flask, diluted to volume
with 50% hexane in ethanol and followed by vigorous vortexing. Then, it is filtered through filter
paper, rejecting the first 10 mL. A 5.0 mL aliquot was transferred to 50 mL volumetric flask and
diluted to volume with 50% hexane in ethanol. Then a 5.0 mL aliquot was transferred to a 50 mL
volumetric flask and the volume completed with 50% hexane in ethanol. The final concentration
of each diluted sample is 20 ppm in 50% hexane in ethanol.
The absorption spectra of samples in solution were obtained in the range of 290 to 320 nm using 1
cm quartz cell, and 50% hexane in ethanol as a blank. The absorption data were obtained in the
range of 290 to 320 (the range of UVB) every 5 nm.
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3. Results And Discussion

The preparation of the sunscreen depends on three main factors:

I. Emulsifier (chemical energy): A key factor to gather both water and oil phases together is the
emulsifier. Beeswax foundation is used as a main emulsifier in this research. It melts at about
60- 63 °C. It is chosen to form the emulsion and can also be used for emulsion stabilization.
II. Heat (thermal energy): Melting the solids in oil phase (bees wax foundation) to facilitate the
mixing with water phase’s ingredients by heating and mixing.
III. Mixing (mechanical energy): one of the most important factors that make creamy texture.
The used ingredients in the preparation of the sunscreen’s cream and their respective purposes
were briefly summarized in Table 2. Paraffin oil (mineral oil) is colourless and odourless. It
consists of light mixtures of higher alkanes.16 Emulsified mixtures of liquid paraffin make
excellent skin creams.16

Table 2. A brief summary about the ingredients that used in the preparation of the sunscreen
cream.

Ingredient Name Purpose Phase Typical

Use Level
Arabic gum It is stabilizer, dissolves in the water phase Aqueous 0.5-3%
and when mixed with the oil phase, it helps
to stabilize the emulsion over a long time.
Glycerine It is used as a humectant where helps to Aqueous 2-5%
retain moisture.
Beeswax Emulsifier and thickener Oil 3-10%
foundation
Stearic acid Thickener. Oil 3-10%
and palmitic acid
Triglyceride Oils Emollients. Oil 8-20%
Citric acid Preservatives. Aqueous 0.1-1%
Titanium Dioxide Inorganic sunscreens. Oil and 1-10%
and Zinc Oxide aqueous

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 F. A. Mosa and R. O. Makhlouf

3.1. Getting the best texture:

To obtain the best cohesive creamy texture, the previous ratios in Table 1 were adjusted as well as
the percentage of water and emulsion were varied, as shown in Table 3, to obtain a good texture.

Table 3. Attempts to get the best creamy texture.

Ingredient Name Texture 1 Texture 2 Texture 3 Texture 4 Texture 5

Distilled water 85% 85% 85% 85% 85%
Beeswax foundation 4% 5% 9%
Stearic acid 4% 5%
Palmitic acid 5%
Paraffin oil 02% 02% 02% 02% 02%
Arabic gum 8% 8% 8% 8% 8%
Glycerine 8% 8% 8% 8% 8%
Zinc oxide 5.8% 5.8% 5.8% 5.8% 5.8%
Citric acid 2.8% 2.8% 2.8% 2.8% 2.8%

In Texture 1, mixing of stearic acid with beeswax foundation in equal ratios led to the light texture.
Likewise, when fatty acids were used as emulsifiers (Textures 4 and 5), it also led to a lighter
texture which is not coherent to the required degree of creamy texture. Furthermore, the best cream
texture was obtained in the case of using only beeswax foundation as emulsifier by 8% (Texture
2). While in the case of texture 3, in which the proportion of emulsion in the oil phase (9%) is
increased, and the proportion of water (57%) is reduced, that led to solidify the cream to undesired
texture. Consequently, texture 2 was used as the main texture for the preparation of samples (A to
J) in this research.

3.2. Preparation of samples:

The sun protection samples were prepared with fixed ratios for the substances that mentioned in
Table 4. Only the used oils, which included olive oil, pond oil, corn oil and sesame oil, were
adjusted (Table 5) to test the effect of these oils on the sun protection’s values.

Table 4. Ingredients that are used with fixed percentages in samples preparation (A to J).

Ingredient Distilled Arabic Glycerine Citric Beeswax ZnO or

Name water gum acid foundation TiO2
Percentage %88 8% 8% 2.8% 8% 5.8%

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Table 5. Percentage of oils and inorganic sun-blockers (ZnO and TiO2) that are used in the
preparation of samples A to J.

Ingredient A B C D E F G H I J
Name
Paraffin 20% 20%
oil
Corn oil 02% 02%
Sesame 02% 02%
oil
Pond oil 02% 02%
Olive oil 02% 02%
ZnO 5.8% 5.8% 5.8% 5.8% 5.8%
TiO2 5.8% 5.8% 5.8% 5.8% 5.8%

These oils in samples (C to J) contain unsaturated fatty acids, in which there is at least one double
bond in their structures so that they can absorb wavelengths from 290–320 nm to achieve the
desired SPF. These purified oils are used in approximately 20% as emulsions and sunscreens.

