Thesis psm2 (moist natural lipstick based on virgin coconut oil) by Juliana Shaibun

MOIST NATURAL LIPSTICK BASED ON VIRGIN COCONUT OIL (VCO)

JULIANA BINTI SHAIBUN

A thesis submitted in fulfilment of the requirements for the award of the degree of Bachelor of Engineering (Chemical - Bioprocess)

Faculty of Chemical Engineering Universiti Teknologi Malaysia

JUNE 2013

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Authorâ&#x20AC;&#x2122;s full name :

JULIANA BINTI SHAIBUN

Date of birth

4th APRIL 1989

Title

MOIST NATURAL LIPSTICK BASED ON VIRGIN COCONUT OIL

Academic Session :

2012/2013-2

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â&#x20AC;&#x153;I declare that this thesis entitled Moist Natural Lipstick Based on Virgin Coconut Oil (VCO) is the result of my own research except as cited in the references. The thesis has not been accepted for any degree and is not concurrently submitted in candidature of any other degreeâ&#x20AC;?.

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I dedicated this entire work to my beloved family, friends and who always be my side… For all their love, support, inspiration and encouragement … Thanks …

ACKNOWLEDGEMENT

I would like to express my gratitude and appreciation to all those who gave me the possibility to complete this proposal. I would like to express my deep gratitude to Prof. Dr. Mohamad Roji Sarmidi, my research supervisors, for his patient guidance, enthusiastic encouragement and useful critiques of this research work.

I would also like to acknowledge with much appreciation the crucial role of Mdm. Norhayati Mohamed Noor who is willing to give me her helping hand in provides valuable information and guidance.

Last but not least, I would like to grateful to my family for their support during the completion of this proposal. Their support has made me brave and persistent to complete this proposal. They helped me by giving me ideas which are inspiring me. Moreover, I would like to thank to my beloved friends who gave me support and help in this project.

ABSTRACT

Virgin coconut oil, known as VCO, is pure oil extracted from fresh coconut meat by mechanical or natural means, with or without using heat. This research involved the formulation of organic lipstick by using Virgin coconut oil, refined coconut oil, cocoa butter, beeswax, vitamin E, vanilla essence, color pigment and hydrogenated palm oil. The physical properties of lipstick such as melting point are study based on consumer acceptance. Besides that, there have some test that we perform in order to investigate the stability of formulated lipstick. They are breaking load test, sensorial test and stability test. The formulation of the lipstick was carried out by using Design Expert 6.0.8 software. In this software Response Surface Method (RSM) was chosen to study on the percentage of the main factors of virgin coconut oil, beeswax and hydrogenated palm oil. A Box-Behnken design in Response Surface Method (RSM) was employed to study the effect of different formulation of lipstick. The formulation consists of natural ingredients was a physically stable cosmetic lipstick.

ABSTRAK

Virgin coconut oil, yang dikenali sebagai VCO, minyak tulen yang diekstrak daripada daging kelapa segar dengan cara mekanikal atau semula jadi, dengan atau tanpa menggunakan haba. Kajian ini melibatkan penghasilan gincu organik dengan menggunakan virgin coconut oil, refined coconut oil, cocoa butter, beeswax, vitamin E, vanilla essence, color pigment dan hydrogenated palm oil. Sifat fizikal gincu seperti takat lebur gincu dikaji berdasarkan penerimaan pengguna. Selain itu, terdapat beberapa ujian yang dilakukan dalam usaha untuk menyiasat kestabilan gincu. Antaranya adalah breaking load test, sensorial test dan stability test. Penggubalan gincu telah dijalankan dengan menggunakan perisian Design Expert 6.0.8. Dalam perisian ini, Response Surface Method (RSM) telah dipilih untuk mengkaji peratusan faktor utama virgin coconut oil, beeswax dan hydrogenated palm oil. Satu reka bentuk Box Behnken dalam RSM telah digunakan untuk mengkaji kesan penggubalan berbeza gincu. Penggubalan terdiri daripada bahan-bahan semula jadi adalah stabil dari segi fizikal.

vii

TABLE OF CONTENTS

CHAPTER

TITLE

PAGE

DECLARATION

DEDICATION

iii

ACKNOWLEDGEMENTS

ABSTRACT

ABSTRAK

TABLE OF CONTENTS

vii

LIST OF TABLES

LIST OF FIGURES

INTRODUCTION

1.1

Research Background

1.2

Problem Statement

1.3

Objective

1.4

Scope of the Study

LITERATURE REVIEW

2.1

Introduction

viii

2.2

2.3

2.2.1 The Epidermis

2.2.2 The Dermis

2.2.3 Subcutaneous Tissue

Formulation of Lipstick

2.3.1 Base Ingredients

2.3.1.1 Beeswax

2.3.1.2 Virgin Coconut Oil

2.3.1.3 Hydrogenated Palm Oil

2.3.2 Active Ingredients

2.3.2.1 Vitamin E

METHODOLOGY

3.1

Introduction

3.2

Preliminary Phase

3.2.1 Determination of the Range of Factor

3.2.2 Design of Experiments (DOE)

Sample Preparation

3.3.1 Material and Equipment

3.3.2 Experiment Procedure

Characterization of Lipstick Properties

3.4.1 Melting Point Measurement

3.4.2 Breaking Load Test

3.4.3 Stability Test

3.4.4 Sensorial Test

3.5

Optimization

3.6

Verification

3.3

3.4

Overview of Lip Structure

RESULT AND DISCUSSION

4.1

Introduction

4.2

Preliminary Phase

4.2.1 Determination of the Range of Factors

4.2.2 Design of Experiments (DOE)

Process Analysis

4.3.1 Model Development

4.3.2 Analysis of Melting Point of the Samples

4.3.3 Analysis of Breaking Load Point of the

4.3

Samples

4.4

4.3.4 Analysis of Sensory Score of the Samples

4.3.5 Response Surface Analysis

4.3.6 Analysis of Stability Test

Optimization

4.4.1 Numerical Optimization Formulation of

Lipstick

CONCLUSION AND RECOMMENDATIONS

5.1

Conclusion

5.2

Recommendation

REFERENCES

LIST OF TABLES

TABLE NO.

