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Journal of the Indian Chemical Society 98 (2021) 100178 Contents lists available at ScienceDirect Journal of the Indian Chemical Society journal homepage: www.editorialmanager.com/JINCS/default.aspx Preparation and characterization of fragrance by extracting the essential oils from different raw materials Arvind K. Gautam a,*, Kuldeep Singh b a Department of Chemical Engineering, National Institute of Technology, Hamirpur, Himachal Pradesh, 177005, India b Department of Chemical Engineering, Raja Balwant Singh Engineering Technical Campus, Bichpuri, Agra, Uttar Pradesh, 283105, India A R T I C L E I N F O Keywords: Fragrance Liquid-liquid extraction Hydrophobic GC/MS Technique Essential oils * Corresponding author. E-mail address: akgautam@nith.ac.in (A.K. Gaut https://doi.org/10.1016/j.jics.2021.100178 Received 27 January 2021; Accepted 22 Septembe 0019-4522/© 2021 Indian Chemical Society. Publi A B S T R A C T The extraction is a simple process and it is widely used to extract the fragrances in fragrance industries from essential oils. There are number of compounds (i.e. flowers, oils, leaves etc.) from which we can prepare the fragrance by extracting the essential oils from them. In this work, we have prepared the fragrance from the essential oils by the liquid-liquid extraction process, where the essential oil presented as the concentrated hy- drophobic liquid containing volatile aroma compounds. We used the combination of Gas chromatography and Mass spectrometry (GC/MS) characterization techniques to make our product more useful, convenient and compitative with the other fragrance available in the market. This study would be helpful to understand the preparation of the fragrance from the concentrated hydrophobic liquid type essential oils which contains volatile aroma compounds by using a significant liquid-liquid extraction process. 1. Introduction The benefits of the essential oils has been utilized by the civilizations from the centuries. The essential oils are not only highly makes the essential oils to define as adaptogens, that usually promoted as homeo- stasis. The essential oils in general are non-greasy and required very limited drops to observe or results a tremendous effects on the emotional wellbeing, spiritual mindfulness, and physical health. There were many uses of essential oils has been address in the medical, cosmetics, food industries. Further, because of the different variety of its properties along with the pleasant odour these essential oils used very frequently as many related household products as well [1]. Basically, the concentrated type hydrophobic liquids which contains therapeutic volatile aroma com- pounds are known as the essential oils. These oils are also treated as ethereal oils, volatile oils, aetherolea oils, or simply as the plant oil from which they were further extracted more efficiently such as clove oil. In order to produce the safe and effective cosmetic products, it is most important to determine the maximum concentration of these oils [2]. These essential oils can be distinguise in more sensible way as it contains am). r 2021 shed by Elsevier B.V. All rights re the ‟essence of” the valuable plant’s fragrance and important character- istics fragrance of the plant from which it is derived significantly [3]. Further, apart from the other uses these essential oils in general are the indispensable and dispensable amino acids for the humans lives [4]. These essential oils evaporate completely in contrast to fatty oils without leaving any stain (residue) while dabbing onto filter paper. There are multiple processes are available in the market at present time. However, in general the distillation, resin tapping, absolute oil extraction, solvent extraction, and cold pressing etc. processes are used more frequently to extract these types of essential oils. In this work, we have prepared the fragrance by extracting the essential oil from the different leaves, flowers, and, roots etc. The liquid- liquid extraction process was used here for the essential oil extraction from the different raw materials (i.e. leaves, flowers, roots etc.) followed by the simple steam distillation process. The outcome after the distilla- tion was very highly concentrated portion of the essential oil which is separated from the flower water. Since these substances can be charac- terized according to their sensory properties [5]. Therefore, this highly concentrated essential oil have been characterize in the fragrance and served. mailto:akgautam@nith.ac.in http://crossmark.crossref.org/dialog/?doi=10.1016/j.jics.2021.100178&domain=pdf www.sciencedirect.com/science/journal/00194522 www.editorialmanager.com/JINCS/default.aspx https://doi.org/10.1016/j.jics.2021.100178 https://doi.org/10.1016/j.jics.2021.100178 Fig. 1. Process block diagram of fragrance preparations from essential oil. Fig. 2. Process block diagram to separate the essential oil and flower water. A.K. Gautam, K. Singh Journal of the Indian Chemical Society 98 (2021) 100178 properties of the plant from which it was extracted and identified. The product prepared from the steam distillation of the essential oils contains true essence including the atractive smell. The smell was the most sen- sitive of the five senses and this study shows that nearly 75% of emotions are prompted by the scent. Our balance blend was especially soothing when gently inhaled it. The employed preparation methods and tech- niques of this product (i.e fragrance) from essential oils has been dis- cussed in the next section of this article along with the flow diagram. 