Research Proposal - Part 11

In partial fulfillment of the requirements for High IV Science Research Comparison and Evaluation of Volatile Oils From Two Different Extraction Methods for Sampaguita Flower Submitted by: Ang, Mark Jesfferson Ang, Michael Yu, Pamela Yung, Clarisse Anne IV-Jehoshaphat Submitted to: Mr - Research Proposal introduction. Ronald Allan Vaguchay 2013 Chapter I Introduction Sampaguita flowers are blooming almost everywhere in the Philippines. Nevertheless, only a few people are knowledgeable of the full uses of this plant.

Around the globe, many researches have already been conducted concerning the volatile oils one could harvest from the plants with rich scents, such as jasmine, rose, and lavander. However, there have been very few researches in the Philippines on the volatile oils of the jasmine, specifically the Jasminum sambac, which is the local plant more commonly known as Sampaguita. This plant is said to be very delicate, requiring meticulous steps in order to obtain the best aroma from it. There are many methods of oil extraction, but not every method is efficient and effective.

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In relation with this, this study is to be conducted to further widen the scope of the knowledge of the people especially the Filipinos, regarding this plant’s properties and uses. Problem This study will answer the question: What is the more efficient and more effective way to obtain the volatile oils of the Sampaguita flower? Hypotheses Null Hypothesis (Ho): There is no significant difference in the quantity, quality, and odor of the essential oils produced. Alternative Hypothesis (Ha): There is a significant difference in the quantity, quality, and odor of the essential oils.

Objectives This study aims to determine the quantity, intensity, and resemblance of the essential oils produced in comparison with the Sampaguita flower using two different methods: solvent extraction and hydro distillation. Specifically, this study aims to achieve the following objectives: 1. To determine which among hydro distillation or solvent extraction is more efficient in producing the desired essential oils 2. To determine the quantity, intensity, and resemblance of the essential oils with the Sampaguita flower 3.

To compare and contrast the two essential oils produced using the two different methods 4. To compare the cost of the two methods Significance of Study Volatile oils give essential benefits, acting as anti-depressant, expectorant and medicine, to its users. It also has countless uses in the manufacturing sector of the society. For example, it can be used in making perfumes and lotions. Thus, additional information in acquiring such produce efficiently and effectively is significant. More so, the plant to be tested in this study is very abundant in the Philippines, giving a greater possibility of utilizing it.

This may result to a lucrative business to whoever desires to engage in a similar study. Scope and Limitations This study on the production of essential oils using two methods, namely solvent extraction, and hydro distillation only covers collection of significant data which proves the quantity, intensity, and odor resemblance of the essential oils produced in comparison with the Sampaguita flower. It only discusses and highlights significant factors that affect the production of essential oils and its properties. However, this study does not look into the shelf life of the essential oils produced.

Furthermore, this study does not include other methods in producing the essential oils. Also, only one product per method is made. No testing on concentrations of the essential oils is performed, and neither is a product made out of the essential oils. Other information on the production of essential oils not mentioned above is not tackled thoroughly in the study. Definition of Terms 1. Volatile oil or essential oil – oil having the odor or flavor of the plant from which it comes; used in perfume and flavorings 2.

Hydro distillation – a variant of steam distillation in which material is soaked for some time in water after which the mixture is heated and volatile materials are carried away in the steam, condensed and separated 3. Solvent extraction – the partial removal of a substance from a solution or mixture by dissolving it in another, immiscible solvent in which it is more soluble. 4. Anti-depressant – any of a class of drugs used to alleviate depression 5. Expectorant – a medicine that promotes the secretion of sputum by the air passages, used esp. o treat coughs. 6. Perforated – pierced with one or more holes 7. Ethanol – An alcohol obtained from the fermentation of sugars and starches or by chemical synthesis 8. Diethyl Ether – A pungent, volatile, highly flammable liquid derived from the distillation of ethyl alcohol with sulfuric acid and widely used as an inhalation anesthetic Chapter II Review of Related Literature Sampaguita Plant Sampaguita plant (Jasminum sambac), also known as Jasmine, is an evergreen woody shrub in the olive family with a height less than two meters.