TITLE

PAGE

3.1

Equipments Used In the Experiment

3.2

Experiment Procedures

3.3

Melting point test procedure

3.4

Breaking load test procedure

4.1

Constraint of the component proportion

4.2

Sets of run conditions determined by the model and

their experimental response values 4.3

Box-Behnken experiments along with actual and predicted

values of responses 4.4

ANOVA table for breaking load test of samples

4.5

ANOVA table for melting point of samples

4.6

ANOVA table for sensory score of samples

4.7

The Solution of the Optimization of VCO Moisturizing Lipstick

LIST OF FIGURES

FIGURE NO.

TITLE

PAGE

2.1

Beeswax

2.2

Virgin Coconut Oil

2.3

Hydrogenated Palm Oil

2.4

Vitamin E

3.1

The product evaluation steps of Virgin Coconut Oil (VCO)

lipstick. 4.1

Normal-residual plots for breaking load point of VCO

lipstick 4.2

Predicted-actual plots for breaking load point of VCO

lipstick 4.3

Effects of hydrogenated palm oil, beeswax and VCO

composition on breaking load test 4.4

Normal-residual plots for melting point of VCO lipstick

4.5

Predicted-actual plots for melting point of VCO lipstick

4.6

Effects of hydrogenated palm oil, beeswax and VCO

composition on melting point 4.7

Normal-residual plots for sensory score of VCO lipstick

4.7

Predicted-actual plots for sensory score of VCO lipstick

4.9

Effects of hydrogenated palm oil, beeswax and VCO

composition on sensory score 4.10

Observation of stability test at storage temperature 4oC, 20-25 oC and 40-45 oC

CHAPTER 1

INTRODUCTION

1.1

Research Background

Cosmetics are products used to enhance the appearance of the human body. Cosmetics include skin-care creams, lotions, perfumes, powders, fingernails and toe nail polish, lipsticks, eye and facial makeup, colored contact lenses, permanents waves, baby products, hair colors, hair sprays and gels, baths oil, bubble baths, bath salts, butters, deodorants and many other types of products are in great demand in developing and developed countries [1]. Cosmetics improve the appearance and attractiveness of human body. This perception has led the cosmetic industry to become one of the most successful sectors worldwide. The cosmetic industry in Malaysia is known to be one of the most successful economic activities [2].

Lipstick is one of the decorative cosmetic products that command a unique market segment [3]. Lipsticks are the common color cosmetics used by women in their daily life. The essential factors are pleasant color, safety, smell, luster, stability, adhesion, and extensibility. Usually customers are concern more about the feel, color, and lasting effects of lipsticks [4]. It has been used for many years to impart color to the lips. The color help to define the mouth area while imparting cosmetic shades that are suitable with fashion trends. The vast ranges of colors of lipstick are derived edible pigments [5].

Every year, users are introduced with various new cosmetics products of the latest trend. Lipsticks contain a variety of emulsifiers, preservatives, emollients, colorants and binders [6]. The previous research proves that the quality of lipstick is directly linked to the basic materials that used in the formulation. By varying the ratio of the ingredient in formulation, the final product characteristics such as viscosity, melting point, texture and hardness of the lipstick can be specified [3]. Furthermore, the ingredients and basic materials used in cosmetic formulation become the most important criteria for consumers in choosing the cosmetic product, as their interest in health and safety awareness grew.

Virgin coconut oil (VCO) has recently become a more popular new material in the cosmetic industries [7]. VCO is defined as the oil obtained from the fresh and mature kernel (12 months old from pollination) of the coconut (Cocos nucifera L.) through mechanical and natural means. It is produce with the use of heat or without the application of heat provided that does not lead to alteration or transformation of the oil [8]. VCO has many benefits, which include the health benefits from the retained vitamins and antioxidants, the antimicrobial and antiviral activity from the lauric acid components. Besides that, the medium chain fatty acids are easily digestible [9]. VCO promotes the development of healthy lustrous skin and hair. A daily application of VCO will delay the onset of wrinkles. Instead of using lotions

with synthetic ingredients, VCO can be applied liberally to the skin to prevent it from drying or chafing. VCO acts as an excellent moisturising agent [10].

A new cosmetic product should be safe, stable and usable within the specified storage, shipping conditions and in addition to mishandling by consumers. In order to achieve this requirement, it is necessary that all new products must be subjected to product stability and compatibility studies conducted over an extended range of temperatures and based on environment condition. The period of stability studies is basically determinate by the expected product shelf life. The expiration time is used to indicate the time period during which 90 percent of the labeled amount of an active ingredient in a cosmetic product remains unchanged even influenced by chemical or physical reaction [11].

1.2

Problem Statement

At present, there is no data available on the stability of Virgin Coconut Oil as lip cosmetic or lipstick. The existing cosmetics products in the market are formulated with artificial fragrance, flavors and colors. The used of synthetic ingredients are known to cause sensitivities problem to some consumers [12]. Any high street lipsticks & Makeup contain ingredients like Octyldodecanol and Polybutene that have been reported as chemicals to be a potential skin, eyes and lungs irritant [13]. Lipsticks are often swallowed away by the user and hence it is imperative that health regulators have a microscopic look at the ingredients that contained in the lipsticks. Due to various adverse effects of available synthetic preparation, this study is to formulate a natural lipstick with minimal or no side effects [14]. Therefore, it is important that there is no unsafe chemicals are used as the lipstick product.

Nowadays, the consumer demands for cosmetic products of high quality, safe to be used or without any long or short term side effects to skin [15]. A common problem in pre-formulation of lipsticks is the optimization of the mixer composition in order to obtain a product with the required characteristic. Statistically, experimental design commonly used to overcome this problem. The primary aim of designing an experiment statistically is to obtained valid results at minimum of time, effort and resources [16].

As we know, our country weather is humid and hot, as a result, the lips can become chapped and look pale if we are not adequately protected. This is because, the lips skin does not contain melanin and hence there is little protection against the effect of sunlight [5]. Hence, lipstick formulation from Virgin Coconut Oil can be used to prevent the lips from becoming chapped due to its softening and moisturizing ingredients. Therefore, the focus of the study is in the lipstick formulation by using natural cosmetic ingredients.