2. Methodology The details of experiment and procedure employed in this study to prepare the fragrance are as follows; 2.1. Materials The orange peel (300 gm), Lemon grass (250 gm), Lavender (250 gm), Rose (250 gm), Myrrh (250 gm), Cypress (300 gm) were collected from different area of resources to prepare the fragrance by the extraction of the essential oil. 2 2.2. Preparation of perfumes There are number of techniques and methods available to prepare perfumes from different flowers by extracting the essential oils [6–8]. The essential oils from the flowers and leaves can be extracted by steam distillation, hydrodistillation, dry distillation, supercritical fluid extrac- tion, etc. The steam distillation and hydrodistillation are traditionally used for the isolation of volatile aroma related compounds from odorif- erous samples [9]. In this study, we prepared the fragrance by using standard methodology through extraction of essential from different flowers and leaves as per the following sequences; ● Collection of samples from their respective sources. ● Reduce the size of sample so as to enhance the surface area. ● Setup the steam distillation apparatus properly. ● Tighten all the attachments so that no vapours are allowed to escape out. ● Put the sample in round bottom flask and add distilled water upto 3/4 by volume. ● Switch on the heating mantle. ● Observe the temperature inside the flask with the help of infrared thermometer so that the temperature will not be exceed more than 1050C otherwise it may affect the quality of oil. 2.3. Extraction We used simple liquid-liquid extraction process to extract the essen- tial oil and separate the flower water. This is an effective technique to process these types of extractions. The path we followed here is shown by the Fig. 1 and the complete process of essential oil extraction is repre- sented by the Fig. 2. Further, the required temperature (T � 1050C) has been used to heat the material mixture (i.e. discussed in section 2.2). The vaporized ammont of water and essential oil then cool down and separate out after collecting in the tank as shown in Fig. 2. Further, we converted this essential oil into fragrance which was characterized by an effective GC/MS technique to achieve the best quality of the product. 3. Results and discussion In this work we have prepared the fragrance from different flowers, leaves andgrass by extracting the essential oil. The prepared essential oil Fig. 3. Characterization results of orange oil by GC/MS technique. (For interpretation of the references to colour in this figure legend, the reader is referred to the Web version of this article.) Fig. 4. Characterization results of lemon grass oil by GC/MS technique. A.K. Gautam, K. Singh Journal of the Indian Chemical Society 98 (2021) 100178 3 Fig. 5. Characterization results of lavender oil by GC/MS technique. Fig. 6. Characterization results of rose oil by GC/MS technique. A.K. Gautam, K. Singh Journal of the Indian Chemical Society 98 (2021) 100178 4 Fig. 7. Characterization results of myrrh oil by GC/MS technique. A.K. Gautam, K. Singh Journal of the Indian Chemical Society 98 (2021) 100178 has been extracted by using liquid-liquid extraction prcoess. This is a very efficient and effective process to extract the essential oil of these type of materials. The fragrance quality has been checked by the Gas chroma- tography and Mass spectrometry (GC/MS) test analysis. This is a very effective analytical technique which has a combination of two different types of analysis as gas-chromatography and mass-spectrometry [10]. It is used to identify the variation of different components within a single test sample. These results are reported in figures from 3 to 8. These fig- ures (i.e. Figs. 3–8) represented the individual qualitative test analysis of orange oil, lemon grass oil, lavender oil, rose oil, myrrh oil, and cypress oil respectively. The Fig. 3 shows abundance peak with respect to time (minutes) of orange oil which was extracted by liquid-liquid extraction process. The upper portion of the figure shows the existance of different components (i.e. Pinene, d-Limonene, cinnamaldehyde, Citral, and benzyl alcohol) in the said sequence. However, the below part of the figure shows the % yield of essential oils over the concentration of these components. The Fig. 4 shows abundance peak with respect to time (minutes) of lemon grass oil which was extracted by liquid-liquid extraction process same as orange oil. The upper portion of the figure shows the existance of different components (i.e. -Pinened, -Pinened, -Citral, -Citral, Y-Pinene, p-Menthadiene, p-Limonene, and benzyl alcohol) in the said sequence. However, the below part of the figure shows the % yield of essential oils over the concentration of these com- ponents. The lemon grass oil is a volatile oil derived from the herb of Cybopogon citratus. Citral is the main constituent of this oil and limo- nene, pinene, menthadiene terpenes benzyl alcohol, and camphene, etc. as shown in Fig. 4 are the other constituents. The lemon grass oil is used very frequently in perfumery and soap industries. Similarly, the Figs. 5–8 shows abundance peak with respect to time 5 (minutes) of lavender oil, rose oil, myrrh oil, and cypress oil respectively, which were extracted by liquid-liquid extraction process as discussed above. The upper portion of the figures shows the existance of different components (i.e. o-Menthanone, menthyl acetate, p-Menthanone, Menthol, 1,3-Cis-menthol, and p-Menthen one for lavender oil, ethyl alcohol, delta