The dark green leaves are ovate with blunt tip, glossy, simple and grow up to seven meters long. The flowers are white and are strongly scented, blossoming singly or in clusters that are usually in threes (3’s). The corolla lobes are oblong to round (Marckwardt, et al. , (1986); Madulid, (1995)). Sampaguita is native to Asia and was introduced to the Philippines in the pre-Spanish era. It blooms all year round, specifically blooming late at night. It is cultivated to make leis and garlands (Madulid, 1995). It is also known as an aphrodisiac, antiseptic and anti-depressant.

It is generally cultivated for its fragrance, cleansing and soothing properties. The flowers of the Jasmine plant also have medicinal properties. Sometimes, it is used as lactifuge. Some people, as passed onto them as a practice, use it for treatment of skin disorders, ulcers of the gums and fever (Santiago, 2010). It is also used to ease menstrual pain, calm irritating coughs and regulate breathing. For the skin, it is used for stretch marks and scars (Cox, Aromatherapy Oils – Jasmine, 2011). Proper Gathering of Sampaguita Flowers There are many ways to obtain the best scent from the Sampaguita flowers.

The first step is to gather the flowers before they fully open and bloom (Dodrill, 2011; Alday, 2009). In harvesting the jasmine flower, one must pick each flower by hand to avoid bruising the flower, which may cause an unpleasant odor in the finished oil (Crow, 2011). However, it is important to note that one should only pick the mature buds and the ones that are already due to open (Alday, 2009). Open flowers are generally not harvested as larger amounts of them are needed to extract oils and they tend to lose their fragrance sooner.

Second, the petals of the selected flowers will be collected in a plastic bag with a zipper to avoid losing its fragrance (Richford, 2012). Flower buds are harvested based on color, firmness, and size which can all vary depending on the weather. Also, the buds have to be white, as green ones may not emit the same characteristic fragrance the Sampaguita flowers are known for. Essential Oils An essential oil is natural aromatic compound found in the seeds, roots, flower and other parts of a plant (Hill, 2008). Essential oils are generally clear, but some oils are amber or yellow in color.

They last up to twelve (12) months when stored in a dark and cool area. A mason jar is commonly used to house the material during the steeping stage of oil extraction (Dodrill, 2011). Essential oils are often used in cosmetics such as facial cleaners, body lotion and acne prevention. They are also used in perfumery, cleaning products, potpourri and craft products. It is also commonly used as massage oil. In this usage, the body is rubbed after applying the oil. Through this process, the oil is absorbed by the skin. It will enter into bloodstream then into the lungs.

As affirmed by other researches, it can bring several health benefits. However, there are certain essential oils, which can be toxic, so care is needed when using these oils (Hill, 2008; Dodrill, 2011). Different Methods of Extraction There are various ways to extract essential oils from plants. A similar research done on extracting essential oils from Thai fragrant flowers was done using different methods, namely hydro distillation, solvent extraction, and enfleurage. The results of this research showed that the solvent extraction using ninety-five percent (95%) ethanol produced the most amount of oil.

However, the one that yielded the oil with the closest scent to the fresh flowers was the enfleurage method, and next to it is the solvent extraction using diethyl ether (Yimnoi, et al. , 2011). Meanwhile, another research recommends the use of supercritical fluid extraction method with carbon dioxide (CO2) as a solvent with the aid of the co-solvents ethanol and methanol. The researchers claim it to be the most effective method as it avoids the contamination of the oil (Din, 2006; Mohd. Faisal, 2006). In fact, supercritical method showed more advantages as compared to hydro distillation (Rezazadeh, et al. 2008). Conventional techniques like steam distillation is rendered inappropriate in extracting essential oils because it inflicts thermal degradation of compounds in the oils, thus, to the natural fragrance (Din, 2006; Mohd. Faisal, 2006). One of the most widely used traditional methods on obtaining essential oils from plants is hydro distillation. This process is usually used by small scale producers. There are many disadvantages in using this process such as the difficulty in controlling the heat. Also, the prolonged exposure to hot water may cause hydrolysis which leads to formation of acids and alcohols.