1.3

Objective

The objective of the study is to establish the formulation of Virgin Coconut Oil (VCO) based moisturizing lipstick.

1.4

Scope of Study

To achieve the objective, the following scopes have been identified in this study, they are:

a) Lipstick formulation based on Virgin Coconut Oil. b) Study the melting point of the lipstick. c) Perform breaking load test, sensory test for human volunteers and heat test.

CHAPTER 2

LITERATURE REVIEW

2.1

Introduction

This chapter reviews the previous studies related to Virgin Coconut Oil (VCO) and formulation of lipstick by using natural ingredients. The overview of the human lips structure is also reviewed to learn about the roles of lipstick. Besides that, all the base and active ingredient that used in lipstick formulation are reviewed to determine the function of each ingredient. Moreover, the stability tests methods such as Heat Test (Melting point), Sensory Test and Breaking Load test are studied so that the product has reduced adverse effect before reaching to consumers.

2.2

Overview of Lips Structure

Knowledge of human lips structure is important to develop a new lip cosmetic and lip-care product. Lips are a visible body part of the mouth and they are soft and serve as the opening for food intake and in the articulation of sound and speech. Even though the lips look different from the rest of human skin, but both of structures are quite similar. The structures are consists of epidermis and dermis layers. The upper and lower lips are known as the "Labium superius oris" and "Labium inferius oris", respectively. Lip skin is different which do not have the same protective outer layer, or stratum corneum, found in other skin. Millions suffer from dry chapped lips each winter. It is due to the structure of the lips themselves. The lips' exposed mucous membrane structure is actually different from other skin [17]. The skin is composed of three primary layers which are epidermis, dermis and subcutaneous tissue. Each layer possesses specific characteristics and functions [18].

Lips are lined externally by skin and internally by mucosa. There is a transition zone between these two, which is known as vermillion. Vermillion is unique to humans where it is red in color due to rich blood supply and due to lack of keratinisation in the epithelium. Epithelial is very thin stranum corneum, a prominent stratum lucidum, abundant melanocytes, numerous dermal papillae with a rich capillary supply [19].

2.2.1

The Epidermis

The lip epithelial is covering by very thin stratum corneum that controls the water balance in the skin. It does not contain melanin that can protect skin from ultraviolet rays. The lips skin thus has higher risk of getting sunburned. Therefore, it is important to use lip balm or lipstick that contains sunscreen to protect lips from ultraviolet rays [19]. The epidermis is the most superficial layer of the skin. It is the outer layer if the skin that function as a protective sheath against environmental influences. The epidermis composed of keratinocyte cells which are from keratin filaments that provide structural support to the skin. It is very important from a cosmetic standpoint because this layer can give texture, moisture and color to skin. The skin will appear aged if the surface of the epidermis is dry [18].

2.2.2

The Dermis

The dermis lies between the epidermis and subcutaneous fat which is in the middle layer of the skin. It is responsible for the thickness of the skin where it plays a key role in cosmetic appearance. With aging, the dermis layer decrease in thickness and moisture. The dermis consists mostly of collagen [18]. The dermis gives skin moisture, firmness and elasticity. It contain contains fewer cells compare to epidermis and mostly consist of fibrous extracellular matrix (ECM). The dermis composed from fibroblast cells, while ECM is an amorphous part of dermis that has highly complex mixture of bioactive macromolecules. Besides that, fibroblasts are specialized in producing two types of protein fibers, which are collagen and elastic fibers constituent of the ECM [20].

2.2.3

Subcutaneous Tissue

The subcutaneous tissue is the third of the three layers of skin. The subcutaneous layer contains fat and connective tissue that composed from larger blood vessels and nerves. This layer is important in the regulation of temperature of the skin and the body. The size of this layer varies throughout the body and different for every person [21]. Subcutaneous tissue or known as hypodermis is the largest tissues in the human body that composed of adipocytes, fibrous tissue, and blood vessels. The subcutaneous tissues, sebaceous glands, sweat glands and hair are absent in lips. Lips have almost no melanin, the natural pigment in skin that helps screen out the sun's harmful rays. As a result of the properties of lip skin, moisture rapidly evaporates from the lips, causing them to dry out very easily. Furthermore, this dryness frequently results in chapping and cracking, and increases the risk of inflammation, infection and burning. So, the only source of moisture of lips is from saliva. As conclusion, lipstick that has moisturizing effect as well as containing oil or wax to prevent moisture loss can be used in extreme of weather [19].

2.3

Formulation of Lipstick

Lipstick is a cosmetic product that is created for purpose of delivering ingredients like pigments, oils, waxes, and butter that applies colour, texture, and protection to the lips and also maintaining the moisture balances of lips skin. The raw materials that typically used to formulate lipstick are base and active ingredients.

2.3.1

Base Ingredients

In lipstick formulation, oil-based ingredient is used in order to formulate effective lipstick. It can give shiny appearance, and then will treat dry lips skin by act as occlusive agent, humectants, and emollient. In this study, beeswax is used as strengthenerâ&#x20AC;&#x;s agent while it also acts as occlusive agent. Besides, Virgin Coconut Oil is used as lip moistener and also act as occlusive agent as same as beeswax. Cocoa butter as emollient and act as shine enhancer.

2.3.1.1 Beeswax

Various waxes are used to provide a textural base for lipstick. The most commonly used and easily obtained wax that is used in lipstick comes from bee honeycomb. Beeswax is a natural product that contains straight chain acids and monohydric alcohols. In fact, the beeswax base represents a safe and natural product [22]. In lipstick formulation, beeswax act as useful material to bind oils due to its higher melting point than other ingredients, 61 to 65oC [24]. Furthermore, beeswax is an occlusive agent that can treat chapped lip by decreasing water loss and increasing level of moisturizing factor. Decreasing the water loss involves providing fatty acids that present in beeswax. Meanwhile, increasing level of moisturizing factor is through increasing the skinâ&#x20AC;&#x;s ability to hold onto water [18]. Beeswax has zero of irritation potential and a comedogenicity rating of 0 - 2, which means that, beeswax will not cause a problem or clog the pores when formulated and used correctly in cosmetic formulations. But, it brings a host of very positive attributes, such as general healing, softening, as an antiseptic, and act as emollient to cosmetic products. Beeswax has unique characteristics where it can build stable emulsions, and also will

improves water binding of ointments and creams. It gives a protective action of a non-inclusive type to the skin. Its elasticity and plasticity improve allow thinner films and provide a greater permanence on skin and lips. So, beeswax become preferred ingredient for lipsticks, because it contributes to sheen, consistency and colour stabilization [23].

