Source: UNIVERSITY OF GEORGIA submitted to NRP
MICROENCAPSULATION TECHNOLOGY USING ESSENTIAL OILS TO PRODUCE SMART TEXTILE FUNCTIONALITIES THAT IMPROVE HUMAN HEALTH
Sponsoring Institution
National Institute of Food and Agriculture
Project Status
COMPLETE
Funding Source
Reporting Frequency
Annual
Accession No.
0220388
Grant No.
(N/A)
Cumulative Award Amt.
(N/A)
Proposal No.
(N/A)
Multistate No.
(N/A)
Project Start Date
Oct 1, 2009
Project End Date
Oct 1, 2014
Grant Year
(N/A)
Program Code
[(N/A)]- (N/A)
Recipient Organization
UNIVERSITY OF GEORGIA
200 D.W. BROOKS DR
ATHENS,GA 30602-5016
Performing Department
College of Family & Consumer Sciences
Non Technical Summary
This new project proposal focuses on the potential of microencapsulation technology using essential oils for producing smart and functional textiles. Biobased microcapsules present several advantages such as?controlled release, prevention of evaporation of volatile oils, and stability against thermal and chemical exposure. Many experiments have been performed to encapsulate various active agents, such as fragrances, skin softeners, insect repellents, dyes, vitamins, antimicrobial agents, phase change materials, fire retardants, and polychromic and thermochromic materials. In spite of these important advances, there is still a critical gap in the knowledge base for developing biobased microcapsules (which are physically and chemically stable) and their durable incorporation into textiles. These limitations have affected the utilization of microcapsules in textile applications. The proposed research is expected to contribute an in-depth understanding of microcapsule formulations, including essential oils and their blends, to produce desired antimicrobial and antiallergenic effects. This project intends to examine the use of inexpensive, effective, renewable essential oils as a core material, and proteins and polysaccharides as shell materials.
Animal Health Component
(N/A)
Research Effort Categories
Basic
(N/A)
Applied
(N/A)
Developmental
(N/A)
Classification

Knowledge Area (KA)Subject of Investigation (SOI)Field of Science (FOS)Percent
80451202000100%
Goals / Objectives
Fabric treatments are highly desirable for apparel,home furnishings,and medical textiles to impart smart functionalities and protect the public from biological threats and other health hazards.While still in its infancy,microencapsulation technology provides the textile industry with a means of imparting finishes and properties to textiles that are cost-effective and safe.Many studies have been designed to develop microcapsules and incorporate them into fabrics.In spite of important advances,there is still a critical gap in the knowledge base regarding the design of durable(physically and chemically stable) microcapsules for desired applications in cotton textiles.This continued need is an important problem because microcapsules are required to be stable against heat and external shocks in order to produce desired effects such as antimicrobial and antiallergenic in cotton fabrics for several cycles of washing and drying.The long-term goal of this research is to expand the knowledge base of microcapsules and to develop smart textiles that will thwart biohazards and improve human health.The objectives of this particular application are:1.Production of protein-based microcapsules loaded with plant-source active agents and 2.Attach and test the efficacy of microcapsules for antimicrobial and antiallergenic effects.Our central hypothesis is that well-established microencapsulation techniques can be used to produce microsize capsules loaded with essential oils extracted from natural sources to produce durable,antimicrobial and antiallergenic functionalities in cotton textiles.In addition to our supportive preliminary literature findings,we have the assembled multidisciplinary research team including investigators from food science,nanostructures,and microbiology who are pursuing research that is complementary to that proposed here.Because of our complementary expertise and shared resources,the setting is conducive to the successful completion of the proposed investigations.The proposed research is creative and original because we are using a novel microencapsulation formulation to develop durable microcapsules for smart textile applications.It is anticipated that this approach will yield the following outcomes:Outcome 1:Specific essential oils and their blends will be encapsulated using microencapsulation methods.Outcome 2:The outcome of the finishing experiments and the evaluation of textiles will enable the potential of microencapsulation technology for developing functional and smart textiles.This research will help us to fulfill our objective of developing durable microcapsules that will catalyze a vertical step in creating barrier fabrics with novel finishes and processes for protection against biological threats.
Project Methods
PROCEDURE Obj1:Develop microcapsules loaded with essential oils Exp1:Chemical Method Microcapsules will be prepared using the oil emulsion method.The shell or coating will be made from proteins incorporating various essential oils.Egg albumin(grade II),keratin,and bovine serum albumin proteins,a surfactant(Span 85),a crosslinking or denaturing agent(glutaraldehyde,grade II,25% in H2O)and essential oils (peppermint,caraway,oregano,allspice,Chenopodium,cinnamon,clove,eucal yptus, rosemary,matrecary,rose,fennel,cayenne pepper,tea tree,and thyme)will be purchased and used as received.The required equipment a mechanical stirrer(max 500 rpm),centrifuge,and microscope,are available in our research laboratory.In addition,an inexpensive home steam distillation unit will be purchased to extract various essential oils.A factorial design methodology will be used to determine the interaction between various independent variables to produce durable microcapsules.We will optimize variables such as type of shell protein,protein concentration,agitation speed,crosslinking or temperature of denaturing and amount of surfactant using a control sample oil.This methodology will produce durable microcapsules from various essential oils.Statistical determination of the size distribution of the microcapsules and their shape and state of grafting onto the cotton fabric will be evaluated using SEM.Both thermal and mechanicalanalyses will be undertaken to determine the stability of microcapsules.Microcapsule production using optimized parameters will be developed several times to improve the precision.We expect to produce durable microencapsulated essential oils with a protein-based shell material.Protein has a wide range of functionalities appropriate for further modification according to the desired effect and durability.Exp2:Microencapsulation of essential oils-Mechanical Method BRACE GmbH company uses a special drip casting process for the production of core-shell microcapsules in a single step.We will utilize their facility to develop microcapsules through this unique process.The recipe used in the chemical method will be sent to BRACE Gmbh to produce these microcapsules.Obj2:Attach and test the efficacy of microcapsules for antimicrobial and antiallergenic effects Exp1:Use chemical methods of grafting that covalently bind the microcapsules to the textile substrates.Cotton textiles(sheeting,suiting,and shirting fabrics)crosslinking reagent 1,2,3,4-butanetetracarboxylic acid and catalyst will be purchased and used as received.The AATCC methods #147 and #100 will be used to determine the efficacy of the antimicrobial effect.The assessment of the efficacy of anti-mite action will be based on culture tests performed according to the standard AFNOR G39-011 and AATCC method #194.The culture will be produced using the method developed by Arilian et al.A statistical determination of the % reduction of dust mites will be conducted.Commercially available textiles with antimicrobial and antiallergenic activity will be used as control samples.