terpinene, 3-carene, Terpinene, D-limonene, and p-Men- thodiene for rose oil, D-limonene, eucalyptol (cineol), Terpinene, ocy- mene, and cinnamaldehyde for myrrh oil, and R-citronellal, D-limonene, citronellol acetate, isopulegol, terpineol, and R-citronellal for cypress oil respectively) in the said sequence. However, the below part of the figure shows the % yield of essential oils over the concentration of these com- ponents. From all these figures it can be noticed that the percentage yield of the essential oils are consistent, which confirms the qualitative extraction of these essential oils from the used raw materials (i.e. orange peel, lemon grass, lavender, rose, myrrh, cypress). The results reported here are consistant with the previous studies [9,11] however they used different raw materials to prepare fragrance. The data reported in Table 1 shows the volume of essential oils extracted from orange peel, lemon grass, lavender, rose, myrrh, cypress respectively. We used 500 ml distilled water for each components to extract the essential oil from these materials by operating at different temperature range as shown in Table 1. The maximized temperature range we used for cypress was 85–900C, however for other components it vary between 80-900C. This temperature range is required to extract the essential oil as it depends on the volatility and other properties of the above materials. Further, this is a qualitative study, can be applicable to do the similar and relative analysis on fragrance and its preparations from different components as well. Fig. 8. Characterization results of cypress oil by GC/MS technique. Table 1 The extraction results of different components (i.e. orange peel, lemon grass, lavender, rose, myrrh, cypress) along with the corresponding temperature range and extracted essential oil quantities are reported in this table. The rawmaterials, its weight, distilled water quantity, required temperature range and extracted essential oil quantities are listed here in column 2, 3, 4, 5, and 6 respectively. The notations used for column no. 2, 3, 4, and 6 can be read as RM - RawMaterial, W - Weight (gm), VDW - Volume of distilled water (ml), VEO - Volume of Essential oil (ml). S.No. RM W VDW Temp. (�C) VEO 1 Orangepeel 300 500 80 � 90 2.0 2 Lemongrass 250 500 80 � 90 1.8 3 Lavender 250 500 70 � 75 0.7 4 Rose 250 500 65 � 70 0.3 5 Myrrh 250 500 80 � 90 1.6 6 Cypress 300 500 85 � 90 1.2 A.K. Gautam, K. Singh Journal of the Indian Chemical Society 98 (2021) 100178 4. Conclusion In this work, we prepared the fragrance from different components (i.e. orange peel, lemon grass, lavender, rose, myrrh, cypress). By extracting the essential oil from liquid-liquid extraction techniques, it was found that this is one of the most promising technique for the essential oil extraction from different components. This type of extraction is temperature sensitive for the materials like oils, resins, hydrocarbons etc., which are completely insoluble in water and may be decompose at their boiling point. Further, the results shows that, the essential oil vol- ume increases while increasing the temperature with respect to time. From this study, it can conclude that the, lemon grass, rose, and cypress have the highest yield and number of components among the other tested samples (i.e. orange, lavender, and myrrh) along with purity. Therefore, these components (i.e. lemon grass, rose, and cypress) are the better 6 sourse to prepare the quality fragrance by extracting the essential oil. Declaration of competing interest The authors declare no conflict of interest. Acknowledgements We are thankful to RBS Engineering Technical Campus, Bichpuri, Agra and NIT Hamirpur, (H.P.), India for providing the required facilities to persue this work. References [1] Sarkic A, Stappen I. Essential oils and their single compounds in cosmetics-A critical review. Cosmetics 2018;5. 01–21. [2] Feczk�o T, Kokol V, Voncina B. Preparation and characterization of ethylcellulose- based microcapsules for sustaining release of a model fragrance. Macromol. Res. 2010;18:636–40. [3] Worwood VA. The Complete Book of Essential Oils and Aromatherapy. 1st edition. New World Library; 1991. p. 1–448. [4] Reeds PJ. Dispensable and indispensable amino acids for humans. J. Nutr. 2000; 148:1835S–40S. [5] Khan F, Dwivedi AK. Study of Eucalyptus and lemongrass essential oil extracted by hydro distillation method. IRJET 2019;6:779–84. [6] Bicchi C, Joulain D. Techniques for preparing essential oils and aromatic extracts. Flavour Fragrance J. 2018;33:133–4. [7] Rassem HHA, Nour AH, Yunus RM. Techniques for extraction of essential oils from Plants: a Review. Aust. J. Basic and Appl. Sci. 2016;10:117–27. [8] Lucchesi ME, Smadja J, Bradshaw S, Louw W, Chemat F. Solvent-free extractionof elletaria cardamomum L.: a multivariate study of a new technique for the extraction of essential oil. J. Food Eng. 2007;79:1079–86. [9] Biniecka M, Caroli S. Analytical methods for the quantification of volatile in Analytical Chemistry. Trends Anal. Chem. 2011;30:1835S–40S. [10] Sparkman OD, Penton Z, Kitson FG. Gas-chromatography and Mass-Spectrometry: A Practicle Guid. Academic Press; 2011. ISBN:978–0–08–092015–3. [11] Augusto F, Lopes AL, Zini CA. Sampling and sample preparation for analysism of aromas and fragrances. 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Introduction 2. Methodology 2.1. Materials 2.2. Preparation of perfumes 2.3. Extraction 3. Results and discussion 4. Conclusion Declaration of competing interest Acknowledgements References
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