Figure 2.1: Beeswax

2.3.1.2 Virgin Coconut Oil

Virgin coconut oil (VCO) is pure oil extracted from fresh coconut meat. It has a fresh, clean coconut smell and taste and should be colourless. It does not undergo any processing so its natural components remain unchanged. In the colorless, pure and fresh VCO are medium chain triglycerides or MCTs which make it easily digestible. Lauric and capliric acid are the types of medium chain triglycerides found in virgin coconut oil. These have anti-bacterial, anti-viral, anti-

fungal and anti-inflammatory properties that are essential to disease treatment and prevention. It have a high melting point, about 24Â°C, if above 24Â°C is colourless, below will solidifies into pure white solid. It is insoluble in water, but soluble in oils because it contains both of the hydrophobic and lipophilics portions in molecule. Coconut oil contains fatty acids that are important in maintaining the skin barrier and thus acts as an occlusive agent. The copious fatty acids in oil are required by skin for the proper formation and function of cell membranes to prevent water loss [18].

Figure 2.2: Virgin Coconut Oil

2.3.1.3 Hydrogenated Palm Oil

Palm oilâ&#x20AC;&#x;s unique composition makes it versatile in the application of food manufacturing and in the chemical, cosmetic and pharmaceutical industries [25]. The

palm oil is high in saturated fatty acids, about 50% and 80% respectively. Palm oil is high in vitamin K and dietary magnesium. In fact, no other vegetable oil has as much Vitamin E as compared to palm oil [26]. Palm oil also contained about 10% linoleic acid, which is an unsaturated omega-6 fatty acid. Linoleic acid is one of the two essential fatty acids that humans require. Besides that, carotenoids in crude palm oil also play an important potential role by acting as biological antioxidants, protecting cells and tissues from the damaging effect of free radicals. Its antioxidant properties bring many benefits to the human body, such as preventing skin aging, preventing fat oxidation and reducing blood pressure [27].

Figure 2.3: Hydrogenated Palm Oil

2.3.2

Active Ingredients

An active ingredient is a substance that makes a product performs its function. The active ingredients typically include phytochemicals, vitamins, enzymes, peptides, and antioxidants. In this study, the active ingredient is vitamin E. 2.3.2.1 Vitamin E

Vitamin E comprises eight naturally occurring forms of a fat-soluble antioxidant that is present in plasma, membranes, and tissues: α-, β-, γ-, and δtocopherols and tocotrienols. Vitamin E is the major lipid soluble antioxidant in skin. Anecdotal reports prove that, vitamin E speeds wound healing and improves the cosmetic outcome of burns and other wounds [28]. Their functions as chain-breaking antioxidants come from their ability to rapidly scavenge lipid-peroxyl radicals before they can react with other lipids, thereby ending the propagation of lipid peroxidation in membranes. In human, vitamin E is the most abundant lipid-soluble antioxidant. It is primary antioxidant in skin that protects cells from oxidative stress [18].

Figure 2.4: Vitamin E

CHAPTER 3

METHODOLOGY

3.1

Introduction

This chapter will describe the materials used in the study. Several experiments are designed to investigate and find the most desired formulation of lipstick. The properties of lipstick are depending on the formulation. Besides that, ingredients and material used in lipstick formulation become the most important criteria for consumers in choosing the lipstick, as their concern in safety issue and health [3]. The overall process of the production and also product evaluation steps of VCO (Virgin Coconut Oil) moisturizing lipstick are shown in Figure 3.1.

Preliminary Phase

Formulation of Lipstick

Characterization of Product Properties

Evaluation Parameters

Test

Melting Point

Breaking Load Test

Optimization

Stability Test

Verification phase

Sensorial Test

Figure 3.1: The product evaluation steps of Virgin Coconut Oil (VCO) lipstick.

3.2

Preliminary Phases

Preliminary phases are the first stage in order to formulate lipstick. The objective of this test is to identify the minimum and maximum values of base ingredients used in the lipstick formulation. These experimental settings were performed by Response Surface Method (RSM). The experimental design of three components system was conducted by using Design Expert (version 6.10) [3]. These results were obtained in the design of experiment (DOE) by using Box-Behnken of Response Surface Methods (RSM).

3.2.1

Determination of the Range of factors

The ranges of factors are determined by using conventional trial and error method.

The base ingredients used in the lipstick formulation are Virgin Coconut

Oil, hydrogenated palm oil and beeswax. Besides that, during the test, the temperature was always in constant condition. Thus, this phase is important to get the minimum and maximum values in order to determine the optimum percentage of the base ingredients without active ingredients.

3.2.2

Design of Experiments (DOE)

Design of Experiments (DOE) is a structured statistical technique used for study the behaviour of a product, process, or simulation by changing some of the design parameters in a specific manner and the results recorded. This study used DOE to optimize the formulation of Moist Natural Lipstick. A Box-Benken Design (BBD) with three factors and three levels was used to identify the relationship between mechanical properties and levels of ingredients [29]. Boxâ&#x20AC;&#x201C;Behnken design was used because it is very efficient. Besides that, it does not contain any point at the vertices of the cubic region formed by the upper and lower limits of the variables [30]. A set of candidate points in the design space was selected using Box Behnken criterion. While, the other ingredients such as Vitamin E and color pigment were held constant.

3.3

Sample Preparation

The aim of sample preparation is to determine the stable composition. During the preparation, temperature and speed of homogenizer were always conducted in constant values for all the samples.

3.3.1

Material and Equipment

The essential ingredients used in lipstick formulation were Virgin coconut oil, refined coconut oil, shea butter, beeswax, vitamin E, vanilla essence, color pigment and hydrogenated palm oil.

Table 3.1: Equipments Used In the Experiment NO

EQUIPMENT/TEST

BRAND/METHOD

Heater

Stuart CB 302

Melting Point

Differential Scanning Calorimeter (DSC)

3.3.2

Experiment Procedure

A lipstick formulation having the formulation composition was prepared as described below.