Progress 10/01/09 to 10/01/14

Outputs
Target Audience:This research presented the use of the essential oils using microencapsulation and their major components as eco-friendly agents for controlling HDMs that are consumer and environmentally friendly replacements for synthetic acaricides in terms of their impact on the environment and human health. This study showed that coacervation method is useful to produce thermally stable microcapsules from natural-based materials. Microencapsulation approach seems cost effective and environmentally friendly to provide durable, long-term health effects of cotton textiles. Essential oils are obviously the alternative and effective source as acaricides in terms of their impact on environment and human health. This study has helped determine that clove, thyme, rosemary and peppermint essential oils can be used as natural acaricides for controlling HDMs in an indoor setting. Upon concluding the research, this study is expected to contribute to and make a new type of material that will significantly reduce health problems related to dust mites, allergens, and bacteria in households as well as other places that use the material for everyday use. This would in turn make healthier people and eliminate allergen problems that don't have a permanent or reliable solution to diminishing those populations and health risks. The knowledge gained through this research will help to produce smart textiles for applications that include vitamins, antibiotics, phase change materials, photochromic material, therapeutic drugs, and insect repellents. This interdisciplinary research includes cooperation between textile and material scientists, microbiologists, and food scientists to produce a multitude of innovative applications for textiles. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided? Nothing Reported How have the results been disseminated to communities of interest?It was mainly through publishing and/or presenting at various scholarly venues such as journal article and conferences. Moreover, one high school student, Lauren Tolbert, invloved in 2010 and worked on indoor air quality and onmicroencapsulation of essential oils later before lending into our undergraduate program.Please see the following list: Kim, Joo-Ran and Sharma, Suraj (2010). Microencapsulation Technology Using Essential Oils to Produce Acaricides Against House Dust Mites, Herman and Myrtle Goldstein Student paper competition, AATCC's International Conference, Atlanta, GA. Kim, J.R. (2010). Microencapsulation technology using essential oils to produce smart textile functionalities. Poster Presentation. Graduate Student Consortium and 10th Annual Graduate Interdisciplinary Research Conference, University of Georgia. Joo Ran Kim, M.S. in Textiles, Merchandising and Interiors with an emphasis in Textile Science - August 2010; Thesis Title: Microencapsulation Technology Using Essential Oils to Produce Acaricides against House Dust Mites. Kim, Joo Ran and Sharma, Suraj. Microencapsulation Technology Using Essential Oils to Produce Durable Textile Functionalities. Abstracts of Papers, 2011 Beltwide Cotton Conferences, Atlanta, GA, United States, January 4-7, 2011. Kim, Joo Ran, and Sharma, Suraj, Acaricidal Activities Of Clove Bud Oil And Red Thyme Oil Using Microencapsulation Against House Dust Mites, Journal of Microencapsulation, 29(1):82-91, 2011. (peer-reviewed). Daubenmire, S, Sharma, S.,and Tolbert, L. (2013) Fumigant Activities of Peppermint Oil and Rosemary Oil against House Dust Mites as well as their Antimicrobial Activities. The Fiber Society International Conference. Sharma, S., Daubenmire, S., and Tolbert, L. (2014) Effects of antimicrobial activities of peppermint and rosemary oils incorporated into textiles. American Association of Textile Chemists and Colorists (AATCC) International Conference. What do you plan to do during the next reporting period to accomplish the goals? Nothing Reported