The process involves a total submerging of the plant material in water and the boiling of the suspension. Deg-bhabka method is an example of this technique (Tandon, 2012). This process requires 100 grams of dry plant material in powdered form. The extraction takes 5 hours using a Clevenger-type apparatus. The volatile distillate will then be collected over normal pentane and refrigerated for one week (Rezazadeh, et al. , 2008). Another specific method is as follows. Plant material will be placed in a 2-liter roundbottomed flask with distilled, deionized water (1 g dry material: 13. ml water and 1 g fresh material: 2ml water) and the essential oil will be extracted by water distillation using a modified clevenger trap. The distillation period is one hour (1 hr) for the fresh samples and one hour and fifteen minutes (1 hr 15 min) for the dried samples (Charles & Simon, 1990). The jasmine flower’s oil is usually extracted through enfleurage method. It is an ancient method used in extracting oils from delicate flowers, and it is rarely used nowadays, for it is very costly and labor-extensive (Tom, 2011). This method requires glasses in wooden frames which are layered with animal fat or shortening.

Above it, the jasmine petals are placed, fully covering the shortening or the fat. This setup is stacked one above the other and are placed under the sun (Cox, Essential Oil Extraction, 2011). The flowers are replaced every 24 hours, and for the jasmine flower, it usually takes 65 replacements before the fat becomes saturated; this is the reason for the costliness of a quality jasmine essential oil (Tom, 2011). After this process, the petals are removed, and fat is dissolved in alcohol, and the alcohol is evaporated from the essential oil (Cox, Essential Oil Extraction, 2011).

Jasmine oil can also be extracted using solvent extraction, a cheaper process than enfleurage but more expensive than distillation (Cox, Essential Oil Extraction, 2011). The highest yield from a research done on the extraction of essential oil from jasmine flower using the solvent extraction method was 14. 53%, which used ethanol (Mohd. Faisal, 2006). Solvent extraction is a process where a solvent is used to separate the components of a certain material (Smith, 2011). In solvent extraction, the petals are placed in the perforated metal trays, and are sprayed with the solvent, usually petroleum ether or hexane.

This solvent dissolves all components that can be extracted such as the aromatic molecules, the non-aromatic waxes and the pigments. The mixture is then filtered, and the solution yielded is warmed and mixed with alcohol, usually ethanol (Cox, Essential Oil Extraction, 2011; Marge, 2012). To further purify the extract, the solution is agitated and frozen at negative thirty-five (-35) degrees Fahrenheit. Lastly, the solution is cold filtered to produce the absolute (Marge, 2012). Many researches have been conducted on supercritical solvent extraction using carbon dioxide (CO2).

More so, it has been proven to be more effective than hydro distillation. However, this process is very expensive. “Supercritical fluid extraction (SFE) is a rapid, selective and convenient method for sample preparation prior to the analysis of compounds in the volatile product of plant matrices (Pourmortazavi & Hajimirsadeghi, 2007). ” Carbon dioxide turns to liquid under high pressure and turns back to gas in normal conditions. Therefore, in the process, it just evaporates after the extraction is done causing it to leave no residue. Aromatic chemicals are also extracted in this technique, giving the essential oil a more intense scent.

The main components of the SFE unit are pump, extraction chamber, a recovery chamber and a collection device (Din, 2006). Use of Coffee as a Neutralizer Coffee has several uses. However, its usage as an odor neutralizer is uncommon to most people (Larkin, 2012). Its main role is to control or to remove unwanted smells. Some people place it in the fridge to absorb the foul odors present. On the other hand, others apply it to their hands to neutralize the smell of some strong plant odors (Fuentes, 2009). It is also known for its ability to neutralize closed rooms.

Aside from its properties as a neutralizer, coffee is also very affordable, easy to find, and very convenient to use (Wharton, 2007). Chapter III Methodology Gathering of Sampaguita The researchers will gather the Sampaguita flowers at night where the flowers’ oils are at its peak. The desired blooms will consist of those mature buds that are just about to open. The researchers will also look at the flowers’ color, firmness, and size to be assured of good quality. It is also important to note that the researchers will only gather white Sampaguita buds as green ones may not emit the same fragrance.