Beeswax and cocoa butter were melted (by double boiled) with maintaining the temperature at from 75o to 85oC with continuous agitation.

ii.

After the waxes were melted, the refined coconut oil was added into the mixture.

iii.

The pigments, vanilla essence (preservative and flavor) and hydrogenated palm oil were added to mixture and heated with agitation at 70oC. Agitation was continued until a proper dispersion achieved.

iv.

Vitamin E and Virgin Coconut Oil then added into the mixture formed in step iii with continuous stirred at 70oC until all the vitamin E fully dissolves.

The experiment was repeated by using different composition of VCO, beeswax, and shear butter to obtain stable formulation.

vi.

The resulting lipstick formulations were poured into molds and leave it at room temperatures to form the lipstick.

Illustration

Description

Beeswax,

cocoa

butter

and

pigment were melted by double boiled method.

All the ingredients were melt together till proper dispersion achieved.

The lipstick formulations were poured into molds.

The finished products of lipstick were leave at room temperature.

Table 3.2: Experiment procedure.

3.4

Characterization of Lipstick Properties

3.4.1

Melting Point Measurement

The melting point of lipsticks is supposedly within the range 55-75oC [32]. Melting point of all product samples were measured by using Differential Scanning Calorimeter (DSC). 50 mg of lipstick sample was taken [31]. The product samples were heated from 20oC to 100oC at scanning rate 10oC/min. The results of DSC data for all of the samples were then analyzed by peak program and the melting temperature was recorded. The temperature at which the first appearance of liquid formation was considered its melting point.

Table 3.3: Melting point test procedure.

Illustration

Description

a) Sample pan and cap. The lipstick samples were put in here. The sample mass is in the range of 5 to 12 mg.

The pan pressure was used to press the cap and pan into one.

The Differential Scanning Calorimeter (DSC) instrument.

Computer to monitor temperature and heat flow.

3.4.2

Breaking Load Test

The objective of breaking point is to determine the strength of lipstick [33]. The test is to find the value of maximum load that a lipstick can withstand before it breaks. The protruded lipstick is subjected to a number of weights hanging from it and the breaking load point is the weight at which the lipsticks break [31]. Table 3.4: Breaking load test procedure. Illustration

Description

The equipment for breaking load test was set up.

The

lipstick

was

held

horizontally in a socket half inch away from the edge of support.

The

weight

gradually

increases by water dropping at

specific

interval

second and weight at which breaks is considered as the breaking point.

3.4.3

Stability Test

Stability test was conducted by examine the organoleptic features of the samples which tested at same temperatures, lighting and packaging conditions. The resulting in appearance, smell, and color were observed after one months of storage. Besides that, the lipsticks were placed for stability studies at different in temperature, 4oC (freezer), 20-25oC (room temperature), 30-40oC (oven) and were observed the effects like bleeding, sweating, streaking and blooming [31].

3.4.4

Sensorial Test

Sensory analysis is a science that measures, evaluate and interprets the reactions of consumer to products as perceived by the senses of sound, smell, sight, taste and touch [34]. The objective of sensory evaluation is to evaluate the quality of the products as perceived by the end users [35]. Sensory analysis of lipstick product was performed by ten responders who are lipstick users, in good health condition and willing to be a part of sensory member by apply all the samples onto hand. This sensorial test was conducted using 10 types of lipsticks with different beeswax, VCO, and hydrogenated palm oil mixture ratio in the formulation together with five commercial lipsticks that are the most common to the responders [33]. The responders requested to observe the hardness, smoothness and moist of the samples. Finally, the responders then were requested to rank the samples based on these characteristics through the Hedonic scale.

3.5

Optimization

In the optimization phase, Box Behnken of Response Surface Methods (RSM) was to study the composition of the base ingredients of lipstick with desired melting point and breaking load point. The optimization was completely done by determining the best formulation by referring to the response model of analysis of variance (ANOVA). The sample then prepared and tested by using sensory test for evaluating the product based on responderâ&#x20AC;&#x;s acceptance.

3.6

Verification

Verification phase was performed based on result obtained from optimization phase. The melting point and breaking load point were measured to compare the predicted and experimental results.

CHAPTER 4

RESULT AND DISCUSSION

4.1

Introduction

This chapter presents the results of the melting point, breaking load point and sensory test on the formulation of Virgin Coconut Oil (VCO) based lipstick. The objectives of this experiment are to study the stability of the cosmetic moisturizing lipstick and formulate it based on the results that the most desired physical properties. The results of the stability test are able to determine the structure stability of the natural derivatives cosmetic lipstick.

4.2

Preliminary Phase

Preliminary phase presents the range of proportion of base ingredients in the lipstick formulation which are obtained through experiment. The Response Surface Method (RSM) is selected to determine the optimum mixture ratio for melting point of lipstick.

4.2.1

Determination of the Range of Factors

In the preliminary test, there are several experiment were carried out to obtain the component proportion of most significant ingredients for lipstick formulation. There are 17 run of experiments were performed by using different composition of beeswax, virgin coconut oil (VCO) and hydrogenated palm oil. The experiment was conducted by referred to the experimental result of the previous study, where the ranges of wax are around 30% to 50% respectively [3]. But, too much beeswax composition in a formulation can lead to poor crystallization and poor stability of the system [36].

The experiment settings are performed by response surface experimental design. The experimental design of three-component system is conducted by using Design Expert (version 6.0.8). A set of candidate points in the design space is selected using the Box-Behnken criterion. In Box- in Table 4.2 and follow the below inequalities: Behnken criterion, there are restrictions on the component proportions

Xi that take the form of lower Li and upper Ui constraint [3]. The constrains of the component proportion is shown in Table 4.1.