Impacts
What was accomplished under these goals? Technical Outcomes:1) Indoor air quality analysis:Analysis of the data collected from various households produced an average colony count for bacteria of 16.4 count per household (CPH), ranging from 8.6 to 29.6; and the average colony count for fungi was 15.8 CPH, ranging from 9.6 to 26. This means that the IAQ of each household fails the standards of air quality because the standard for very poor quality is 12+ CPH. Since IAQ is related to the health and comfort of the occupants, the occupants of the failed quality houses are advised to take necessary steps such as washing bed coverings and sheets in hot water with detergent and fabric-save bleach, dusting all surfaces, wiping down all appliances with a clean rag and disinfectant, and vacuuming the floors. By doing this regularly, the colonies of HDMs are diminished. This is a good method to use even though it is not a long-term eliminator of the HDMs in houses and spaces. 2) Microencapsulation of thyme and clove essential oils and their characterization:The outcome of this study showed that the coacervation microencapsulation method was useful for encapsulating thyme and clove oils into the microcapsules enclosed with gelatin, exhibiting size of 4 to 85 μm in the suspension. A Factorial design statistical method was used to determine the effect of main variables (type of oil, oil to gelatin ratio, stirring speed and surfactant) on the size of microcapsules. Results showed that stirring speed and type of oil (viscosity effect) were the critical variables to control the size of microcapsules. In addition, it was observed that vacuum drying can be an effective process to prevent aggregation of microcapsules and attach mechanically to the fabric without any binder. TGA testing showed that microcapsules loaded with thyme oil exhibited more consistent or narrow range of oil loading (50 to 80% w/w oil content). Conditions with 1:2 ratio of gelatin to oil and without surfactant showed the average diameter of microcapsules under 8 μm and with clove oil loading of 40% and thyme oil loading of 60%.Furthermore detailed studies of surfactant and vacuum drying processes are required. Additionally interactions between factors are needed to get more precise results. 3) Acaricide study of thyme and essential oils using fumigation method and on microencapsulated treated fabric:From GC-MS analysis, thymol was the main monoterpenoid, comprising 54% of thyme red oil. It has been indicated to be effective as an antimicrobial and antifungal agent (Pierce 1999). The second largest constituent, para-cymene, also exhibited antimicrobial activity (Deans & Ritchie 1987). Eugenol and B-caryophyllene were the main phenolic monoterpenoids in the clove bud oil comprising 84% and 12%, respectively. In our direct contact test with open lids, clove bud and thyme red were the most effective acaricidal agents on HDM (Der. f) with up to 100% mortality at 0.05 mg cm-2, whereas a control maintained the starting number of HDM. In our study, the mites exposed to clove and thyme oils, the natural plant extracts, showed a leg movement patterns similar to death induced by natural causes. The long-term (72 hours) examination of acaricidal activity of textiles with attached mcirocapsules reduced the colony of dust mites significantly (94 % for clove and 84% for thyme). In summary, our results showed that it was possible to control HDM using microencapsulated clove and thyme oils containing specific phenolic monoterpenoids such as eugenol and thymol. Among the two encapsulated essential oils, constituents of clove bud oil could be an efficient agent in reducing the population of live house dust mites (Der. f) because of its antioxidation properties from its allyl-structure and the natural defense functions of phenylpropanoids against herbivores. During the production of microcapsules, clove bud oil can maintain stability due to better antioxidant property and lose less phenolic properties affecting the mortality of HDMs than thyme red oil. From our experiments, HDM showed the symptoms of knockdown type death with forwarding leg movements induced by natural plant sources in both clove and thyme oils. The results of this study and previous studies demonstrated that clove bud oil could be an effective natural alternative to synthetic chemicals in reducing the population of HDMs. This research supports the use of essential oils and their major components as eco-friendly agents for the control of HDM (Der. f). For the practical use of essential oils, it is necessary to examine the safety of these materials to humans and to develop formulations to improve their efficacy and stability.Further detailed studies of surfactant and vacuum drying processes are needed since this method was limited to the low quantity and small size of microcapsules. There needs to be more study using confocal microscope to investigate the wall thickness of microcapsules. 3) Acaricide study of rosemary and peppermint essential oils using fumigation method and on microencapsulated treated fabric:In subsequent research, the study of two essential oils, rosemary oil and peppermint oil, and their effects on various bacteria, fungi, and allergens were investigated and evaluated. Rosemary is an evergreen perennial bush that tends to be shrubby. It can grow to 1.5 meters high, having blue flowers and green needle-shaped leaves. Rosemary is marketed and sold in several different forms and is effective on many harmful bacteria and fungi such as Escherichia coli, Salmonella typhi, S. enteritidis, and Shigella sone (Bozin et al. 2007). It is a sweet smelling and fresh herb. The oil is usually extracted by the steam distillation method, and is in the form of a clear liquid. Peppermint is a perennial invasive herb that has hairy leaves and pink flowers and may grow to 1 meter high. Peppermint contains trichomes which contain secretory cells arranged in an eight-celled disc which contributes to the synthesis of the oil (Rios-Estepa et al. 2010). Like rosemary oil, the extraction method is usually steam distillation, but typically has a yellow tinge and a very strong, minty aroma.The main constituent of peppermint oil, monoterpene laevo-menthol, comprises 53.6% of it. Menthol has been tested against microbial strains such as S. aureus and E. coli showing that it does have antimicrobial properties since it prevented the growth of such strains (Trombetta et al. 2005). The second and third largest constituents, iso-menthone (7.2%) and 1,8-cineole (5%), are also crucial constituents that contain necessary antimicrobial properties. In rosemary, the largest constituent, α-pinene (21%), exhibits antimicrobial activity against E. coli, Staphylococcus aureus, Micrococcus luteus, and Bacillus subtilis (Derwich et al. 2010). β-pinene (14%) and 1,8-cineole (13%), the second and third largest constituents of rosemary also exercise the necessary antimicrobial properties. Once the microcapsules were solidified through vacuum drying, their surface and shape were analyzed using a scanning electron microscope. Microencapsulation and vacuum drying used together have been marked as an effective way in preventing aggregation of small microcapsules. Microcapsules in this study were found to be around 20 µm in size and sometimes covered in a foamy coating, though they still did retain a spherical shape.By using the AATCC test method 194-2007 the acaricidal activity of the essential oils, Figure 5 shows the effects of the oils on the dust mites which are dead. This means that the oils effectively kill the dust mitesand would in turn be a plausible solution towards containing the HDMs in a sustainable way. ?