The petals of the selected flowers will then be collected in a plastic bag with zipper to avoid losing its fragrance and preserve the quality of the flower. Experimental Procedure In the experiment, the researchers will be testing the amount of essential oils produced, the intensity of its fragrance, and its resemblance to the odor of the Sampaguita flower. These three dependent variables will be tested using two methods, namely hydro distillation, and solvent extraction. The researchers will also keep the amount of flowers, its weight, location, and period constant to avoid any discrepancies. Flowchart

Solvent Extraction SampaguitaEssential Petals Oils Hydro Distillation List of Materials Project Data Materials| Experimental Materials| Bond paper| Hydro distillation apparatus| Computer| Ethanol| Standard Deskjet Printer| Diethyl Ether| Ink for Printer| Sampaguita Flowers| Ballpen| Perforated Metal Tray| Folder | Graduated cylinder| Digital Camera| Bowl| | Container| Hydro Distillation To begin the distillation process, the Sampaguita petals will be placed in the still. The still is a part of the distillation device that consists of a cooling device and a vessel into which heat is added using a Bunsen burner.

The petals are then placed in the vessel. The steam will then be added by heating water at one hundred (100) degree Celsius using the Bunsen burner, and passed through the petals. If the temperature is allowed to rise above 100 degrees Celsius, it is possible for the petals and its essential oils to become damaged, so close monitoring will be done. Through steaming, the petals will open their sockets, releasing the flower’s aromatic molecules that will rise with the steam. The vapors carrying these molecules will then pass through the condenser.

The condenser will be filled with cold water to cool the steam that will pass through it making the steam condense and transforming it to liquid form which is called the distillate. The distillate is comprised primarily of the hydrosols – aromatic water produced after a distillation process – and the essential oils from the flower petals. The liquid will then pass through a closed system and transporting it to the receiving flask. Inside the receiving flask, the distillate, containing two substances will separate into two layers; the upper layer containing the oil, the other containing water.

The liquids will be transferred to a separatory funnel to allow the hydrosols to be drained, leaving only the oil. The oil will then be placed in a glass container for the next procedure. Solvent Extraction 8000 individual blossoms are required to produce one gram (approx one ml) of absolute. The perfect petals or the petals without bruises are to be thinly placed in the perforated metal trays and are to be submerged in diethyl ether. The washing process will be repeated for many times. The mixture will then be filtered, and the filtrate will be subjected to low pressure distillation or vacuum processing to extract the solvent.

This concrete is extracted at room temperature or under gentle heat. The waxy mass left will be first left to cool. This agitation and cooling process may last up to several weeks. After that, the concrete will be warmed and stirred with pure ethanol at 115-125 degrees Fahrenheit. During the heating and stirring, the concrete should break up into tiny globules. To further purify the extract, the solution is agitated and frozen at negative thirty-five (-35) or negative thirty (-30) degrees Fahrenheit, making the wax precipitate. Lastly, the solution is to be cold filtered or steam distilled under reduced pressure to produce the absolute.

Here, the alcohol is made to evaporate. A low pressure distillation apparatus is where evaporation takes place at sub-atmospheric pressures. An evaporation chamber has a feed liquid inlet port, a concentrated liquid outlet port, and a vapor outlet port. The vapor outlet port is connected to a vapor treating device, specifically a rotating impeller pump, immersed in distillate in a distillate chamber (Keane, Shafaghi, & Spencer, 1992). Data Collection The end-products of the three methods will be tested by thirty-six (36) panelists. A sensory evaluation using preference test will be conducted (Yimnoi, et al. 2011). In between the evaluation, coffee will be used to neutralize the scent of the past essential oil for a more comprehensive data collection. An appropriate volume of graduated cylinder will be used as a tool to measure the amount of essential oil after the extraction of the oil. Meanwhile, the subjects will evaluate the odor and the similarities between the oil and the plant based on the rubric that will be handed to them. After evaluating certain oil, the panelists will be asked to smell coffee beans to neutralize the scent that they inhaled, to clearly identify the scent of the oil.

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