Li < Xi < Ui Table 4.1: Constraint of the component proportion Ingredient (Xi)

Lower Limit (Li)

Upper Limit (Ui)

Beeswax

VCO

Hydrogenated Palm Oil

4.2.2

Design of Experiments (DOE)

The Design of Experiment (DOE) is selected because this technique allows simultaneous evaluation of a number of independent runs that is required in a conventional step by step approach. In addition, DOE is structured statistical techniques, which increases productivity by minimizing the number of experiments involving a variety of experimental parameters and thus maximize the accuracy of the results. Boxâ&#x20AC;&#x201C;Behnken design of experiments was chosen to evaluate the combined effect of the three-component system on the three responses using 17 set of experiments. The ranges and levels of independent variables are shown in Table 4.2. Boxâ&#x20AC;&#x201C;Behnken design was used because it is very efficient and does not contain any point at the vertices of the cubic region formed by the upper and lower limits of the component. It has been used along with RSM to optimize various physical, chemical and biological processes [37]. The design consists of 17 combination composition. A set of candidate points made by 17 experiments are reported in Table 4.2

Table 4.2: Sets of run conditions determined by the model and their experimental response values

Order

Std

Run

Component

A: Beeswax

B: VCO (%)

(%)

Component 3

Response 1

Response 2

Response 3

C: Hydrogenated palm

Melting point (oC)

Breaking load point (g)

Sensory score

oil (%)

5.5

31.17

200.91

6.5

34.33

126.32

6.75

34.67

341.75

5.5

34.17

392.91

6.19

5.5

32.67

215.2

6.83

5.5

33.67

338.9

5.53

34.5

206.13

6.78

5.5

35.17

351.81

5.67

32.67

101.83

6.14

30.67

239.94

6.97

35.67

251.03

7.31

35.67

183.45

7.03

Order

Std

Run

Component

A: Beeswax

B: VCO (%)

(%)

Component 3

Response 1

Response 2

Response 3

C: Hydrogenated palm

Melting point (oC)

Breaking load point (g)

Sensory score

oil (%)

5.5

33.67

243.93

6.97

5.5

32.33

286

6.56

5.5

36.17

93.72

6.47

5.5

33.17

89.5

6.44

5.5

276.19

5.86

4.3

Process Analysis

The analysis process is conducted after the experimental response of the studied properties obtained. There are several steps involved in the analysis process to investigate the relationship between proportions of base-ingredients with response. Firstly, the transformation is carried out to find out the best fit that can improve the model. Then, the root square mean per mixture (RSM) has been used to evaluate the RSM. Finally, the Analysis of Variance (ANOVA) and diagnostic are used to evaluate the model obtained. The details of the design experiments along with experimental and predicted values of the three responses are shown in Table 4.3.

4.3.1 Model Development

Using RSM, the results were fitted to an empirical quadratic polynomial model for three parameters expressed as shown in Eq. (1). Y = βo + β1A + β2B + β3C + β11A2 + β22B2 + β33C2 + β12AB + β23BC + β31CA

(1)

Where, Y is the response variable, β0 the intercept, β1, β2, β3 coefficients of the independent variables, β11, β22, β33 quadratic coefficients, β12, β23, β31 interaction coefficients and A, B, C are the independent variables. Multivariate regression analysis and optimization process with the help of RSM were performed using Design Expert software version 6.10. Analysis of variance (ANOVA) of the data was performed and the values were considered significant when p-value <0.05 [4].

Following the experimental design present in Table 4.3, empirical third order polynomial equations were developed for the three response variables, melting point, breaking load point and sensory test in term of three independent variables as shown in Equations (2), (3) and (4).

Y1 = 244.45 + 126.75A + 0.69B + 22.13C - 2.70A2 - 23.26B2 - 1.04C2 + 2.17AB + 6.67AC + 8.44BC

(2)

Y2 = 32.57 + 0.17A + 1.33B - 0.33C + 0.90A2 + 1.07B2 + 0.49C2 - 0.38AB - 0.54AC + 0.96BC

(3)

Y3 = 6.54 - 0.36A + 0.095B + 0.22C - 0.70A2 + 0.18B2 + 0.30C2 + 0.028AB + 0.020C + 0.022BC

(4)

Where Y1, Y2, and Y3 represent Breaking load test, Melting point test, and Sensory test, respectively. A, B and C are the coded values of beeswax (%), VCO (% )and hydrogenated palm oil (%).

The experimental data for Breaking load test, Melting point test, and Sensory test were statically analyzed by analysis of variance and the results are shown in Table 4.4 , Table 4.5 and Table 4.6.

Table 4.3: Box-Behnken experiments along with actual and predicted values of responses.

Run

Melting point (oC)

Experimental Factor Beeswax

VCO

Hydrogenated

(%)

(째C)

palm oil (%)

Breaking load point (g)

Sensory score

Experimental

Predicted

Experimental

Predicted

Experimental

Predicted

5.5

32.33

32.57

286.00

244.45

6.56

6.54

33.67

33.75

338.90

342.37

5.53

5.54

33.67

32.57

243.93

244.45

6.97

6.54

33.00

32.57

276.19

244.45

5.86

6.54

5.5

33.17

32.67

89.50

93.21

6.44

6.32

5.5

35.17

35.67

351.81

348.10

5.67

5.79

32.67

32.57

215.20

244.45

6.83

6.54

5.5

32.67

33.59

101.83

98.49

6.14

6.31

35.67

36.09

251.03

251.40

7.31

7.36

31.17

32.57

200.91

244.45

6.50

6.54

34.67

35.00

341.75

338.66

5.50

5.54

34.17

33.25

392.91

396.25

6.19

6.02

5.5

30.67

31.50

239.94

233.13

6.97

7.13

5.5

35.67

34.84

183.45

190.26

7.03

6.87

Run

Melting point (oC)

Experimental Factor Beeswax

VCO

Hydrogenated

(%)

(째C)

palm oil (%)

Breaking load point (g)

Sensory score

Experimental

Predicted

Experimental

Predicted

Experimental

Predicted

5.5

36.17

36.09

93.72

90.25

6.47

6.46

5.5

34.50

34.08

206.13

205.76

6.78

6.73

5.5

34.33

34.00

126.32

129.41

6.75

6.71

4.3.2

Analysis of Breaking Load Point of the Samples.

The quality of moist lipstick moist natural lipstick based on virgin coconut oil (VCO) is directly linked to the ratio of ingredient used in the formulation. Therefore, the Breaking load test, Melting point test, and Sensory test of 17 samples is measured in the experiment. By using design expert software, a transformation was perform by analysis of the breaking load point of sample.