Publications

  • Type: Theses/Dissertations Status: Published Year Published: 2010 Citation: Joo Ran Kim, M.S. in Textiles, Merchandising and Interiors with an emphasis in Textile Science  August 2010; Thesis Title: Microencapsulation Technology Using Essential Oils to Produce Acaricides against House Dust Mites.
  • Type: Conference Papers and Presentations Status: Accepted Year Published: 2013 Citation: Daubenmire, S, Sharma, S.,and Tolbert, L. (2013) Fumigant Activities of Peppermint Oil and Rosemary Oil against House Dust Mites as well as their Antimicrobial Activities. The Fiber Society International Conference.
  • Type: Journal Articles Status: Published Year Published: 2011 Citation: Kim, Joo Ran, and Sharma, Suraj, Acaricidal Activities Of Clove Bud Oil And Red Thyme Oil Using Microencapsulation Against House Dust Mites, Journal of Microencapsulation, 29(1):82-91, 2011. (peer-reviewed).
  • Type: Conference Papers and Presentations Status: Accepted Year Published: 2010 Citation: Kim, Joo-Ran and Sharma, Suraj (2010). Microencapsulation Technology Using Essential Oils to Produce Acaricides Against House Dust Mites, Herman and Myrtle Goldstein Student paper competition, AATCCs International Conference, Atlanta, GA.
  • Type: Conference Papers and Presentations Status: Accepted Year Published: 2011 Citation: Kim, Joo Ran and Sharma, Suraj. Microencapsulation Technology Using Essential Oils to Produce Durable Textile Functionalities. Abstracts of Papers, 2011 Beltwide Cotton Conferences, Atlanta, GA, United States, January 4-7, 2011.
  • Type: Conference Papers and Presentations Status: Accepted Year Published: 2014 Citation: Sharma, S., Daubenmire, S., and Tolbert, L. (2014) Effects of antimicrobial activities of peppermint and rosemary oils incorporated into textiles. American Association of Textile Chemists and Colorists (AATCC) International Conference.