3.3. Solubility of sunscreen cream:

To obtain the best solubility of the prepared samples, a different mixtures of ethanol (polar
solvent) and hexane (non-polar solvent) were used as shown in Table 6 (entries 1-4). In brief, the
best solubility of sunscreen cream is obtained using equal proportions of hexane and ethanol (entry
3).

Table 6. Results of the solubility of sample of sunscreen cream.

Entry Solvent mixtures Solvents ratios Observation

1 Hexane : Ethanol 1:4 Very little solubility
2 Hexane : Methanol 2:3 little solubility
3 Hexane : Ethanol 2.5 : 2.5 Good solubility
4 Ethanol : Water 1:4 Very little solubility
5 Hexane : Ethanol : Water 2.5 : 2 : 0.5 Two separate layers

3.4. Calculations of pH for sunscreen samples:

The acidity of some samples (Table 7) can be attributed to the use of citric acid as a preservative in
the preparative method. Acidification can be adjusted with the addition of a small percentage of

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 F. A. Mosa and R. O. Makhlouf

sodium bicarbonate while, the basicity can be adjusted with the addition of small amounts of citric
acid.

Table 7. PH values for samples (A to J).

Samples A B C D E F G H I J
PH 5.52 8.25 5.24 5.09 5.05 7.34 5.31 5.57 5.04 5.00

Calculations of solar protection factor (SPF)

The absorbance of prepared solutions (20 ppm in 50% hexane in ethanol) is measured in the range
of 290-320 nm, each time the wavelength range is changed by 5 nm in each measurement. The
Mansur mathematical equation (1) is used to calculate the SPF values of the samples (A- J).13-16

∑ ( ) ( ) ( ) ( )

Where: CF is the correction factor (=10); ―EE‖, the erythemal effect of radiation at wavelength λ;
―I‖, the intensity of the solar spectrum; and ―ABS‖, the absorbance at wavelengths 290-320 nm.
―EE‖, ―I‖, and ―ABS‖ are values obtained or applied for every wavelength (λ). The values for each
of the [EE(λ) x I(λ)] are constants have been reported by the authors as normalized on the basis of
the work by Sayre et. al., and are shown in Table 8.13-15

Table 8. The values of EE x I as they were determined by Sayre et al (1979).

Wave length (nm) 290 295 300 305 310 315 320
EE x I 0.0150 0.0812 0.2874 0.3278 0.1864 0.0837 0.0180

Appling absorbance values in Mansur equation (1) to calculate the SPF values for these prepared
samples (A-J) is shown in Table 9.
Table 9. The SPF values for prepared samples (A-J).
Samples Active ingredients (organic filter and inorganic filter) Calculated SPF
A Paraffin oil and zinc oxide 6.84
B Paraffin oil and titanium oxide 6.22
C Corn oil and zinc oxide 6.74
D Corn oil and titanium oxide 6.01
E Sesame oil and titanium oxide 6.20
F Sesame oil and zinc oxide 6.81
G Pond oil and titanium oxide 6.15

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 Sunscreen Cream Formulation with …..

H Pond oil and zinc oxide 6.10

I Olive oil and zinc oxide 7.03
J Olive oil and titanium oxide 7.11

It can be observed from Table 8 that the SPF values found for triglyceride oils were in between 6
and 7. By comparing SPF values for triglyceride oils, the best protection value is obtained using
olive oil with both inorganic filters (zinc oxide or titanium oxide) as shown in both Figures 2 and
3. For other oils were found to be around 6. Therefore it can be founded that triglyceride oils have
absorbency in UV region so that these oils can be used in the formulation of sunscreens as
emollients and sun blockers.

7
6.8
6.6
SPF

6.4
6.2
6
5.8
Paraffin Olive oil Pond oil Sesame Corn oil
oil oil
Used oils with zinc oxide

Figure 2. Relationship between SPF values and the used oil with inorganic filter Zinc oxide.

7.5
7
6.5
SPF

6
5.5
5
Paraffin Olive oil Pond oil Sesame Corn oil
oil oil

Used oils with titanium oxide

Figure 3. Relationship between SPF values and oil used with inorganic filter titanium oxide

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 F. A. Mosa and R. O. Makhlouf

4. Conclusions

The preparation of a sunscreen cream carried out using inorganic filters and five kinds of different
oils. These fixed oils can be formulated in the form of cosmetics formulation due to their superior
acceptability, less irritant nature and also these are less costly. The used beeswax foundation is less
costly and available. The used Arabic gum is completely nature and inexpensive. The preservative
was citric acid and no organic filter was used except triglycerides oils. The used
spectrophotometric method, to calculate SPF, is an inexpensive and easy to apply. Moreover, this
method can calculate SPF for organic filters but it cannot used to calculate SPF values for
inorganic filters, such as zinc oxide and titanium oxide, as an active ingredient. Then, this
spectrophotometric method evaluates only cosmetic product that contains organic filters.

5. Recommendations
To a prepare a cream must be the availability of certain conditions, including a good emulsion,
pure oil (free of impurities and odorless) and high speed mixer to obtain the best texture. One of
the best shakers recommended is Silverson Mixer. It is also preferable to measure the viscosity of
the cream produced using the viscometer.

References
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