Analysis of variance (ANOVA) is used in this study to examine the fitness and significance of model.

Table 4.4: ANOVA table for breaking load test of samples

ANOVA for Response Surface Quadratic Model Analysis of variance table [Partial sum of squares] Source

Sum of

Squares

Mean

F Value

Prob > F

Square

Model

1.353E+005

15033.12

18.55

0.0004

1.285E+005

158.63

< 0.0001

3.84

4.735E-003

0.9471

3917.90

4.84

0.0638

30.68

0.038

0.8512

2278.84

2.81

0.1374

4.59

5.667E-003

0.9421

18.88

0.023

0.8830

177.82

0.22

0.6537

285.10

0.35

0.5717

Pure error

5485.39

1371.35

0.045

0.9854

Cor total

1.410E+005

Table 4.3 show the ANOVA table for breaking load test measurement by response surface quadratic model. Based on the ANOVA table, the model is highly significant, as the F-values for the model are 18.55 and the corresponding of p-values is 0.0004 which lower than 0.05.

There are two diagnostic plots, Normal Plot of Residuals and Predicted-actual values plot for breaking load test of VCO lipstick as represent in Figure 4.1 and Figure 4.2 respectively. Figure 4.1 shows that the difference between the studentized residuals and normal % probability was quiet large due to the sinificant errors existed. Figure 4.2 shows the points following a straight line, where the actual is almost directly proportional to the predicted breaking load point reading. This indicates that the residuals follow a normal distribution and the analysis just have small improvable by the transformation change. Figure 4.3 shows the surface response plots of the effects of beeswax, VCO and hydrogenated palm oil composition on the breaking load point.

Figure 4.1: Normal-residual plots for breaking load point of VCO lipstick.

Figure 4.2: Predicted-actual plots for breaking load point of VCO lipstick.

a(i)

a(ii)

b(i)

b(ii)

c(i)

c(ii)

Figure 4.3: Effects of hydrogenated palm oil, beeswax and VCO composition on breaking load test (a) composition of hydrogenated palm oil kept constant at 5.5% (b) composition of beeswax kept constant at 40% (c) composition of VCO kept constant at 3%.

4.3.3

Analysis of Melting Point of the Samples

Melting point of the lipstick samples are measured by using Differential Scanning Calorimeter (DSC). The melting point of samples can be observed in the study ranges from 30.67oC to 36.17oC and the ratio of maximum to minimum is 1.17932. Thus, the transformation is not required as the ratio is smaller than 10.

Table 4.5: ANOVA table for melting point of samples

ANOVA for Response Surface Quadratic Model Analysis of variance table [Partial sum of squares] Source

Sum of

Squares

Mean

F Value

Prob > F

Square

Model

30.99

3.44

3.19

0.0704

0.22

0.21

0.6625

14.23

13.16

0.0084

0.89

0.82

0.3941

3.45

3.19

0.1174

4.84

4.48

0.0721

1.00

0.92

0.3683

0.56

0.52

0.4941

1.17

1.08

0.3335

3.67

3.39

0.1081

Pure error

3.42

0.86

Cor total

38.56

Table 4.4 presents the ANOVA for melting point of the sample, where the response surface quadratic model is selected to provide best fit of the experimental data. From the table, it can be observed that the model for melting point was not

significant because the p-value was 0.0704, which greater than 0.01. the insignificant model is due to the differentces in melting point for replication of experiment.

The models of response are graphically analyzed by using the diagnostic test. Figure 4.4 shows the Normal-residual plots for melting point of samples that used to test the normality of the model. From the figure, it can be said that the plot was normal and acceptable in the study as the â&#x20AC;&#x17E;Sâ&#x20AC;&#x; shape that indicate the normal of model is appeared. Figure 4.5 shows the Predicted-actual values plot for melting point of VCO lipstick. The large difference between the actual and predicted value cause the model of melting point becomes insignificant.

Figure 4.4: Normal-residual plots for melting point of VCO lipstick.

Figure 4.5: Predicted-actual plots for melting point of VCO lipstick.

a(i)

a(ii)

b(i)

b(ii)

c(i)

c(ii)

Figure 4.6: Effects of hydrogenated palm oil, beeswax and VCO composition on melting point (a) composition of hydrogenated palm oil kept constant at 5.5% (b) composition of beeswax kept constant at 40% (c) composition of VCO kept constant at 3%.

4.3.4

Analysis of Sensory score of the Samples

Sensory tests are performed in this study to investigate the customer acceptance for moist lipstick. The transformation is not required for sensory score due to the response ranges from 5.5 to 7.31. The ratio of maximum to minimum is only 1.32909, which smaller than 10. The quadratic model is selected as the desired terms from the model list and provides the best p-values. The ANOVA for sensory score of the samples is shown in table 4.5. The p-value is 0.0551, which greater than 0.01. the insignificant model is due to the differentces in melting point for replication of experiment.

Table 4.6: ANOVA table for sensory score of samples

ANOVA for Response Surface Quadratic Model Analysis of variance table [Partial sum of squares] Source

Sum of

Squares

Mean

F Value

Prob > F

Square

Model

3.97

0.44

3.53

0.0551

1.06

8.48

0.0226

0.072

0.58

0.4718

0.39

3.14

0.1199

2.05

16.38

0.0049

0.14

1.10

0.3294

0.37

2.99

0.1272

3.025E-003

0.024

0.8807

1.600E-003

0.013

0.9130

2.025E-003

0.016

0.9022

Pure error

0.73

0.18

Cor total

4.84

The diagnostic test for sensory score is shown in figure 4.7. The result of the test is also quite similar to the melting point where the plot is normal and acceptable in the study. Meanwhile, the Predicted-actual values plot for sensory score shows only small difference between the actual and predicted values.

Figure 4.7: Normal-residual plots for sensory score of VCO lipstick.

Figure 4.8: Predicted-actual plots for sensory score of VCO lipstick.

a(i)

a(ii)

b(i)

b(ii)

c(i)

c(ii) Figure 4.9: Effects of hydrogenated palm oil, beeswax and VCO composition on sensory score (a) composition of hydrogenated palm oil kept constant at 5.5% (b) composition of beeswax kept constant at 40% (c) composition of VCO kept constant at 3%.