Progress 01/01/11 to 12/31/11

Outputs
OUTPUTS: The long-term goal of this research is to expand the knowledge base of microcapsules and to develop functional textiles that will improve human health and wellbeing. The objectives of this research project are: 1. Production of protein-based microcapsules loaded with plant-source active agents 2. Attach and test the efficacy of microcapsules for antimicrobial and antidustmite effects To accomplish these objectives, first study was conducted to identify the effectiveness of various essential oils, such as clove, rosemary, peppermint and thyme oils. Simple coacervation method was used to develop microcapsules loaded with these oils. Factorial design was used to determine the effect of main variables (type of oil, oil to gelatin ratio, stirring speed and surfactant) on the size of microcapsules. PARTICIPANTS: Dr. Suraj Sharma, Ms. Joo Ran Kim TARGET AUDIENCES: For apparel and furnishing manufacturers. PROJECT MODIFICATIONS: Not relevant to this project.

Impacts
Clove, rosemary, peppermint and thyme oils were found to be effective acaricides. Results showed that stirring speed and type of oil (viscosity effect) were the critical variables to control the size of microcapsules. In addition, it was observed that vacuum drying can be an effective process to prevent aggregation of microcapsules and attach mechanically to the fabric without any binder. In another study, through bioassay against HDM (Der.f), we observed that all studied oils had significant effect in reducing the growth of dustmites. This study showed that simple coacervation method is useful to produce thermally stable microcapsules from natural-based materials. Microencapsulation approach seems cost effective and environmentally friendly to provide durable, long-term health effects of cotton textiles. Essential oils are obviously the alternative and effective source as acaricides in terms of their impact on environment and human health.

Publications

  • Kim, Joo Ran; *Sharma, Suraj. Microencapsulation Technology Using Essential Oils to Produce Durable Textile Functionalities. Abstracts of Papers, 2011 Beltwide Cotton Conferences, Atlanta, GA, United States, January 4-7, 2011.
  • Kim, Joo Ran, and Sharma, Suraj, Acaricidal Activities Of Clove Bud Oil And Red Thyme Oil Using Microencapsulation Against House Dust Mites, Journal of Microencapsulation, 29(1):82-91, 2011. (peer-reviewed)


Progress 01/01/10 to 12/31/10

Outputs
OUTPUTS: Dr. Sharma's research group used coacervation method to develop microcapsules loaded with essential oils such as clove and thyme. A factorial design method was used to determine the effect of most influential variables (type of oils, oil to gelatin ratio, stirring speed and surfactant) on the size of microcapsules. PARTICIPANTS: Not relevant to this project. TARGET AUDIENCES: Not relevant to this project. PROJECT MODIFICATIONS: Not relevant to this project.

Impacts
To accomplish the stated objectives in the proposal, first study was conducted to identify the effectiveness of various essential oils. Clove and Thyme oils were found to be effective acaricides or dustmites killing efficacy. Through a study utilizing fumigation method and bioassay against HDM (Der.f), we observed that clove containing phenolic compound (85% eugenol) was more effective in reducing the number of house dust mites than thyme oil.Subsequently, simple coacervation method was used to develop microcapsules loaded with these oils. Factorial design approach was used to determine the effect of main variables (type of oils, oil to gelatin ratio, stirring speed and surfactant) on the size of microcapsules. Results showed that stirring speed and type of oil (viscosity effect) were the critical variables to govern the size of microcapsules. In addition, it was observed that vacuum drying can be an effective process to prevent aggregation of microcapsules and attach mechanically to the fabric without any binder. This study showed that coacervation method is useful to produce thermally stable microcapsules from natural-based materials. Microencapsulation approach seems cost effective and environmentally friendly to provide durable, long-term health effects of cotton textiles. Essential oils are obviously the alternative and effective source as acaricides in terms of their impact on environment and human health.

Publications

  • Kim, Joo-Ran and Sharma, Suraj (2010). Microencapsulation Technology Using Essential Oils to Produce Acaricides Against House Dust Mites, Herman and Myrtle Goldstein Student paper competition, AATCC International Conference, Atlanta, GA
  • Joo Ran Kim, M.S. in Textiles, Merchandising and Interiors with an emphasis in Textile Science,August 2010; Thesis Title: Microencapsulation Technology Using Essential Oils to Produce Acaricides against House Dust Mites