4.3.5

Response Surface Analysis.

The response surface plots and it corresponding contour plots (Figures 4.3, Figure 4.6 and Figure 4.9 for a(i), a(ii), b(i), b(ii), c(i), c(ii)) are generated with one variable kept at its optimum level and varying the others within the experimental range. The interactions of beeswax (%), VCO (% )and hydrogenated palm oil (%) for Breaking load test, Melting point test, and Sensory score are depicted in Figures 4.3, Figure 4.6 and Figure 4.9.

From Figure 4.3 a(i), it is evident that the hardness of lipstick is increase with increasing of beeswax (%), the maximum region being in composition range between 38% and 41%, as evident from the contour plot from Figure a(ii). While Figure 4.3 b(i) shows that breaking load point slightly increase with the increase of VCO composition up to 3.0% and then slightly decrease irrespective of the palm oil composition. Besides that, Figure 4.3 c(i) show that the breaking load point increase with increasing of hydrogenated palm oil composition.

From Figure 4.6 a(i), it is evident that the melting point of lipstick is increase with increasing of VCO (%). While Figure 4.6 b(i) shows that the melting point of lipstick is increase with increasing of hydrogenated palm oil (%). Besides that, Figure 4.6 c(i) show that the melting point of lipstick is increase with increasing of beeswax (%).

From Figure 4.9 a(i), it is evident that the sensory score of lipstick is increase with increasing of beeswax (%) up to 40% and then slightly decrease irrespective to VCO composition, as evident from contour plot a(ii). While Figure 4.9 b(i) shows that the sensory score of lipstick is increase with increasing of VCO (%). Besides that, Figure 4.9 c(i) show that the sensory score of lipstick is increase with increasing of hydrogenated palm oil(%).

As conclusion from graphs as above, it can be seen that all parameters involved were significant between each other. As result, breaking load point, melting point and sensory score increases as parameters which are composition of beeswax, hydrogenated palm oil and VCO increases. However, increasing of beeswax composition has limitation. This phenomenon can be seen in all Figure 4.9 a(i) where it shown that after 1 point (40%) , there will be reducing in sensory score.

4.3.6

Analysis of Stability Test

Stability test is important for cosmetic products to ensure the products meet the specified physical, microbiological and chemical quality standard. In this study, stability test have been done for moisturizing lipstick based on Virgin Coconut Oil. This test is conducted under normal and accelerated condition through observation of variation in organoleptic features after certain period of storage.

The observation of samples in the variation of appearance, odour, and spreability was carried out after one month storage in 4oC, 20-25 oC and 40-45 oC. From the observation, the samples did not have any changes in appearance before and after the testing as shown in Figure 4.10.

Figure 4.10: Observation of stability test at storage temperature 4oC, 20-25 oC and 40-45 oC.

Temperature (oC)

Before testing

After testing

Observation: There have no blooming, no streaking, no sweating and no bleeding.

20-25

Observation: There have no blooming, no streaking, no sweating and no bleeding.

40-45

Observation: Lipstick texture shows a little bit soft due to high temperature effect.

4.4

Optimization

4.4.1

Numerical Optimization Formulation of Lipstick

For the numerical optimization, all the three component (beeswax, VCO and hydrogenated palm oil) are set in the range of 30% to 50%, 1% to 5% and 1% to 10% respectively. The breaking load point and melting point are targeted from 250g to 300g and 31oC to 36.17oC respectively. Meanwhile the sensory score is targeted to maximum so that the highest customer acceptance can be achieved.

Table 4.7: The Solution of the Optimization of VCO Moisturizing Lipstick. Number

VCO (%)

Hydrogenated palm oil (%)

41.27

34.20

Breaking load point (g)

268.539

171.796

Melting point (oC)

35.1761

34.4661

Sensory score

7.30999

7.31

0.914

0.848

Beeswax (%)

Desirability

Table 4.5 shows the two solutions that were obtained with the different desirability value after the optimization process. The first formulation is selected as optimal formulation as the desirability is higher than second formulation, which is 0.914. Furthermore, the first formulation gives a little bit higher sensory score or customer acceptance than the first formulation.

CHAPTER 5

CONCLUSION AND RECOMMENDATIONS

5.1

Conclusion

The main conclusions from the study are as follow:

1. The preliminary phase of experiment shows that the significant ingredients in moist natural lipstick were Virgin coconut oil, beeswax and hydrogenated palm oil. The constraints of the component proportion are ranges from 1.0% to 5.0%, 30.0% to 50.0% and 1.0% to 10.0% for Virgin coconut oil, beeswax and hydrogenated palm oil respectively.

2. The melting point of lipstick can be manipulated by changing the composition of virgin coconut oil, beeswax and hydrogenated palm oil. The melting point of the lipstick increase with increasing of beeswax. On the other hand, the melting point of the lipstick is reduced with the

increasing of virgin coconut oil composition.

Y2 = 32.57 + 0.17A + 1.33B - 0.33C + 0.90A2 + 1.07B2 + 0.49C2 - 0.38AB 0.54AC + 0.96BC

Where Y2 Melting point test .A, B and C are the coded values of beeswax (%), VCO (% )and hydrogenated palm oil (%).

3. The moist natural lipstick is stable with the stability test due to high amount of oily ingredients that provides microbiological stability.

4. The optimization was carried out using Box-Behnken response surface method. The composition of optimal product was 5.0% of VCO, 10.0% of hydrogenated palm oil and 41.27% beeswax. The prediction values for breaking load point, melting point and sensory score of optimal product were 268.539g, 35.1761oC and 7.30999 respectively with desirability equal to 0.914.

5.2

Recommendation

Based on the results and conclusion obtained in this study, the future work can be drawn by the following recommendations:

1. The melting point of Virgin Coconut Oil lipstick should be in the range of 5575 oC in order to meet the acceptable limit according on previous study.

2. The formulation ingredients can be added by appropriate amount of colorant, flavor and other active ingredient in order to increase customer acceptance level.

3. The breaking load test should be done by suitable equipment like CT3 Texture Analyzer utilizes TA-LC Lipstick Cantilever Fixture in order to get more accurate result.

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